U.S. patent application number 11/988320 was filed with the patent office on 2009-11-05 for food articles with delivery devices and methods for the preparation thereof.
Invention is credited to Micheele M. Boyden, Peter C. Dea, Brenda Y. Fong, Richard A. Gorski, Deepa Mathew, Pete H. Mattson, Suzette Rejeanne Robert, Sharon Ann Spurvey, Laura M. Tringale.
Application Number | 20090274791 11/988320 |
Document ID | / |
Family ID | 38712274 |
Filed Date | 2009-11-05 |
United States Patent
Application |
20090274791 |
Kind Code |
A1 |
Mattson; Pete H. ; et
al. |
November 5, 2009 |
Food Articles With Delivery Devices and Methods for the Preparation
Thereof
Abstract
Disclosed are food articles comprising delivery devices. Methods
of preparing such food articles are also disclosed.
Inventors: |
Mattson; Pete H.; (The Sea
Ranch, CA) ; Gorski; Richard A.; (San Jose, CA)
; Fong; Brenda Y.; (San Mateo, CA) ; Tringale;
Laura M.; (San Francisco, CA) ; Mathew; Deepa;
(San Ramon, CA) ; Dea; Peter C.; (San Ramon,
CA) ; Spurvey; Sharon Ann; (Middle Sackville, CA)
; Robert; Suzette Rejeanne; (Saulnierville, CA) ;
Boyden; Micheele M.; (Halifax, CA) |
Correspondence
Address: |
Ballard Spahr Andrews & Ingersoll, LLP
SUITE 1000, 999 PEACHTREE STREET
ATLANTA
GA
30309-3915
US
|
Family ID: |
38712274 |
Appl. No.: |
11/988320 |
Filed: |
June 23, 2006 |
PCT Filed: |
June 23, 2006 |
PCT NO: |
PCT/US2006/024735 |
371 Date: |
June 4, 2009 |
Related U.S. Patent Documents
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
|
|
11435605 |
May 17, 2006 |
|
|
|
11988320 |
|
|
|
|
60697092 |
Jul 7, 2005 |
|
|
|
60811503 |
Jun 7, 2006 |
|
|
|
60811830 |
Jun 8, 2006 |
|
|
|
Current U.S.
Class: |
426/2 ; 426/100;
426/103; 426/72; 426/89; 426/92; 426/93; 426/96 |
Current CPC
Class: |
A23V 2002/00 20130101;
A23C 9/1528 20130101; A23P 10/30 20160801; A23V 2002/00 20130101;
A23L 33/40 20160801; A23C 2260/152 20130101; A23C 9/1315 20130101;
A23V 2300/41 20130101 |
Class at
Publication: |
426/2 ; 426/89;
426/103; 426/72; 426/96; 426/92; 426/100; 426/93 |
International
Class: |
A23K 1/18 20060101
A23K001/18; A23L 1/00 20060101 A23L001/00; A23L 1/30 20060101
A23L001/30; A23L 1/216 20060101 A23L001/216; A23L 1/31 20060101
A23L001/31; A23L 1/36 20060101 A23L001/36 |
Claims
1. A food article comprising a microcapsule, wherein the
microcapsule comprises an agglomeration of primary microcapsules
and a loading substance, each individual primary microcapsule
having a primary shell, wherein the loading substance is
encapsulated by the primary shell, and wherein the agglomeration is
encapsulated by an outer shell.
2. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise a
surfactant, gelatin, polyphosphate, polysaccharide, or a mixture
thereof.
3. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise gelatin
type A, gelatin type B, polyphosphate, gum arabic, alginate,
chitosan, carrageenan, pectin, starch, modified starch,
alfa-lactalbumin, beta-lactoglobumin, ovalbumin, polysorbiton,
maltodextrin, cyclodextrin, cellulose, methyl cellulose, ethyl
cellulose, hydropropylmethylcellulose, carboxymethylcellulose, milk
protein, whey protein, soy protein, canola protein, albumin, kosher
gelatin, non-kosher gelatin, Halal gelatin, non-Halal gelatin, or a
mixture thereof.
4. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise fish
gelatin.
5. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise pork
gelatin.
6. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise a
gelatin with a Bloom number of from about 0 to about 50.
7. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise a
gelatin with a Bloom number of from about 51 to about 300.
8. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise a
gelatin with a Bloom number of about 0, about 210, about 220, or
about 240.
9. The food article of claim 1, wherein the primary shell, the
outer shell, or both the primary and outer shells comprise a
complex coacervate.
10. The food article of claim 9, wherein the complex coacervate is
a complex coacervate of gelatin and polyphosphate.
11. The food article of claim 1, wherein the outer shell has an
average diameter of from about 1 .mu.m to about 2,000 .mu.m.
12. The food article of claim 1, wherein the primary shell has an
average diameter of from about 40 nm to about 10 .mu.m.
13. The food article claim 1, wherein the primary shell, the outer
shell, or both the primary and outer shells comprises an
antioxidant.
14. The food article of claim 1, wherein the loading substance
comprises a biologically active substance, a nutritional
supplement, a flavoring substance, a vitamin, a mineral, a
carbohydrate, a steroid, a trace element, a protein, or any mixture
thereof.
15. The food article of claim 1, wherein the loading substance
comprises one or more oils chosen from a microbial oil, algal oil,
fungal oil, and plant oil.
16. The food article of claim 1, wherein the loading substance
comprises fish oil.
17. The food article of claim 16, wherein the fish oil comprises an
Atlantic fish oil, Pacific fish oil, Mediterranean fish oil, light
pressed fish oil, alkaline treated fish oil, heat treated fish oil,
light and heavy brown fish oil, bonito oil, pilchard oil, tuna oil,
sea bass oil, halibut oil, spearfish oil, barracuda oil, cod oil,
menhaden oil, sardine oil, anchovy oil, capelin oil, Atlantic cod
oil, Atlantic herring oil, Atlantic mackerel oil, Atlantic menhaden
oil, salmonid oil, or shark oil.
18. The food article of claim 1, wherein the loading substance
comprises an omega-3 fatty acid, and ester of an omega-3 fatty
acid, and/or a mixture thereof.
19. The food article of claim 18, wherein the ester of an omega-3
fatty acid comprises an alkyl ester of an omega-3 fatty acid, a
monoglyceride of an omega-3 fatty acid, a diglyceride of an omega-3
fatty acid, a triglyceride ester of an omega-3 fatty acid, a
phytosterol ester of an omega-3 fatty acid, an ester of an omega-3
fatty acid and an antioxidant, a furanoid ester of an omega-3 fatty
acid, and/or a mixture thereof.
20. The food article of claim 1, wherein the loading substance
comprises docosahexaenoic acid and/or eicosapentaenoic acid, a
C.sub.1-C.sub.6 alkyl ester thereof, a triglyceride ester thereof,
a phytosterol ester thereof, and/or a mixture thereof.
21. The food article of claim 1, wherein the loading substance
further comprises a preservative, antimicrobial, chelating agent,
thickener, flavoring, diluent, emulsifier, dispersing aid, binder
or any mixture thereof.
22. The food article of claim 1, wherein the loading substance is
from about 20% to about 90% by weight of the microcapsule.
23-34. (canceled)
35. The food article of claim 1, wherein the food article is a wet
soup.
36. The food article of claim 1, wherein the food article is a
dehydrated and culinary food.
37. The food article of claim 1, wherein the food article is a
beverage.
38. The food article of claim 1, wherein the food article is a
frozen food.
39. The food article of claim 1, wherein the food article is a
seasoning.
40. The food article of claim 1, wherein the food article is apple
sauce.
41. The food article of claim 1, wherein the food article is baby
food.
42. The food article of claim 1, wherein the food article is a
breaded meat.
43. The food article of claim 1, wherein the food article is a
pasteurized process cheese food.
44. The food article of claim 1, wherein the food article is a
granola bar or cereal bar.
45. The food article of claim 1, wherein the food article is a
bread, cereal, or waffle.
46. The food article of claim 1, wherein the food article is
soymilk.
47. The food article of claim 1, wherein the food article is a
gummy candy.
48. The food article of claim 1, wherein the food article is a
pasta or pasta sauce.
49. The food article of claim 1, wherein the food article is a
tomato sauce.
50. The food article of claim 1, wherein the food article is orange
juice.
51. The food article of claim 1, wherein the food article is a
snack food.
52. The food article of claim 51, wherein the snack food is a
potato chip, corn chip, or tortilla chip.
53. The food article of claim 1, wherein the food article is a chip
and the loading substance comprises an omega-3 fatty acid.
54. The food article of claim 53, wherein the microcapsule is
present at less than or equal to about 6% by weight, based on the
total weight of the chip.
55. The food article of claim 53, wherein the microcapsule is
present at less than or equal to about 5% by weight, based on the
total weight of the chip.
56. The food article of claim 53, wherein the microcapsule is
present at from about 1% to about 4% by weight, based on the total
weight of the chip.
57. The food article of claim 1, further comprising a
probiotic.
58. A method of delivering a loading substance to a subject,
comprising administering to the subject the food article of claim
1.
59-66. (canceled)
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of priority to U.S.
Provisional Patent Application 60/697,092, filed Jul. 7, 2005, U.S.
Provisional Patent Application 60/811,830, filed Jun. 8, 2006, U.S.
Provisional Patent Application 60/811,503, filed Jun. 7, 2006, and
U.S. Utility application Ser. No. 11/435,605, filed May 17, 2006,
which are all incorporated by reference herein in their
entireties.
FIELD
[0002] The disclosure generally relates to food articles comprising
delivery devices. Methods of preparing such food articles are also
disclosed.
BACKGROUND
[0003] Polyunsaturated fatty acids, for example, omega-3 fatty
acids, are vital to everyday life and function. Such compounds play
critical roles in the structure of cell membranes and they form the
foundation for the synthesis of many cell mediators (e.g.,
prostaglandins and leukotrienes). These cell mediators are an
important part of human physiology and can affect, for example,
cell proliferation, cell signaling, gene expression, coagulation,
and inflammation.
[0004] As an example, omega-3 fatty acids and their derivates are
known to be primary components of brain and nerve tissue. Also,
omega-3 fatty acids can reduce thrombogenisis and inflammation by
altering certain pathways leading to the production of inflammatory
mediators (e.g., prostaglandins, leukotrienes and thromboxanes).
See e.g., Sugano, Michihiro. "Balanced intake of polyunsaturated
fatty acids for health benefits." Journal of Oleo Science (2001),
50(5):305-311. Further, omega-3 fatty acids are known to positively
affect heart function, hemodynamics, and arterial endothelial
function. The American Heart Association has reported that omega-3
fatty acids can reduce cardiovascular and heart disease risk.
[0005] The primary source of such polyunsaturated fatty acids is
through diet. Diets rich in polyunsaturated fatty acids like
omega-3 fatty acids are known to have beneficial effects for heart
disease, cancer, arthritis, allergies, and other chronic diseases.
(See e.g., The American Heart Association, Scientific Statement,
"Fish Consumption, Fish Oil, Omega-3 Fatty Acids and Cardiovascular
Disease," November 2002; Radack et al., "The effects of low doses
of omega-3 fatty acid supplementation on blood pressure in
hypertensive subjects: a randomized controlled trial." Arch.
Intern. Med. (1991) 151:1173-1180; Appel et al., "Does
supplementation of diet with `fish oil` reduce blood pressure? A
meta-analysis of controlled clinical trials. Arch. Intern. Med.
(1993) 153(12): 1429-1438; GISSI-Prevenzione Investigators.
"Dietary supplementation with omega-3 polyunsaturated fatty acids
and vitamin E after myocardial infarction: results of the
GISSI-Prevenzione trial." Lancet (1999) 354:447-455.)
[0006] The American Heart Association has recommended that people
may need 2 to 4 grams of omega-3 fatty acids per day.
Unfortunately, most western diets are deficient in these beneficial
fatty acids. Even a 1 gram/day dose may be more than can readily be
achieved through diet alone. Thus, people who desire to increase
their intake of such polyunsaturated fatty acids typically turn to
dietary supplements. Such supplements, however, are usually
sensitive to oxidation and can be foul smelling and tasting.
Further, compliance with dietary supplement regimens requires
discipline, which is often wanting.
[0007] In light of the health benefits of polyunsaturated fatty
acids and the problems associated with adequate intake of such
compounds, what is needed in the art are food articles containing
beneficial compounds such as, for example, polyunsaturated fatty
acids and which are more palatable and pleasing to the consumer.
The subject matter disclosed herein meets these and other
needs.
SUMMARY
[0008] In accordance with the purposes of the disclosed materials,
compounds, compositions, articles, and methods, as embodied and
broadly described herein, the disclosed subject matter, in one
aspect, relates to compounds and compositions and methods for
preparing and using such compounds and compositions. In a further
aspect, the disclosed subject matter relates to articles of food
comprising delivery devices. In a still further aspect, the
disclosed subject matter relates to methods of preparing such food
articles. In yet a further aspect, the disclosed subject matter
relates to homogenized formulations that comprise microcapsules,
and to food articles prepared with or comprising homogenized
formulations. In a still further aspect, the disclosed subject
matter relates to methods of making and using the disclosed
homogenized formulations and food articles prepared from and
comprising them.
[0009] Additional advantages will be set forth in part in the
description that follows, and in part will be obvious from the
description, or may be learned by practice of the aspects described
below. The advantages described below will be realized and attained
by means of the elements and combinations particularly pointed out
in the appended claims. It is to be understood that both the
foregoing general description and the following detailed
description are exemplary and explanatory only and are not
restrictive.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The accompanying figures, which are incorporated in and
constitute a part of this specification, illustrate several aspects
described below.
[0011] FIG. 1 is a schematic of a process for applying the
disclosed microencapsulated nutrients on to chips.
DETAILED DESCRIPTION
[0012] The materials, compounds, compositions, articles, and
methods described herein can be understood more readily by
reference to the following detailed description of specific aspects
of the disclosed subject matter and the Examples included therein
and to the FIGURE.
[0013] Before the present materials, compounds, compositions,
articles, and methods are disclosed and described, it is to be
understood that the aspects described below are not limited to
specific synthetic methods or specific reagents, as such may, of
course, vary. It is also to be understood that the terminology used
herein is for the purpose of describing particular aspects only and
is not intended to be limiting.
[0014] Also, throughout this specification, various publications
are referenced. The disclosures of these publications in their
entireties are hereby incorporated by reference into this
application in order to more fully describe the state of the art to
which the disclosed matter pertains. The references disclosed are
also individually and specifically incorporated by reference herein
for the material contained in them that is discussed in the
sentence in which the reference is relied upon.
[0015] In this specification and in the claims that follow,
reference will be made to a number of terms, which shall be defined
to have the following meanings:
[0016] Throughout the description and claims of this specification
the word "comprise" and other forms of the word, such as
"comprising" and "comprises," means including but not limited to,
and is not intended to exclude, for example, other additives,
components, integers, or steps.
[0017] As used in the description and the appended claims, the
singular forms "a", "an", and "the" include plural referents unless
the context clearly dictates otherwise. Thus, for example,
reference to "a compound" includes mixtures of two or more such
compounds, reference to "an omega-3 fatty acid" includes mixtures
of two or more such omega-3 fatty acids, reference to "the
microcapsule" includes mixtures of two or more such microcapsules,
and the like.
[0018] "Optional" or "optionally" means that the subsequently
described event or circumstance can or cannot occur, and that the
description includes instances where the event or circumstance
occurs and instances where it does not.
[0019] Ranges can be expressed herein as from "about" one
particular value, and/or to "about" another particular value. When
such a range is expressed, another aspect includes from the one
particular value and/or to the other particular value. Similarly,
when values are expressed as approximations, by use of the
antecedent "about," it will be understood that the particular value
forms another aspect. It will be further understood that the
endpoints of each of the ranges are significant both in relation to
the other endpoint, and independently of the other endpoint. It is
also understood that there are a number of values disclosed herein,
and that each value is also herein disclosed as "about" that
particular value in addition to the value itself. For example, if
the value "10" is disclosed, then "about 10" is also disclosed. It
is also understood that when a value is disclosed that "less than
or equal to" the value, "greater than or equal to the value" and
possible ranges between values are also disclosed, as appropriately
understood by the skilled artisan. For example, if the value "10"
is disclosed, then "less than or equal to 10" as well as "greater
than or equal to 10" is also disclosed. It is also understood that
throughout the application data are provided in a number of
different formats and that these data represent endpoints and
starting points and ranges for any combination of the data points.
For example, if a particular data point "10" and a particular data
point "15" are disclosed, it is understood that greater than,
greater than or equal to, less than, less than or equal to, and
equal to 10 and 15 are considered disclosed as well as between 10
and 15. It is also understood that each unit between two particular
units are also disclosed. For example, if 10 and 15 are disclosed,
then 11, 12, 13, and 14 are also disclosed.
[0020] References in the specification and concluding claims to
parts by weight of a particular element or component in a
composition denotes the weight relationship between the element or
component and any other elements or components in the composition
or article for which a part by weight is expressed. Thus, in a
compound containing 2 parts by weight of component X and 5 parts by
weight component Y, X and Y are present at a weight ratio of 2:5,
and are present in such ratio regardless of whether additional
components are contained in the compound.
[0021] A weight percent of a component, unless specifically stated
to the contrary, is based on the total weight of the formulation or
composition in which the component is included.
[0022] As used herein, by a "subject" is meant an individual. Thus,
the "subject" can include domesticated animals (e.g., cats, dogs,
etc.), livestock (e.g., cattle, horses, pigs, sheep, goats, etc.),
laboratory animals (e.g., mouse, rabbit, rat, guinea pig, etc.),
and birds. "Subject" can also include a mammal, such as a primate
or a human.
[0023] Reference will now be made in detail to specific aspects of
the disclosed materials, compounds, compositions, articles, and
methods, examples of which are illustrated in the accompanying
Examples and FIGURE.
[0024] Certain materials, compounds, compositions, and components
disclosed herein can be obtained commercially or readily
synthesized using techniques generally known to those of skill in
the art. For example, the starting materials and reagents used in
preparing the disclosed compounds and compositions are either
available from commercial suppliers such as Ocean Nutrition Canada
(Dartmouth, Nova Scotia), Aldrich Chemical Co., (Milwaukee, Wis.),
Acros Organics (Morris Plains, N.J.), Fisher Scientific
(Pittsburgh, Pa.), or Sigma (St. Louis, Mo.) or are prepared by
methods known to those skilled in the art following procedures set
forth in references such as Fieser and Fieser's Reagents for
Organic Synthesis, Volumes 1-17 (John Wiley and Sons, 1991); Rodd's
Chemistry of Carbon Compounds, Volumes 1-5 and Supplementals
(Elsevier Science Publishers, 1989); Organic Reactions, Volumes
1-40 (John Wiley and Sons, 1991); March's Advanced Organic
Chemistry, (John Wiley and Sons, 4th Edition); and Larock's
Comprehensive Organic Transformations (VCH Publishers Inc.,
1989).
[0025] Also, disclosed herein are materials, compounds,
compositions, and components that can be used for, can be used in
conjunction with, can be used in preparation for, or are products
of the disclosed methods and compositions. These and other
materials are disclosed herein, and it is understood that when
combinations, subsets, interactions, groups, etc. of these
materials are disclosed that while specific reference of each
various individual and collective combinations and permutation of
these compounds may not be explicitly disclosed, each is
specifically contemplated and described herein. For example, if a
compound is disclosed and a number of modifications that can be
made to a number of components of the compound are discussed, each
and every combination and permutation that are possible are
specifically contemplated unless specifically indicated to the
contrary. Thus, if a class of components A, B, and C are disclosed
as well as a class of components D, E, and F and an example of a
combination compound A-D is disclosed, then even if each is not
individually recited, each is individually and collectively
contemplated. Thus, in this example, each of the combinations A-E,
A-F, B-D, B-E, B-F, C-D, C-E, and C-F are specifically contemplated
and should be considered disclosed from disclosure of A, B, and C;
D, E, and F; and the example combination A-D. Likewise, any subset
or combination of these is also specifically contemplated and
disclosed. Thus, for example, the sub-group of A-E, B-F, and C-E
are specifically contemplated and should be considered disclosed
from disclosure of A, B, and C; D, E, and F; and the example
combination A-D. This concept applies to all aspects of this
disclosure including, but not limited to, steps in methods of
making and using the disclosed compositions. Thus, if there are a
variety of additional steps that can be performed it is understood
that each of these additional steps can be performed with any
specific aspect or combination of aspects of the disclosed methods,
and that each such combination is specifically contemplated and
should be considered disclosed.
Food Articles
[0026] Disclosed herein are food articles that comprise one or more
delivery devices. A delivery device, as is more fully described
herein, can contain a loading substance that is to be delivered to
a subject upon eating/drinking the food article. The disclosed food
articles can be any article that can be consumed (e.g., eaten,
drank, or ingested) by a subject. For example, the food article can
be a composition for human and animal consumption, including
foods/beverages for consumption by agricultural animals, pets and
zoo animals. It can be desired that the food article be a palatable
and popular food article. By using food articles that are widely
accepted, compliance with dietary or dosage regimens for the
loading substance can be increased.
[0027] Those of ordinary skill in the art of preparing and selling
food articles (i.e., edible foods or beverages, or precursors
thereof) are well aware of a large variety of classes, subclasses,
and species of food articles, and utilize well-known and recognized
terms of art to refer to those articles while endeavoring to
prepare and sell variations of those articles. Such a list of terms
of art is enumerated below, and it is specifically contemplated
hereby that the various delivery devices disclosed herein can be
used to deliver a loading substance to a subject by incorporating
the delivery device(s) into or on a food article as listed herein,
either singly or in all reasonable combinations or mixtures
thereof:
[0028] One or more confectioneries, chocolate confectionery,
tablets, countlines, bagged selflines/softlines, boxed assortments,
standard boxed assortments, twist wrapped miniatures, seasonal
chocolate, chocolate with toys, alfajores, other chocolate
confectionery, mints, standard mints, power mints, boiled sweets,
pastilles, gums, jellies and chews, toffees, caramels and nougat,
medicated confectionery, lollipops, liquorice, other sugar
confectionery, gum, chewing gum, sugarized gum, sugar-free gum,
functional gum, bubble gum, bread, packaged/industrial bread,
unpackaged/artisanal bread, pastries, cakes, packaged/industrial
cakes, unpackaged/artisanal cakes, cookies, chocolate coated
biscuits, sandwich biscuits, filled biscuits, savory biscuits and
crackers, bread substitutes, breakfast cereals, RTE (ready-to-eat)
cereals, family breakfast cereals, flakes, muesli, other RTE
cereals, children's breakfast cereals, hot cereals, sweet and
savory snacks, fruit snacks, chips/crisps, extruded snacks,
tortilla/corn chips, popcorn, pretzels, nuts, other sweet and
savory snacks, snack bars, granola bars, breakfast bars, energy
bars, fruit bars, other snack bars, meal replacement products,
slimming products, convalescence drinks, ready meals, canned ready
meals, frozen ready meals, dried ready meals, chilled ready meals,
dinner mixes, dessert mixes, frozen pizza, chilled pizza, soup,
canned soup, dehydrated soup, instant soup, chilled soup, frozen
soup, pasta, canned pasta, dried pasta, chilled/fresh pasta,
noodles, plain noodles, instant noodles, frozen noodles, cups/bowl
instant noodles, pouch instant noodles, chilled noodles, snack
noodles, canned food, canned meat and meat products, canned
fish/seafood, canned vegetables, canned tomatoes, canned beans,
canned fruit, canned ready meals, canned pasta, other canned foods,
frozen food, frozen processed red meat, frozen processed poultry,
frozen processed fish/seafood, frozen processed vegetables, frozen
meat substitutes, frozen potatoes, oven baked potato chips, other
oven baked potato products, non-oven frozen potatoes, frozen bakery
products, frozen desserts, other frozen food, dried food, chilled
processed meats, chilled fish/seafood products, chilled processed
fish, chilled coated fish, chilled smoked fish, chilled lunch kit,
chilled/fresh pasta, chilled noodles, oils and fats, olive oil,
vegetable and seed oil, cooking fats, butter, margarine, spreadable
oils and fats, functional spreadable oils and fats, sauces,
dressings and condiments, tomato pastes and purees, bouillon/stock
cubes, stock cubes, gravy granules, liquid stocks and fonds, herbs
and spices, fermented sauces, soy based sauces, pasta sauces, wet
sauces, dry sauces/powder mixes, ketchup, mayonnaise, regular
mayonnaise, mustard, salad dressings, regular salad dressings, low
fat salad dressings, vinaigrettes, dips, pickled products, other
sauces, dressings and condiments, spreads, jams and preserves,
honey, chocolate spreads, nut-based spreads, and yeast-based
spreads.
[0029] Some other specific examples of suitable food articles
include, but are not limited to, fruit, vegetable, meat, a grain
food, a starch food, a confectionery such as sweets (hard and soft
candy, jelly, jam, candy bar, etc.), gum, a baked confectionery or
molded confectionery (cookie, biscuit, etc.), a steamed
confectionery, a cacao or cacao product (chocolate and cocoa), a
frozen confectionery (ice cream, ices, etc.), a beverage (fruit
juice, soft drink, carbonated beverage, health drink), a health or
nutritional bar, baked good, pasta, a milk product, a cheese
product, an egg product, a condiment, a soup mix, a snack food, a
nut product, a plant protein product, a poultry product, a
granulated sugar (e.g., white or brown), a sauce, a gravy, a syrup,
a dry beverage powder, a fish product, or pet companion food. In
other examples, a suitable food article can include, but is not
limited to, bread, tortillas, cereal, sausage, chicken, ice cream,
yogurt, milk, salad dressing, rice bran, fruit juice, a dry
beverage powder, rolls, cookies, crackers, fruit pies, or cakes. In
some particular examples, the food article can be a chip (potato
chip, corn chip, tortilla chip, etc.), pretzel, cracker, and the
like. In still other examples, the food article can include, but is
not limited to, frozen foods (e.g., frozen vegetables). In a
further example, the food article is a salty, savory snack food
such as, for example, a rice cake or popcorn.
[0030] Further examples of food articles that can contain delivery
devices, as disclosed herein, can be the in the Wet Soup Category,
the Dehydrated and Culinary Food Category, the Beverage Category,
the Frozen Food Category, the Snack Food Category, and seasonings
or seasoning blends.
[0031] "Wet Soup Category" means wet/liquid soups regardless of
concentration or container, including frozen soups. For the purpose
of this definition soup(s) means a food prepared from meat,
poultry, fish, vegetables, grains, fruit and other ingredients,
cooked in a liquid, which may include visible pieces of some or all
of these ingredients. It may be clear (as a broth) or thick (as a
chowder), smooth, pureed or chunky, ready-to-serve, semi-condensed
or condensed and can be served hot or cold, as a first course or as
the main course of a meal or as a between meal snack (sipped like a
beverage). Soup can be used as an ingredient for preparing other
meal components and can range from broths (consomme) to sauces
(cream or cheese-based soups).
[0032] "Dehydrated and Culinary Food Category" means: (i) Cooking
aid products such as: powders, granules, pastes, concentrated
liquid products, including concentrated bouillon, bouillon and
bouillon like products in pressed cubes, tablets or powder or
granulated form, which are sold separately as a finished product or
as an ingredient within a product, sauces and recipe mixes
(regardless of technology); (ii) Meal solutions products such as:
dehydrated and freeze dried soups, including dehydrated soup mixes,
dehydrated instant soups, dehydrated ready-to-cook soups,
dehydrated or ambient preparations of ready-made dishes, meals and
single serve entrees including pasta, potato and rice dishes; and
(iii) Meal embellishment products such as: condiments, marinades,
salad dressings, salad toppings, dips, breading, batter mixes,
shelf stable spreads, barbecue sauces, liquid recipe mixes,
concentrates, sauces or sauce mixes, including recipe mixes for
salad, sold as a finished product or as an ingredient within a
product, whether dehydrated, liquid or frozen.
[0033] "Beverage Category" means beverages, beverage mixes, and
concentrates including, but not limited to, alcoholic and
non-alcoholic beverages, ready to drink and dry powdered beverages,
carbonated and non-carbonated beverages, e.g., sodas, fruit or
vegetable juices.
Homogenized Formulations
[0034] Also disclosed herein are methods for preparing a
homogenized formulation that comprises providing a pre-homogenized
composition comprising one or more delivery devices (e.g.,
microcapsules) and homogenizing the composition. In these methods,
the delivery devices are present in the pre-homogenized composition
prior to homogenization. Thus, when the pre-homogenized composition
undergoes homogenization, as disclosed herein, the delivery devices
are present during and subjected to the homogenization process.
Further, in many examples disclosed herein the homogenized
formulations are further processed (e.g., pasteurized/sterilized).
Thus, the disclosed homogenized formulations can also be
pasteurized or sterilized formulations. In many examples, the
disclosed homogenized formulations can be incorporated into (e.g.,
used to prepare) many of the food articles disclosed herein. For
example, disclosed herein are combinations of food articles and
homogenized formulations.
[0035] In the disclosed homogenized formulations, the amount of
delivery devices in a homogenized formulation can be at least 50%
of the amount of delivery devices in a pre-homogenized composition.
In other examples, the amount of delivery devices in a homogenized
formulation can be at least about 55, 60, 65, 70, 75, 80, 85, 90,
95, 97, 98, or 99% of the amount of delivery devices in a
pre-homogenized composition, where any of the stated values can
form an upper or lower endpoint of a range. The amount of delivery
devices in the disclosed homogenized formulations and
pre-homogenized compositions can be determined by methods known in
the art (for example, see the Examples disclosed herein).
[0036] The disclosed homogenized formulations and methods have
certain advantages over many existing compositions. For example, by
having delivery devices present in the "crude" starting material
(i.e., prior to homogenization and, in some cases, prior to other
processing techniques such as pasteurization or sterilization), a
plant's existing processing streams can be used, thus avoiding
costly modifications to most existing designs where pasteurization
is performed directly before or after homogenization. Another
advantage is that the delivery devices are subjected to the
homogenization process (and, in other examples, pasteurization and
sterilization processes as well). This can avoid regulatory issues
that surround methods where delivery devices (or other additives)
are added after pasteurization/sterilization, which usually require
that the product be re-pasteurized or re-sterilized.
[0037] Further advantages of certain homogenized formulations
(e.g., dairy formulations) and methods disclosed herein can include
a narrower particle size distribution of the delivery devices in
the homogenized formulations as compared to formulations where the
delivery devices were added after homogenization and thus not
homogenized. Also, when the homogenized formulations are
pasteurized, as is typically done for dairy products, milk proteins
can assemble around the outer shell of the delivery devices during
pasteurization. The degree and amount of assembly is believed to be
dependent on the time and temperature of pasteurization. The
assembly of the milk proteins (e.g. whey proteins and caesins) can
improve the flavor of the formulation, since such proteins are
known to be good absorbers of certain flavors and odors. Also, the
associated milk proteins can provide further stability to the
delivery devices and their contents.
[0038] In the disclosed methods, the pre-homogenized composition
can be any fluid that is to be homogenized. Thus, the disclosed
methods are not intended to be limited in any way by the particular
pre-homogenized compositions. For example, the pre-homogenized
composition can be any comestible, cosmetic, pharmaceutical,
nutritional, or health care product that is to be homogenized. In
certain specific examples, the pre-homogenized composition can be a
dairy product (e.g., milk).
[0039] It is understood that suitable pre-homogenized compositions
can have already been homogenized one or more times before. As long
as these compositions are to be homogenized at least once again,
they are acceptable pre-homogenized compositions for the disclosed
methods.
[0040] The pre-homogenized can also be either pasteurized or
un-pasteurized. For example, a dairy composition that is
pasteurized, but has yet to be homogenized, is a suitable
pre-homogenized composition. Also, a dairy composition that has yet
to be either homogenized or pasteurized (in any order) is a
suitable pre-homogenized composition.
[0041] The disclosed pre-homogenized compositions, as well as the
resulting homogenized formulations and food articles provided
therefrom, can comprise one or more delivery devices, as described
herein. In some examples the disclosed pre-homogenized compositions
and resulting homogenized formulations can comprise the same type
of delivery devices and, in other examples, different types of
delivery devices (e.g., microcapsules containing different loading
substances).
[0042] Some specific examples of homogenized formulations disclosed
herein comprise microcapsules having about 130 mg of DHA per gram
of microcapsule (e.g., a microcapsule wherein the loading substance
comprises a 5:25 oil derived from tuna and/or bonito) and the outer
shell of the microcapsules comprises pork or fish gelatin. In
another specific example, the homogenized formulations disclosed
herein comprise a microcapsule having about 150 mg of DHA and EPA
per gram of microcapsule (e.g., a microcapsule wherein the loading
substance comprises a 18:12 oil derived from sardine and/or
anchovy) and the outer shell of the microcapsules comprises pork or
fish gelatin. Any of these formulations can be infant formula,
milk, or yogurt formulations for example.
[0043] Any of the disclosed delivery devices can be added to any of
the disclosed pre-homogenized compositions. The particular method
of addition will depend on the particular pre-homogenized
composition, the particular delivery devices, the homogenized
composition, including its end use and methods and apparatus of
preparation, as well as preference. The disclosed methods are not
intended to be limited by any particular method of adding
microcapsules to the pre-homogenized composition. In some example,
the delivery devices are manually added or poured into the
pre-homogenized composition (or added to a homogenized composition
that is to be homogenized again). In other example, the delivery
devices or solutions thereof can be pumped into the pre-homogenized
compositions or added via a hopper. Other suitable methods of
adding the delivery devices into the pre-homogenized composition
are known in the art. Further, mixing can be also be desired in
order to fully incorporate the delivery devices into the
pre-homogenized compositions. Such mixing can also be accomplished
by methods known in the art such as, but not limited to, mechanical
stirrers, magnetic stirrers, shakers, bubbling gas, sonication,
vortexing, and the like.
[0044] The particular amount of delivery devices that can be
present in the pre-homogenized compositions will depend on the
preference and the particular end use of the homogenized
formulations. For example, if one desires or requires a particular
amount delivery devices in the homogenized formulations disclosed
herein, then about the same amount can be present in or added to
the pre-homogenized compositions. Specific examples of amounts of
delivery devices in homogenized dairy formulations, for example,
can be from about 0.005% to about 25%, from about 0.01% to about
20%, from about 0.05% to about 18%, from about 0.1% to about 16%,
from about 1% to about 10%, by weight of the total composition.
Other examples can include formulations containing from about 0.005
to about 5%, from about 0.01 to about 5%, or from about 0.1 to
about 5% delivery devices by weight of the total composition. In
still other examples, the disclosed homogenized formulations can
contain about 0.005, 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, 5, 6, 7, 8,
9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, or
25% delivery devices by weight of the total composition, where any
of the stated values can form an upper or lower endpoint when
appropriate.
[0045] In the disclosed methods, the pre-homogenized compositions
are homogenized. Any homogenization technique and apparatus known
in the art can be used in the disclosed methods. Such
homogenization techniques and apparatuses are commonly used in, for
example, the food, dairy, pharmaceutical, cosmetic, and fragrance
industries. Many suitable homogenizers are commercially available.
Homogenization can involve the use of sonication, pressure, and/or
mechanical devices to homogenize the fluid. For example, the
homogenization can be a single stage homogenization, a multi-step
or multi-stage homogenization (e.g., a two-stage homogenization), a
high pressure homogenization (e.g., single or multi-stage high
pressure homogenizations), a very-high pressure homogenization, a
rotator-stator homogenization, a blade homogenization, and the
like.
[0046] In some examples, the homogenization step can be a
pressure-based homogenization technique operating at pressures of
from about 200 to about 15,000 psi, from about 500 to about 12,000
psi, from about 1,000 to about 9,000 psi, or from about 3,000 to
about 6,000 psi. In still other examples, the homogenization step
can be performed at about 200, 500, 1000, 1500, 2000, 2500, 3000,
3500, 4000, 4500, 5000, 5500, 6000, 6500, 7000, 7500, 8000, 8500,
9000, 9500, 10000, 10500, 11000, 11500, or 12000, 12500, 13000,
13500, 14000, 14500, 15000, where any of the stated values can form
an upper or lower endpoint. It is further contemplated that
multiple passes of homogenization at any of these pressures can be
used, including combinations thereof.
[0047] After homogenization, the disclosed homogenized formulations
can undergo further processing. For example, the homogenized
formulations can be sterilized or pasteurized. Examples of
typically pasteurization conditions are high temperature short time
pasteurization (HTST), ultra pasteurization (UP), and ultra high
temperature (UHT) pasteurization. The homogenized formulations can
also be further processed after homogenization by, e.g., the
addition of additives, further formulation into the final product,
packaged, spray dried, etc. In some examples, the homogenized
formulations can be steam injected. Steam injection is a known
technique that is sometimes used in the dairy industry. Generally,
steam is injected into the milk to remove odors produced when the
moisture is flashed off during pasteurization. This process is
typically used on milks that are UHT pasteurized.
[0048] It is also contemplated that the pre-homogenized
compositions comprising one or more microcapsules can be processed
prior to homogenization. For example, such pre-homogenized
compositions comprising one or more microcapsules can first be
sterilized or pasteurized and then homogenized. Likewise, the
pre-homogenized compositions comprising one or more microcapsules
can be subject to other processing steps prior to homogenization
(e.g., the addition of additives, etc.).
[0049] The disclosed homogenized formulations have many and varied
uses. Any current use of a homogenized fluid can also be suitable
for the disclosed homogenized formulations. For comestible
formulations, the homogenized formulations disclosed herein can
generally be taken orally and can be in any form suitable for oral
administration. For example, the homogenized formulation can be
spray dried and then formed into a tablet or provided in a sachet.
Alternatively, the homogenized formulations can be incorporated
into gel-caps, capsules, liquids, syrups, ointments, lotions,
creams, gels, or drops.
[0050] The homogenized formulations can also be designed for humans
or animals, based on the recommended dietary intake for a given
individual. Such considerations are generally based on various
factors such as species, age, and sex as described above, which are
known or can be determined by one of skill in the art. In one
example, the disclosed formulations can be used as a component of
feed for animals such as, but not limited to, livestock (e.g.,
pigs, chickens, cows, goats, horses, and the like), and domestic
pets (e.g., cats, dogs, birds, and the like).
[0051] The disclosed homogenized formulations can also include
additional carriers, as well as flavorings, thickeners, diluents,
buffers, preservatives, surface active agents, emulsifiers,
dispersing aids, or binders and the like in addition to the
microcapsules disclosed herein.
[0052] Other examples of homogenized formulations or products
derived therefrom than can be prepared by the methods disclosed
herein include fresh/pasteurized milk, full fat fresh/pasteurized
milk, semi skimmed fresh/pasteurized milk, long-life/UHT milk, full
fat long life/UHT milk, semi skimmed long life/UHT milk, fat-free
long life/UHT milk, goat milk, condensed/evaporated milk, plain
condensed/evaporated milk, flavored, functional and other condensed
milk, flavored milk drinks, dairy only flavored milk drinks,
flavored milk drinks with fruit juice, soy milk, sour milk drinks,
fermented dairy drinks, coffee whiteners, powder milk, flavored
powder milk drinks, cream, cheese, processed cheese, spreadable
processed cheese, unspreadable processed cheese, unprocessed
cheese, spreadable unprocessed cheese, hard cheese, packaged hard
cheese, unpackaged hard cheese, yogurt, plain/natural yogurt,
flavored yogurt, fruited yogurt, probiotic yogurt, drinking yogurt,
regular drinking yogurt, probiotic drinking yogurt, chilled snacks,
fromage frais and quark, plain fromage frais and quark, flavored
fromage frais and quark, and kifer.
[0053] Alternatively, the disclosed homogenized formulations can be
prepared in a powdered form (e.g., via spray drying or dehydration)
and contained in articles such as sachets or shakers, which can be
used to pour or sprinkle the disclosed compositions onto and into
food and beverages. Still other examples include baked goods (e.g.,
breads, rolls, cookies, crackers, fruit pies, or cakes), pastas,
condiments, salad dressings, soup mixes, snack foods, processed
fruit juices, sauces, gravies, syrups, beverages, dry beverage
powders, jams or jellies, or pet companion food that have been
prepared with a homogenized formulation as disclosed herein.
Delivery Devices
[0054] Examples of delivery devices that can be used in the
disclosed food articles and methods include, but are not limited
to, microcapsules, microspheres, nanospheres or nanoparticles,
liposomes, noisome, emulsions, or powders.
[0055] Loading substances, as are described more fully herein, can
be incorporated into liposomes. As is known in the art, liposomes
are generally derived from phospholipids or other lipid substances.
Liposomes are formed by mono- or multi-lamellar hydrated liquid
crystals that are dispersed in an aqueous medium. Any non-toxic,
physiologically acceptable and metabolizable lipid capable of
forming liposomes can be used. The liposome can also contain
stabilizers, preservatives, excipients, and the like. Examples of
suitable lipids are the phospholipids and the phosphatidyl cholines
(lecithins), both natural and synthetic. Methods of forming
liposomes are known in the art. See e.g., Prescott, Ed., Methods in
Cell Biology, Volume XIV, Academic Press, New York, p. 33 et seq.,
1976, which is hereby incorporated by reference herein for its
teachings of liposomes and their preparation. In other examples,
the liposomes can be cationic liposomes (e.g., DOTMA, DOPE, DC
cholesterol) or anionic liposomes.
[0056] As described herein, niosomes are delivery devices that can
be used to deliver a loading substance as disclosed herein.
Noisomes are multilamellar or unilamellar vesicles involving
non-ionic surfactants.
[0057] Solid-lipid nanoparticles, as described herein, are other
delivery devices that can be used to deliver a loading substance as
disclosed herein. Solid-lipid nanoparticles are nanoparticles,
which are dispersed in an aqueous surfactant solution. They are
comprised of a solid hydrophobic core having a monolayer of a
phospholipid coating and are usually prepared by high-pressure
homogenization techniques.
[0058] Microcapsules
[0059] Microcapsules, as described herein, are yet further examples
of delivery devices that can be used in the disclosed food articles
and methods as disclosed herein. In contrast to liposomal delivery
systems, microcapsules (including microspheres) typically do not
have an aqueous core but a solid polymer matrix or membrane. These
delivery devices are obtained by controlled precipitation of
polymers, chemical cross-linking of soluble polymers, and
interfacial polymerization of two monomers or high-pressure
homogenization techniques. The encapsulated compound (i.e., loading
substance) is gradually released from the depot by erosion or
diffusion from the particles. Successful formulations of short
acting peptides, such as LHRH agonists like leuprorelin and
triptoreline, have been developed. Poly(lactide co-glycolide)
(PLGA) microspheres are currently used as monthly and three monthly
dosage forms in the treatment of advanced prostrate cancer,
endometriosis, and other hormone responsive conditions. Leuprolide,
an LHRH superagonist, was incorporated into a variety of PLGA
matrices using a solvent extraction/evaporation method. As noted,
all of these delivery devices can be used in the food articles and
methods disclosed herein.
[0060] The use of microcapsules can protect certain compositions
from oxidation and degradation, keeping the loading substance
fresh. Also, because microcapsules can hide the unpleasant odor or
taste of certain compositions, the food articles and methods
disclosed herein can be particularly useful for delivering and
supplementing unpleasant compositions. Still further, the use of
microcapsules can allow various loading substances to be added to
food articles which are otherwise not amenable to supplementation.
For example, omega-3 fatty acids can degrade or oxidize in air and
can be sensitive to food preparation techniques (e.g., baking). By
the use microencapsulated omega-3 fatty acids, these compositions
can be added to food without significant degradation during food
preparation.
[0061] Microcapsules that are suitable for use in the disclosed
food articles are defined as small particles of solids, or droplets
of liquids, inside a thin coating of a shell material such as
beeswax, starch, gelatine, or polyacrylic acid. They are used, for
example, to prepare liquids as free-flowing powders or compressed
solids, to separate reactive materials, to reduce toxicity, to
protect against oxidation and/or to control the rate of release of
a substance such as an enzyme, a flavor, a nutrient, a drug,
etc.
[0062] Over the past fifty years, much focus has been on so-called
"single-core" microcapsules. However, one of the problems with
single-core microcapsules is their susceptibility to rupture. To
increase the strength of microcapsules, the thickness of the
microcapsule wall can be increased. However, this can lead to a
reduction in the loading capacity of the microcapsule. Another
approach has been to create so-called "multi-core" microcapsules.
For example, U.S. Pat. No. 5,780,056 discloses a "multi-core"
microcapsule having gelatine as a shell material. These
microcapsules are formed by spray cooling an aqueous emulsion of
oil or carotenoid particles such that the gelatine hardens around
"cores" of the oil or carotenoid particles. Yoshida et al.
(Chemical Abstract 1990:140735 or Japanese Patent Publication JP
01-148338) discloses a complex coacervation process for the
manufacture of microcapsules in which an emulsion of gelatine and
paraffin wax is added to an arabic rubber solution and then mixed
with a surfactant to form "multi-core" microcapsules. Ijichi et al.
(J. Chem. Eng. Jpn. (1997) 30(5):793-798) microencapsulated large
droplets of biphenyl using a complex coacervation process to form
multi-layered microcapsules. U.S. Pat. Nos. 4,219,439 and 4,222,891
disclose "multi-nucleus," oil-containing microcapsules having an
average diameter of about 3 to about 20 .mu.m with an oil droplet
size of about 1 to about 10 .mu.m for use in pressure-sensitive
copying papers and heat sensitive recording papers.
[0063] Particularly suitable microcapsules include those that are
resistant to rupture during the preparation of the food article
(including packaging, transportation, and storage of the food
article). In some examples, the microcapsules can be of a size and
consistency that does not detract from the texture and constitution
of the food article.
[0064] Microcapsules suitable for use in the disclosed articles and
methods can be any microcapsule as disclosed herein. In specific
examples, the microcapsules can comprise an agglomeration of
primary microcapsules and a loading substance. Each individual
primary microcapsule has a primary shell. The loading substance is
encapsulated by the primary shell and the agglomeration is
encapsulated by an outer shell. These microcapsules are referred to
herein as "multicore microcapsules." In another example, described
herein are microcapsules that comprise a loading substance, a
primary shell, and a secondary shell, wherein the primary shell
encapsulates the loading substance and the secondary shell
encapsulates the composition and primary shell. These microcapsules
are referred to herein as "single-core microcapsules." Unless
stated otherwise, the term "microcapsule" is used herein to refer
to multicore, single-core, or a mixture of multicore and
single-core microcapsules. Particularly suitable microcapsules are
disclosed in U.S. Pat. Nos. 6,974,592 and 6,969,530 and US
Publication No. 2005-0019416-A1, which are all incorporated by
reference herein in their entireties for at least their disclosures
of microcapsules, their methods of preparation, and their methods
of use.
[0065] The microcapsules disclosed herein generally have a
combination of high payload and structural strength. For example,
the disclosed microcapsules are strong enough to survive the
homogenization process. Further, the payloads of loading substances
in the disclosed microcapsules can be from about 20% to about 90%,
about 50% to about 70% by weight, or about 60% by weight of the
microcapsule. In other examples, the disclosed microcapsules can
contain about 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80,
85, or 90% by weight of the microcapsule, where any of the stated
values can form an upper or lower endpoint when appropriate.
[0066] It is also contemplated that one or more additional shell
layers can be placed on the outer shell of the microcapsules. The
techniques described in International Publication No. WO
2004/041251 A1, which is incorporated by reference in its entirety,
can be used to add additional shell layers to the
microcapsules.
[0067] A number of different polymers can be used to produce the
shell layers of the single-core and multicore microcapsules. For
example, the primary shell and/or outer shell material of the
disclosed microcapsules can comprise a surfactant, gelatin,
protein, polyphosphate, polysaccharide, or mixtures thereof.
Further examples of suitable materials for the primary shell and/or
outer shell include, but are not limited to, gelatin type A,
gelatin type B, polyphosphate, gum arabic, alginate, chitosan,
carrageenan, pectin, starch, modified starch, alfa-lactalbumin,
beta-lactoglobumin, ovalbumin, polysorbiton, maltodextrin,
cyclodextrin, cellulose, methyl cellulose, ethyl cellulose,
hydropropylmethylcellulose, carboxymethylcellulose, milk protein,
whey protein, soy protein, canola protein, albumin, chitin,
polylactides, poly-lactide-co-glycolides, derivatized chitin,
poly-lysine, kosher gelatin, non-kosher gelatin, Halal gelatin, and
non-Halal gelatin, including combinations and mixtures thereof. It
is also contemplated that derivatives of these polymers can be used
as well. One specific type of primary shell and/or outer shell
material that can be used in the disclosed microcapsules is fish
gelatin or pork gelatin.
[0068] In many examples of suitable microcapsules, the primary
shell and/or outer shell material can have a Bloom number of from
about 0 to about 350. The Bloom number describes the gel strength
formed at 10.degree. C. with a 6.67% solution gelled for 18 hours.
Determining the Bloom number of a substance can be accomplished by
methods known in the art. It is contemplated that the primary shell
and/or outer shell material can have a Bloom number of about 0, 1,
2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20,
21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37,
38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54,
55, 56, 57, 58, 59, 60, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70,
70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 80, 81, 82, 83, 84, 85,
86, 87, 88, 89, 90, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, 100,
100, 101, 102, 103, 104, 105, 106, 107, 108, 109, 110, 110, 111,
112, 113, 114, 115, 116, 117, 118, 119, 120, 120, 121, 122, 123,
124, 125, 126, 127, 128, 129, 130, 130, 131, 132, 133, 134, 135,
136, 137, 138, 139, 140, 140, 141, 142, 143, 144, 145, 146, 147,
148, 149, 150, 150, 151, 152, 153, 154, 155, 156, 157, 158, 159,
160, 160, 161, 162, 163, 164, 165, 166, 167, 168, 169, 170, 170,
171, 172, 173, 174, 175, 176, 177, 178, 179, 180, 180, 181, 182,
183, 184, 185, 186, 187, 188, 189, 190, 190, 191, 192, 193, 194,
195, 196, 197, 198, 199, 200, 200, 201, 202, 203, 204, 205, 206,
207, 208, 209, 210, 210, 211, 212, 213, 214, 215, 216, 217, 218,
219, 220, 220, 221, 222, 223, 224, 225, 226, 227, 228, 229, 230,
230, 231, 232, 233, 234, 235, 236, 237, 238, 239, 240, 240, 241,
242, 243, 244, 245, 246, 247, 248, 249, 250, 250, 251, 252, 253,
254, 255, 256, 257, 258, 259, 260, 260, 261, 262, 263, 264, 265,
266, 267, 268, 269, 270, 270, 271, 272, 273, 274, 275, 276, 277,
278, 279, 280, 280, 281, 282, 283, 284, 285, 286, 287, 288, 289,
290, 290, 291, 292, 293, 294, 295, 296, 297, 298, 299, 300, 300,
301, 302, 303, 304, 305, 306, 307, 308, 309, 310, 310, 311, 312,
313, 314, 315, 316, 317, 318, 319, 320, 320, 321, 322, 323, 324,
325, 326, 327, 328, 329, 330, 330, 331, 332, 333, 334, 335, 336,
337, 338, 339, 340, 340, 341, 342, 343, 344, 345, 346, 347, 348,
349, or 350, where any of the stated values can form an upper or
lower end point where appropriate. In some specific examples the
primary and/or outer shell material can have a Bloom number of from
about 0 to about 50, and in other examples the primary and/or outer
shell material can have a Bloom number of from about 51 to about
350. Still other specific examples include microcapsules comprising
a primary shell and/or outer shell material having a Bloom number
of about 0, about 210, about 220, or about 240. In one example, the
microcapsule does not contain "low Bloom" gelatine, which is
gelatin having a Bloom number less than 50.
[0069] The shell material can be a two-component system made from a
mixture of different types of polymer components. In other
examples, the shell material can be a complex coacervate between
two or more polymer components (e.g., gelatine A and
polyphosphate). Component A can be gelatine type A, although other
polymers like those mentioned above for the shell materials are
also contemplated as component A. Component B can be gelatine type
B, polyphosphate, gum arabic, alginate, chitosan, carrageenan,
pectin, carboxymethyl-cellulose or a mixture thereof. Again other
polymers like those disclosed above for the shell materials are
also contemplated as component B. The molar ratio of component
A:component B that is used depends on the type of components but is
typically from about 1:5 to about 15:1. For example, when gelatine
type A and polyphosphate are used as components A and B
respectively, the molar ratio of component A:component B can be
about 8:1 to about 12:1; when gelatine type A and gelatine type B
are used as components A and B respectively, the molar ratio of
component A:component B can be about 2:1 to about 1:2; and when
gelatine type A and alginate are used as components A and B
respectively, the molar ratio of component A:component B can be
about 3:1 to about 5:1. In many of the disclosed microcapsules the
primary shell and/or outer shell can comprise a complex coacervate.
For example, the primary shell and/or outer shell can comprise a
complex coacervate of gelatin and polyphosphate.
[0070] In the disclosed microcapsules the outer shell can have an
average diameter of from about 1 .mu.m to about 2,000 .mu.m, from
about 20 .mu.m to about 1,000 .mu.m, or from about 30 .mu.m to
about 80 .mu.m. In further examples, the average diameter of the
outer shell can be about 1, 10, 20, 30, 40, 50, 60, 70, 80, 90,
200, 300, 400, 500, 600, 700, 800, 900, 1000, 1200, 1300, 1400,
1500, 1600, 1700, 1800, 1900, or 2000 .mu.m, where any of the
stated values can form an upper or lower endpoint when
appropriate.
[0071] The primary shells of the disclosed microcapsules can have
an average diameter of from about 40 nm to about 10 .mu.m or from
about 0.1 .mu.m to about 5 .mu.m. In further examples, the average
diameter of the primary shell can be about 40 nm, 50 nm, 60 nm, 70
nm, 80 nm, 90 nm, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm,
700 nm, 800 nm, 900 nm, 1000 nm, 2 .mu.m, 3 .mu.m, 4 .mu.m, 5
.mu.m, 6 .mu.m, 7 .mu.m, 8 .mu.m, 9 .mu.m, 10 .mu.m, where any of
the stated values can form an upper or lower endpoint when
appropriate.
[0072] Particle size can be measured using any typical equipment
known in the art, for example, a Coulter LS230 Particle Size
Analyzer, Miami, Fla., USA.
[0073] Loading Substances
[0074] In the disclosed delivery devices, the loading substance can
be any substance that one desires to be delivered to a subject. In
many examples, a suitable loading substance is not entirely soluble
in an aqueous mixture. The loading substance can be a solid, a
hydrophobic liquid, or a mixture of a solid and a hydrophobic
liquid. In many of the examples herein, the loading substance can
comprise a long chain polyunsaturated fatty acid, specific examples
of which are included below. Further, the loading substance can
comprise a biologically active substance, a nutrient such as a
nutritional supplement, a flavoring substance, a polyunsaturated
fatty acid like an omega-3 fatty acid, a vitamin, a mineral, a
carbohydrate, a steroid, a trace element, and/or a protein, and the
like including mixtures and combinations thereof. In other
examples, the loading substance can comprise microbial oil, algal
oil (e.g., oil from a dinoflagellate such as Crypthecodinium
cohnii), fungal oil (e.g., oil from Thraustochytrium,
Schizochytrium, or a mixture thereof), and/or plant oil (e.g.,
flax, vegetables), including mixtures and combinations thereof. In
other examples, the loading substance can be a pharmaceutical
composition (e.g., a drug and/or an enzyme) or a flavor. The
loading substance can also be a hydrophobic liquid, such as grease,
oil or a mixture thereof. Typical oils can be fish oils, vegetable
oils (e.g., canola, olive, corn, rapeseed), mineral oils,
derivatives thereof or mixtures thereof. The loading substance can
comprise a purified or partially purified oily substance such as a
fatty acid, a triglyceride, or a mixture thereof.
[0075] In still other examples, a suitable loading substance can
comprise marine oil, such as natural and refined and concentrated
fish oil. Examples of suitable fish oils include, but are not
limited to, Atlantic fish oil, Pacific fish oil, Mediterranean fish
oil, light pressed fish oil, alkaline treated fish oil, heat
treated fish oil, light and heavy brown fish oil, bonito oil,
pilchard oil, tuna oil, sea bass oil, halibut oil, spearfish oil,
barracuda oil, cod oil, menhaden oil, sardine oil, anchovy oil,
capelin oil, Atlantic cod oil, Atlantic herring oil, Atlantic
mackerel oil, Atlantic menhaden oil, salmonid oil, and shark oil,
including mixtures and combinations thereof. Non-alkaline treated
fish oil is also a suitable loading substance. Other marine oils
suitable for use herein include, but are not limited to, squid oil,
cuttle fish oil, octopus oil, krill oil, seal oil, whale oil, and
the like, including mixtures and combinations thereof. Any marine
oil and combination of marine oil can be used in the disclosed
delivery devices and in the disclosed food articles and
methods.
[0076] Many of the microbial, algal, fungal, plant, and marine oils
disclosed herein contain omega-3 fatty acids. As such, certain
delivery devices disclosed herein can contain a loading substance
that comprises an omega-3 fatty acid, an alkyl ester of an omega-3
fatty acid, a triglyceride ester of an omega-3 fatty acid, a
phytosterol ester of an omega-3 fatty acid, and/or mixtures and
combinations thereof. An omega-3 fatty acid is an unsaturated fatty
acid that contains as its terminus CH.sub.3--CH.sub.2--CH.dbd.CH--.
Generally, an omega-3 fatty acid has the following formula:
##STR00001##
wherein R.sup.1 is a C.sub.3-C.sub.40 alkyl or alkenyl group
comprising at least one double bond and R.sup.2 is H or alkyl
group. The term "alkane" or "alkyl" as used herein is a saturated
hydrocarbon group (e.g., methyl, ethyl, n-propyl, isopropyl,
n-butyl, isobutyl, s-butyl, t-butyl, n-pentyl, isopentyl, s-pentyl,
neopentyl, hexyl, heptyl, octyl, nonyl, decyl, dodecyl, tetradecyl,
hexadecyl, eicosyl, tetracosyl, and the like). The term "alkene" or
"alkenyl" as used herein is a hydrocarbon group containing at least
one carbon-carbon double bond. Asymmetric structures such as
(AB)C.dbd.C(CD) are intended to include both the E and Z isomers
(cis and trans). In a further example, R.sup.1 can be a
C.sub.5-C.sub.38, C.sub.6-C.sub.36, C.sub.8-C.sub.34,
C.sub.10-C.sub.32, C.sub.12-C.sub.30, C.sub.14-C.sub.28,
C.sub.16-C.sub.26, or C.sub.18-C.sub.24 alkenyl group. In yet
another example, the alkenyl group of R.sup.1 can have from 2 to 6,
from 3 to 6, from 4 to 6, or from 5 to 6 double bonds. Still
further, the alkenyl group of R.sup.1 can have from 1, 2, 3, 4, 5,
or 6 double bonds, where any of the stated values can form an upper
or lower endpoint as appropriate.
[0077] Specific examples of omega-3 fatty acids that are suitable
loading substances that can be used in the disclosed delivery
devices include, but are not limited to, .alpha.-linolenic acid
(18:3.omega.3), octadecatetraenoic acid (18:4.omega.3),
eicosapentaenoic acid (20:5.omega.3) (EPA), eicosatetraenoic acid
(20:4.omega.3), henicosapentaenoic acid (21:5.omega.3),
docosahexaenoic acid (22:6.omega.3) (DHA), docosapentaenoic acid
(22:5.omega.3) (DPA), including derivatives and mixtures thereof.
Many types of fatty acid derivatives are well known to one skilled
in the art. Examples of suitable derivatives are esters, such as
phytosterol esters, furanoid esters, branched or unbranched
C.sub.1-C.sub.30 alkyl esters, branched or unbranched
C.sub.2-C.sub.30 alkenyl esters or branched or unbranched
C.sub.3-C.sub.30 cycloalkyl esters, in particular phytosterol
esters and C.sub.1-C.sub.6 alkyl esters. In a further example, the
loading substance can be a phytosterol ester of docosahexaenoic
acid and/or eicosapentaenoic acid, a C.sub.1-C.sub.6 alkyl ester of
docosahexaenoic acid and/or eicosapentaenoic acid, a triglyceride
ester of docosahexaenoic acid and/or eicosapentaenoic acid, and/or
a mixture thereof.
[0078] Other examples of suitable loading substances that can be
present in the disclosed delivery devices comprise at least 4, at
least 6, at least 8, at least 10, at least 12, at least 14, at
least 16, at least 18, or at least 20 carbon atoms. In some other
examples, the loading substance can contain about 8, 9, 10, 11, 12,
13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29,
30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, or 45
carbon atoms, where any of the stated values can form an upper or
lower endpoint when appropriate. In still other examples, the
loading substance can comprise a mixture of fatty acids (including
derivatives thereof) having a range of carbon atoms. For example,
the loading substance can comprise from about 8 to about 40, from
about 10 to about 38, from about 12 to about 36, from about 14 to
about 34, from about 16 to about 32, from about 18 to about 30, or
from about 20 to about 28 carbon atoms.
[0079] Some further examples of loading substances are those that
contain at least one unsaturated bond (i.e., a carbon-carbon double
or triple bond). For example, the loading substance can contain at
least 2, at least 3, at least 4, at least 5, at least 6, at least
7, or at least 8 carbon-carbon double bonds, triple bonds, or any
combination thereof. In another example, the loading substance can
comprise 1, 2, 3, 4, 5, 6, 7, or 8 unsaturated bonds, where any of
the stated values can form an upper or lower endpoint as
appropriate.
[0080] Some specific examples of loading substances, which are
unsaturated fatty acids, are shown in the following tables.
Derivatives of these fatty acids are also suitable and are thus
contemplated herein.
TABLE-US-00001 TABLE 1 Examples of Monoene Acids Total number of
Carbon number where double bond begins. carbon atoms in the ("c"
denotes a cis double bond; "t" denotes fatty acid chain a trans
double bond) 10 4c 12 4c 14 4c and 9c 16 3t, 4c, 5t, 6c, 6t, 9c
(palmitooleic), and 11c 18 3t, 5c, 5t, 6c (petroselinic), 6t, 9c
(oleic), 10c, 11c (cis-vaccenic), 11t (vaccenic), and 13c 20 5c, 9c
(gadolenic), 11c, 13c, and 15c 22 5c, 11c (cetoleic), 13c (erucic),
and 15c 24 15c (selacholeic, nervonic) 26 9c, and 17c (ximenic) 28
9c, 19c (lumequic) 30 21c
[0081] Unsaturated fatty acids that contain at least one pair of
methylene interrupted unsaturated bonds are also suitable loading
substances. By "methylene interrupted unsaturated bond" is meant
that one carbon-carbon double or triple bond is separated from
another carbon-carbon double or triple bond by at least one
methylene group (i.e., CH.sub.2). Specific examples of such loading
substances include, but are not limited to, the n-1 family derived
from 9, 12, 15-16:3; n-2 family derived from 9, 12, 15-17:3, 15:3,
17:3, 17:4, 20:4; n-3 family derived from 9, 12, 15-18:3, 15:2,
15:3, 15:4, 16:3, 16:4, 18:3 (.alpha.-linolenic), 18:4, 18:5, 20:2,
20:3, 20:4; 20:5 (EPA), 21:5, 22:3, 22:5 (DPA), 22:6 (DHA), 24:3,
24:4, 24:5, 24:6, 26:5, 26:6, 28:7, 30:5; n-4 family derived from
9, 12-16:2, 16:2, 16:3, 18:2, 18:3; n-5 family derived from 9,
12-17:2, 15:2, 17:2, 17:3, 19:2, 19:4, 20:3, 20:4 21:4, 21:5; n-6
family derived from 9, 12-18:2, 15:2, 16:2, 18:2 (linoleic acid),
18:3 (.gamma.-linolenic acid); 20:2, 20:3, 20:4 (arachidonic acid),
22:2, 22:3, 22:4 (adrenic acid), 22:5, 24:2, 24:4, 25:2, 26:2,
30:4; n-7 family derived from 9-16:1, 15:2, 16:2, 17:2, 18:2, 19:2;
n-8 family derived from 9-17:1, 15:2, 16:2, 17:2, 18:2, 19:2; n-9
family derived from 9-18:1, 17:2, 18:2, 20:2, 20:3, 22:3, 22:4;
n-11 family 19:2, and the n-12 family 20:2. In one particular
specific example, the loading substance can comprise arachidonic
acid.
[0082] In the above paragraph (and throughout) the compounds are
identified by referring first to the "n-x family," where x is the
position in the fatty acid where the first double bond begins. The
numbering scheme begins at the terminal end of the fatty acid,
where, for example, the terminal CH.sub.3 group is designated
position 1. In this sense, the n-3 family would be an omega-3 fatty
acid, as described above. The next number identifies the total
number of carbon atoms in the fatty acid. The third number, which
is after the colon, designates the total number of double bonds in
the fatty acid. So, for example, in the n-1 family, 16:3, refers to
a 16 carbon long fatty acid with 3 double bonds, each separated by
a methylene, wherein the first double bond begins at position 1,
i.e., the terminal end of the fatty acid. In another example, in
the n-6 family, 18:3, refers to an 18 carbon long fatty acid with 3
methylene separated double bonds beginning at position 6, i.e., the
sixth carbon from the terminal end of the fatty acid, and so
forth.
[0083] Further examples of loading substances that contain at least
one pair of methylene interrupted unsaturated bonds are shown in
Table 2.
TABLE-US-00002 TABLE 2 Examples of Polyene Acids Total number of
Carbon number where double bond begins. carbon atoms in the ("c"
denotes a cis double bond; "t" fatty acid chain denotes a trans
double bond) 18 5, 9 5, 11 2t, 9, 12 3t, 9, 12 5t, 9, 12 5, 9, 12
5, 11, 14 3t, 9, 12, 15 5, 9, 12, 15 20 5, 11 5, 13 7, 11 7, 13 5,
11, 14 7, 11, 14 5, 11, 14, 17 22 5, 11 5, 13 7, 13 7, 15 7, 17 9,
13 9, 15
[0084] Specific examples of suitable loading substances that
contain conjugated unsaturated bonds include, but are not limited
to, those in Table 3. By "conjugated unsaturated bond" is meant
that at least one pair of carbon-carbon double and/or triple bonds
are bonded together, without a methylene (CH.sub.2) group between
them (e.g., CH.dbd.CH--CH.dbd.CH--).
TABLE-US-00003 TABLE 3 Examples of Conjugated Polyene Acids Total
number of Carbon number where double bond begins. carbon atoms in
the ("c" denotes a cis double bond; "t" fatty acid chain. denotes a
trans double bond) 10 2t, 4t, 6c 2c, 4t, 6t 3t, 5t, 7c 3c, 5t, 7t
12 3, 5, 7, 9, 11 14 3, 5, 7, 9, 11 18 10t, 12t 8c, 10t, 12c
(jacaric) 8t, 10t, 12c (calendic) 8t, 10t, 12t 9t, 11t, 13c
(catalpic) 9c, 11t, 13t (.alpha.-eleostearic) 9c, 11t, 13c
(punicic) 9t, 11t, 13t (.beta.-eleostearic) 9c, 11t, 13t, 15c
(.alpha.-parinaric) 9t, 11t, 13t, 15t (.beta.-parinaric)
[0085] In the above examples of suitable loading substances,
derivatives of the disclosed loading substances can also be used.
By "derivatives" is meant the ester of a fatty acid (e.g., methyl
and ethyl esters), salts of the fatty acids (e.g., sodium and
potassium salts), and triglycerides, diglycerides, and
monoglycerides, sterol esters, antioxidant-oil conjugates (e.g.,
ascorbyl palmitate), and naturally derivatives such as furanoid
fatty acid derivatives.
[0086] The loading substances disclosed herein can also be crude
oils, semi-refined (also called alkaline refined), or refined oils
from such sources disclosed herein. Still further, the disclosed
compositions and methods can use oils comprising re-esterified
triglycerides.
[0087] It is contemplated herein that one or more of the disclosed
loading substances can be used. For example the disclosed delivery
devices can contain two or more different loading substances.
Further, the loading substance can be present in an amount of from
about 1% to about 50% by weight of a microcapsule. In specific
examples, the loading substance can be present in an amount of from
about 1% to about 40%, from about 1% to about 30%, from about 1% to
about 20%, from about 1% to about 15%, or from about 1% to about
10% by weight of a microcapsule.
[0088] In one example, the loading substance is not a fatty acid
conjugate. A fatty acid conjugate is a fatty acid that has been
coupled to (e.g., bonded to) another chemical moiety, such as a
metal (e.g., chromium) or cofactor (CoQ.sub.10).
[0089] In one example, the loading substances can contain an
antioxidant. Suitable examples of antioxidants include, but are not
limited to, a phenolic compound, a plant extract, or a
sulfur-containing compound. In certain examples disclosed herein
the antioxidant can be ascorbic acid or a salt thereof, e.g.,
sodium ascorbate. In other examples, the antioxidant can be citric
acid or a salt thereof. In still other examples, the antioxidant
can be vitamin E, CoQ.sub.10, tocopherols, lipid soluble
derivatives of more polar antioxidants such as ascobyl fatty acid
esters (e.g., ascobyl palmitate), plant extracts (e.g., rosemary,
sage and oregano oils), algal extracts, and synthetic antioxidants
(e.g., BHT, TBHQ, ethoxyquin, alkyl gallates, hydroquinones,
tocotrienols).
[0090] The disclosed loading substance can also contain other
nutrient(s) such as vitamins other trace elements, minerals, and
the like. Further, the loading substances can comprise other
components such as preservatives, antimicrobials, anti-oxidants,
chelating agents, thickeners, flavorings, diluents, emulsifiers,
dispersing aids, or binders, including any mixture thereof.
SPECIFIC EXAMPLES
[0091] Specific examples of suitable delivery devices include
microcapsules that contain any of the shell materials and any of
the loading substances disclosed herein. Some specific examples
include, but are not limited to, microcapsules where the shell
materials are complex coacervates, e.g., coacervates of gelatin and
polyphosphate. The shell material can, in certain examples,
comprise gelatin with a Bloom number of from about 0 to about 50.
Loading substances that can be used can, in many instances, include
marine oils (e.g., fish oils and algal oils). Loading substances
that comprise omega-3 fatty acids such as EPA and DHA can also be
desirable. Further, derivatives of omega-3 fatty acids, such as
mono-, di-, and triglycerides, alkyl esters, sterol esters,
antioxidant esters (e.g., ascorbyl and citryl esters), and furanoid
esters, can also be suitable loading substances.
[0092] Some particularly suitable microcapsules include
microcapsules containing fish oils. Examples of such fish oils
include, but are not limited to, sardine, anchovy, bonito, and/or
tuna oil. Fish oils can also be referred to herein by the
approximate ratio of EPA and DHA, or derivatives thereof, found in
the oil. For example, 18:12 oils generally comprise a ratio of EPA
to DHA (or their triglyceride esters for example) of about 18:12.
Likewise, 5:25 oils generally comprise a ratio of EPA to DHA of
about 5:25. Any of these oils can be encapsulated in a complex
coacervate comprising and fish or pork gelatin. Such microcapsules
can be Generally Regarded as Safe (GRAS), kosher, and/or Halal.
Also, such microcapsules can have at least about 130 mg of DHA or
at least about 150 mg of EPA and DHA per gram of powder. Further,
antioxidants such as ascorbic acid, citric acid, and/or phosphoric
acid (or salts thereof) can be present in such microcapsules.
[0093] Some specific examples of food articles disclosed herein
comprise microcapsules having about 130 mg of DHA per gram of
microcapsule (e.g., a microcapsule wherein the loading substance
comprises a 5:25 oil derived from tuna and/or bonito) and the outer
shell of the microcapsules comprises pork or fish gelatin. In
another specific example, a food article disclosed herein can
comprise a microcapsule having about 150 mg of DHA and EPA per gram
of microcapsule (e.g., a microcapsule wherein the loading substance
comprises a 18:12 oil derived from sardine and/or anchovy) and the
outer shell of the microcapsules comprises pork or fish
gelatin.
[0094] In one instance, the loading substance is not a conjugated
fatty acid. In another instance, the microcapsule does not comprise
a low Bloom gelatin.
[0095] Method of Making Microcapsules
[0096] Microcapsules prepared by the processes disclosed herein
typically have a combination of payload and structural strength
that are suitable for the disclosed food articles and methods. In
one example, the methods disclosed in U.S. Pat. Nos. 6,974,592 and
6,969,530, which are incorporated by reference in their entirety,
can be used to prepare microcapsules that can be incorporated into
the food articles disclosed herein. It is also contemplated that
one or more additional shell layers can be placed on the outer
shell of the single-core or multicore microcapsules. In one
example, the techniques described in International Publication No.
WO 2004/041251 A1, which is incorporated by reference in its
entirety, can be used to add additional shell layers to the
single-core and multicore microcapsules.
[0097] In general, suitable microcapsules can be prepared by a
process that comprises providing an emulsion comprising a first
polymer component and a loading substance; adding a second polymer
component to the emulsion; adjusting pH, temperature,
concentration, mixing speed, or a combination thereof to form an
aqueous mixture comprising a primary shell material, wherein the
primary shell material comprises the first and second polymer
components and surrounds the loading substance; cooling the aqueous
mixture to a temperature above the gel point of the primary shell
material until the primary shell material forms agglomerations; and
further cooling the aqueous mixture to form an outer shell around
the agglomeration.
[0098] In these methods, the first polymer component and second
polymer component can be the same as any of the primary and outer
shell materials described herein. That is, the first and second
polymer components can become the primary and/or outer shell
materials in the disclosed methods for preparing microcapsules.
Furthermore, any of the loading substances described herein can be
used in these methods for preparing microcapsules.
[0099] In the disclosed methods, an aqueous mixture of a loading
substance, a first polymer component of the shell material, and a
second polymer component of the shell material is formed. The
aqueous mixture can be a mechanical mixture, a suspension, or an
emulsion. When a liquid loading substance is used, particularly a
hydrophobic liquid, the aqueous mixture can be an emulsion of the
loading substance and the polymer components. In another example, a
first polymer component is provided in aqueous solution, together
with processing aids, such as antioxidants. A loading substance can
then be dispersed into the aqueous mixture, for example, by using a
homogenizer. If the loading substance is a hydrophobic liquid, an
emulsion is formed in which a fraction of the first polymer
component begins to deposit around individual droplets of loading
substance to begin the formation of primary shells. If the loading
substance is a solid particle, a suspension is formed in which a
fraction of the first polymer component begins to deposit around
individual particles to begin the formation of primary shells. At
this point, another aqueous solution of a second polymer component
can be added to the aqueous mixture.
[0100] In the processes for preparing microcapsules disclosed
herein, providing an emulsion of the first polymer component and
the loading substance can be accomplished by methods and apparatus
known in the art, e.g., homogenization and high pressure/high shear
pumps. For example, emulsification can take place by emulsifying at
from about 1,000 to about 15,000 rpm. The emulsification step can
be monitored by removing a sample of the mixture and analyzing it
under such methods as microscopy, light scattering, turbidity, etc.
Generally, emulsification can be performed until an average droplet
size of less than about 1,000, 750, 500, 100, or 10 nm is obtained.
Not wishing to be bound by theory but it is believed that by
varying the emulsification speed it is possible to produce single
or multicore microcapsules. For example, when lower emulsification
speeds are used (e.g., 1,000 to 2,000 rpm), the droplets of the
loading substance are large enough to form a single particle, which
upon encapsulation, produces a single core microcapsule.
Conversely, if high emulsification speeds are used (e.g., 5,000 to
15,000 rpm), the resultant droplets of loading substance are
usually small (e.g., from 1 to 10 .mu.m). These tiny droplets can
have higher surface energy and can readily form agglomerations when
pH and/or temperature is adjusted accordingly, which results in the
formation of multicore microcapsules upon encapsulation. Particle
size can be measured using any typical equipment known in the art,
for example, a COULTER.TM. LS230 Particle Size Analyzer, Miami,
Fla. USA.
[0101] The emulsification step can be performed at greater than
room temperature, greater than 30, 40, 50, 60, 70, or 80.degree.
C., where any of the stated values can form an upper or lower
endpoint when appropriate. Specific examples include emulsifying
the mixture at from about 30.degree. C. to about 60.degree. C. or
from about 40.degree. C. to about 50.degree. C.
[0102] It is further contemplated that antioxidants and/or
surfactants, which are also described herein, can be added to the
aqueous mixture. Such antioxidants and/or surfactants can be added
before, during, and/or after the emulsion is provided.
[0103] The amount of the polymer components of the shell material
provided in the aqueous mixture is typically sufficient to form
both the primary shells and the outer shells of the loading
agglomeration of microcapsules. The loading substance can be
provided in an amount of from about 1% to about 15% by weight of
the aqueous mixture, from about 3% to about 8% by weight, or about
6% by weight.
[0104] The pH, temperature, concentration, mixing speed, or a
combination thereof can be adjusted to form an aqueous mixture
comprising a primary shell material, wherein the primary shell
material comprises the first and second polymer components and
surrounds the loading substance. If there is more than one type of
polymer component, complex coacervation will occur between the
components to form a coacervate, which further deposits around the
loading substance to form primary shells of shell material. The pH
adjustment depends on the type of shell material to be formed. For
example, the pH may be adjusted to a value from 3.5 to 5.0, or from
4.0 to 5.0. If the pH of the mixture starts in the desired range,
then little or no pH adjustment is required.
[0105] The initial temperature of the aqueous mixture can be from
about 20.degree. C. to about 60.degree. C., or about 30.degree. C.
to about 50.degree. C.
[0106] Mixing can be adjusted so that there is good mixing without
breaking the microcapsules as they form. Particular mixing
parameters depend on the type of equipment being used. Any of a
variety of types of mixing equipment known in the art may be used.
In one example, an axial flow impeller, such as LIGHTNIN A310 or
A510, can be used.
[0107] In many examples disclosed herein, the primary shell and the
outer shell of the disclosed microcapsules can comprise a complex
coacervate. The complex coacervate can be formed from the first and
second polymer components. For example, the primary shell and the
outer shell can comprise a complex coacervate between gelatin and
polyphosphate. All combinations of first and second polymer
components are contemplated herein for the complex coacervate and
the primary and outer shell.
[0108] The aqueous mixture can then be cooled under controlled
cooling rate and mixing parameters to permit agglomeration of the
primary shells to form encapsulated agglomerations of primary
shells. Not wishing to be bound by theory, the encapsulated
agglomerations are discrete particles themselves. It is
advantageous to control the formation of the encapsulated
agglomerations at a temperature above the gel point of the shell
material, and to let excess shell material form a thicker outer
shell. It is also possible at this stage to add more polymer, where
the polymer is the same or different as the shell material being
used, in order to thicken the outer shell and/or produce
microcapsules having primary and outer shells of different
composition. The outer shell encapsulates the agglomeration of
primary shells to form a rigid encapsulated agglomeration of
microcapsules.
[0109] Cooling the aqueous mixture can be accomplished by methods
known in the art (e.g., the use of a chiller). The rate of cooling
can be about 1.degree. C. per about 1 to about 100 minutes. For
example, the rate of cooling can be about 1.degree. C. per about 1,
5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85,
90, 95, or 100 minutes, where any of the stated values can form an
upper or lower endpoint when appropriate. In specific examples the
rate of cooling can be about 1.degree. C./5 minutes. Cooling can
take place until the mixture reaches a temperature of from about
5.degree. C. to about 10.degree. C., e.g., about 5.degree. C.
[0110] Processing aids can be included in the shell material (e.g.,
primary and/or outer shells). Processing aids can be used for a
variety of reasons. For example, they may be used to promote
agglomeration of the primary microcapsules, stabilize the emulsion
system, improve the properties of the outer shells, control
microcapsule size, and/or to act as an antioxidant. In one aspect,
the processing aid can be an emulsifier, a fatty acid, a lipid, a
wax, a microbial cell (e.g., yeast cell lines), a clay, or an
inorganic compound (e.g., calcium carbonate). Not wishing to be
bound by theory, these processing aids can improve the barrier
properties of the microcapsules. In one aspect, one or more
antioxidants can be added to the shell material. Antioxidant
properties are useful both during the process (e.g., during
coacervation and/or spray drying) and in the microcapsules after
they are formed (i.e., to extend shelf-life, etc). Preferably a
small number of processing aids that perform a large number of
functions can be used. In one aspect, the antioxidant can be a
phenolic compound, a plant extract, or a sulphur-containing amino
acid. In one aspect, ascorbic acid or citric acid (or a salt
thereof such as sodium or potassium ascorbate or sodium or
potassium citrate) can be used to promote agglomeration of the
primary microcapsules, to control microcapsule size and to act as
an antioxidant. The antioxidant can be used in an amount of about
100 ppm to about 12,000 ppm, or from about 1,000 ppm to about 5,000
ppm. Other processing aids such as, for example, metal chelators,
can be used as well. For example, ethylene diamine tetraacetic acid
can be used to bind metal ions, which can reduce the catalytic
oxidation of the loading substance.
[0111] In the disclosed microcapsules, the shell material can also
be cross-linked. Thus, the disclosed methods can further involve
the addition of a cross-linker. The cross-linker can be added to
further increase the rigidity of the microcapsules by cross-linking
the shell material in both the outer and primary shells and to make
the shells insoluble in both aqueous and oily media. In one
example, the cross-linker is added after the outer shell of the
microcapsule is produced. Any suitable cross-linker can be used and
the choice of cross-linker can vary depending upon the selection of
the first and second polymer component. In another example, the
cross-linkers can be enzymatic cross-linkers (e.g.
transglutaminase), aldehydes (e.g. formaldehyde or gluteraldehyde),
tannic acid, alum or a mixture thereof. In another aspect, the
cross-linker can be a plant extract or a phenolic. It is also
contemplated that one or more loading substances (e.g.,
antioxidants) can be used with the cross-linker. When the
microcapsules are to be used in a formulation that is to be
delivered to an organism, the cross-linkers are preferably
non-toxic or of sufficiently low toxicity. The amount of
cross-linker used depends on the components selected and can be
adjusted to provide more or less structural rigidity as desired. In
one aspect, the amount of cross-linker that can be used is in the
amount of about 0.1% to about 5.0%, about 0.5% to about 5.0%, about
1.0% to about 5.0%, about 2.0% to about 4.0%, or about 2.5%, by
weight of the first polymer component. In general, one skilled in
the art can routinely determine the desired amount in any given
case by simple experimentation. The cross-linker can be added at
any stage of the process, however it, can typically be added after
the cooling step.
[0112] Further, the disclosed microcapsules can be washed with
water and/or dried to provide a free-flowing powder. Thus, the
disclosed methods of preparing microcapsules can comprise a drying
step for the microcapsules. Drying can be accomplished by a number
of methods known in the art such as, for example, freeze drying,
drying with ethanol, or spray drying. In one aspect, spray drying
can be used for drying the microcapsules. Spray drying techniques
are disclosed in "Spray Drying Handbook", K. Masters, 5th edition,
Longman Scientific Technical UK, 1991, the disclosure of which is
hereby incorporated by reference at least for its teaching of spray
drying methods.
Methods of Preparing the Food Articles
[0113] The food articles disclosed herein contain delivery devices,
such as those disclosed herein, and can be used to deliver loading
substances encapsulated within the delivery device (e.g., omega-3
fatty acids) to a subject for nutritional or medical purposes. In
one example, the delivery device is a microcapsule. The
microcapsules disclosed herein have good rupture strength to help
reduce or prevent breaking of the microcapsules during
incorporation into food or other formulations. Furthermore, the
microcapsule's shells are insoluble in both aqueous and oily media,
and help reduce or prevent oxidation and/or deterioration of the
loading substance during preparation of the microcapsules, during
long-term storage, and/or during incorporation of the microcapsules
into a formulation vehicle, for example, into food articles.
[0114] The particular method of preparing the disclosed food
articles will depend on such factors as the particular food
article, the delivery device, and the loading substance. In some
examples, the delivery device (e.g., microcapsules) can be mixed
with the ingredients of the food article before the food article is
prepared. Examples of this can include adding delivery devices to
batter or breading for various food articles (e.g., fish, shrimp,
poultry, vegetables) and then cooking the food. In other examples,
the delivery devices can be added to (e.g., contacted to or poured
or sprinkled on) the food article after it is prepared, but before
packaging. Typical examples of this method involve contacting the
food article with the delivery device. Such contacting steps can be
combined with other seasoning steps. In still another example, the
delivery device can be packaged separately from the food article
(e.g., microcapsules can be packaged alone as a condiment pack or
mixed into other seasonings) and then added to the food article
prior to consumption (e.g., by the consumer or food preparation
personnel).
[0115] In one example, delivery devices, along with other optional
seasonings, can be pulse sprayed or mist sprayed onto the surface
of the food article. Alternatively, a drum can contain the delivery
devices and the food article can be introduced into the drum and
agitated (e.g., rolled around inside the drum). FIG. 1 depicts one
example of this technique, where, for example, a seasoning and
delivery device comprising omega-3 fatty acids are mixed in a
horizontal mixer 1. The mixture is then placed in a sprayer 2,
which then applies the mixture to the food article 4 present in
drum 3. Drum 3 can be rotated while the mixture is sprayed onto the
food article in order to ensure even distribution of the mixture to
the food article. Suitable apparatus for introducing delivery
devices can be obtained commercially from suppliers such as FMC
Technologies (Chalfont, Pa.).
[0116] The amount of delivery devices (and thus loading substance)
that can be used with the disclosed food articles will depend on
such factors as the type of food article, the type of loading
substance, the presence of additional seasonings, the desired
dietary intake, preference, and the like. Guidance can be found in
the literature for appropriate amounts for given classes of loading
substances and determining a particular amount is within the skill
in art. Generally, an amount of delivery devices that will provide
the desired amount of loading substance to a subject, but not
detract from the taste and texture of the food article can be
used.
[0117] In one example, the disclosed food article comprises a snack
food (e.g., a chip) and a microcapsules. In a further example, the
food article is a chip and the loading substance comprises an
omega-3 fatty acid. Typical amounts of microcapsules that can be
used for chips are about 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 2.9%, 3.0%,
3.5%, 4.0%, 1.5%, 5.0%, 5.5%, or 6.0% by weight, based on the total
weight of the chip, where any of the stated values can form an
upper or lower end point when appropriate. In other examples, less
than or equal to about 6.0%, less than or equal to about 5.0%, less
than or equal to about 4.0%, less than or equal to about 3.0%, less
than or equal to about 2.0%, or less than or equal to about 1.0% by
weight, based on the total weight of the chip can be used. In other
examples, a chip can have about 0.5, 1.0, 1.5, 2.0, 2.5, 2.9, 3.0,
3.5, 4.0, 4.5, 5.0, 5.5, or 6.0 parts by weight microcapsules,
where any of the stated values can form an upper or lower end point
when appropriate. In other examples, a chip can have less than or
equal to about 6.0, less than or equal to about 5.0, less than or
equal to about 4.0, less than or equal to about 3.0, less than or
equal to about 2.0, or less than or equal to about 1.0 parts by
weight microcapsule. In another example, a chip can have
microcapsules at from about 1 to about 6, from about 2 to about 4,
or about 3% by weight based on the total weight of the chip. Still
further, a chip can have from about 1 to about 6, from about 2 to
about 4, and about 3 parts by weight microcapsules.
[0118] In another example, the disclosed food article can comprise
seasonings in addition to the delivery devices. The seasonings can
be blended with the microcapsules and then added to the food
article (e.g., chip). As such, disclosed herein is a seasoning for
a food article that comprises a microcapsule. In one example, the
delivery device comprises a microcapsule. Exemplary amounts of
microcapsules that can be blended with a seasoning are about 5%,
6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%,
20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%,
33%, 34%, 35%, 36%, 37%, 38%, 39%, or 40% by weight, based on the
total weight of the blend, where any of the stated values can form
an upper or lower end point when appropriate. In other examples,
from about 20 to about 25%, from about 15 to about 30%, from about
10 to about 35%, from about 5 to about 40%, from about 5 to about
20%, from about 20 to about 40% by weight, based on the total
weight of the blend can be used. Also, microcapsules can be blended
with a seasoning at about 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15,
16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32,
33, 34, 35, 36, 37, 38, 39, or 40 parts by weight, where any of the
stated values can form an upper or lower end point when
appropriate. In other examples, a seasoning blend can contain from
about 20 to about 25, from about 15 to about 30, from about 10 to
about 35, from about 5 to about 40, from about 5 to about 20, from
about 20 to about 40 parts by weight microcapsules.
[0119] When the seasoning is a chip seasoning, it can be present in
an amount of about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%,
12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20% by weight based on
the total amount of the chip, where any of the stated values can
form an upper or lower endpoint when appropriate. In other
examples, a chip can contain about 1, 2, 3, 4, 5, 6, 7, 8, 9, 10,
11, 12, 13, 14, 15, 16, 17, 18, 19, or 20 parts by weight
seasoning, where any of the stated values can form an upper or
lower endpoint when appropriate.
[0120] When preparing chips, the chip can also contain oil in an
amount of about 1, 2, 3, 4, 5, 6, 7, or 8% by weight, where any of
the stated values can form an upper or lower endpoint when
appropriate.
[0121] Other methods disclosed herein involve mixing the delivery
device (e.g., microcapsule) with one or more ingredients used to
prepare the food article prior to preparing the food article.
Alternative or additional methods involve contacting an already
prepared food article with the delivery device. For example, the
delivery device can be blended with a seasoning for the food
article. The delivery device can also be sprayed onto the food
article. Further, the delivery device can be mixed with the food
article.
[0122] The amount of delivery device used to prepare a food article
can vary depending on the type of food article, the type of
delivery device, the amount of loading substance, the desired
dosage, preference, and the like. In general, the amount of loading
substance desired to be delivered will be a main consideration. As
an example, a microcapsule containing EPA and DHA can be added in
such an amount that the food article containing the microcapsule
can have from about 10 to about 250 mg of EPA+DHA per serving. For
example the food article can have about 10, 20, 30, 40, 50, 60, 70,
80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, 200, 210,
220, 230, 240, or 250 mg of the loading substance per serving,
where any of the stated values can form an upper or lower endpoint
when appropriate. When a delivery device contains large amounts of
loading substance, then less of the deliver device needs to be used
in the food article to obtain a desired level of a loading
substance. When a deliver device contains small amounts of loading
substance, then more of the deliver device will need to be used in
the food article to obtain a desired level of a loading substance.
Also, when more loading substance is desired, then more delivery
device can be added, and when less loading substance is desired,
then less delivery device can be added.
[0123] In other examples, the food articles can contain other
additives and components. For example, the food articles disclosed
herein can also comprise a probiotic. Probiotics are live
microorganisms that can be administered to a subject and which can
confer a beneficial health effect on the subject. Examples of
suitable probiotics include, but are not limited to, Lactobacillus
species, Lactococcus species, and Pediococcus species. In one
example the probiotic can be one or more bacteria chosen from
Lactobacillus acidophilus, Lactobacillus sakei, Lactococcus lactis,
and Pediococcus acidilactici. These bacteria can be particularly
useful in the methods and compositions disclosed herein because
they are food safe (i.e., safe to use in, on, or near foods).
Methods of Use
[0124] In one aspect, disclosed herein are methods of delivering a
loading substance to a subject by administering to the subject a
food article as disclosed herein. In a particular example, the
disclosed food articles can be used as a source of fatty acids
(e.g., omega-3 fatty acids), lowering triglycerides and influencing
diabetes related biochemistry. In another particular example,
disclosed herein are methods of supplementing omega-3 fatty acids
in a subject by administering an effective amount of a food article
disclosed herein, wherein the loading substance comprises an
omega-3 fatty acid. In another example, disclosed herein are
methods of lowering cholesterol levels, triglyceride levels, or a
combination thereof in a subject by administering an effective
amount of a food article disclosed herein.
[0125] Omega-3 fatty acids are vital to everyday life and function.
For example, the beneficial effects of omega-3 fatty acids like
cis-5,8,11,14,17-eicosapentaenoic acid (EPA) and
cis-4,7,10,13,16,19-docosahexaenoic acid (DHA) on lowering serum
triglycerides are well established. These compounds are also known
for other cardioprotective benefits such as preventing cardiac
arrhythmias, stabilizing atherosclerotic plaques, reducing platelet
aggregation, and reducing blood pressure. See e.g., Dyrberg et al.,
In: Omega-3 Fatty Acids: Prevention and Treatment of Vascular
Disease. Kristensen et al., eds., Bi & Gi Publ.,
Verona-Springer-Verlag, London, pp. 217-26, 1995; O'Keefe and
Harris, Am. J. Cardiology 2000, 85:1239-41; Radack et al., "The
effects of low doses of omega-3 fatty acid supplementation on blood
pressure in hypertensive subjects: a randomized controlled trial."
Arch. Intern. Med. 1991, 151:1173-80; Harris, "Extending the
cardiovascular benefits of omega-3 fatty acids." Curr Atheroscler
Rep 2005, 7:375-80; Holub, "Clinical nutrition: 4 omega-3 fatty
acids in cardiovascular care." CMAJ2002, 166(5):608-15. Indeed, the
American Heart Association has also reported that omega-3 fatty
acids can reduce cardiovascular and heart disease risk. Other
benefits of omega-3 fatty acids are those related to the prevention
and/or treatment of inflammation and neurodegenerative diseases,
and to improved cognitive development. See e.g., Sugano and
Michihiro, "Balanced intake of polyunsaturated fatty acids for
health benefits." J. Oleo Sci. 2001, 50(5):305-11.
[0126] The fatty acids EPA and DHA can be synthesized in the human
body from .alpha.-linolenic acid (18:3); however, the conversion
rate from this precursor molecule is limited (Muskiet et al., "Is
docosahexaenoic acid (DHA) essential? Lessons from DHA status
regulation, our ancient diet, epidemiology and randomized
controlled trials." J Nutr. 2004, 134(1):183-6). Accordingly, EPA
and DHA in the body are primarily derived from dietary sources
(e.g., oily fish). Diets rich in fish oils are known to have many
beneficial effects for heart disease, cancer, arthritis, allergies,
and other chronic diseases. Epidemiological clinical trials have
shown that increasing the dietary intake of omega-3 fatty acids, in
the form of fish or of fish oil supplements, may reduce various
risk factors associated with cardiovascular disease. See e.g., The
American Heart Association, Scientific Statement, "Fish
Consumption, Fish Oil, Omega-3 Fatty Acids and Cardiovascular
Disease," November 2002; Appel et al., "Does supplementation of
diet with `fish oil` reduce blood pressure? A meta-analysis of
controlled clinical trials." Arch. Intern. Med. 1993,
153(12):1429-1438; GISSI-Prevenzione Investigators. "Dietary
supplementation with omega-3 polyunsaturated fatty acids and
vitamin E after myocardial infarction: results of the
GISSI-Prevenzione trial." Lancet 1999, 354:447-55.
[0127] Despite the strong evidence for the benefit of omega-3 fatty
acids like EPA and DHA in prevention of cardiovascular disease, the
average daily consumption of these fatty acids by North Americans
is estimated to be between 0.1 to 0.2 grams, compared to a
suggested daily intake of 0.65 grams to confer benefit (Webb,
"Alternative sources of omega-3 fatty acids." Natural Foods
Merchandiser 2005, XXVI (8):40-4). Since altering dietary patterns
of populations is difficult and many people do not like to eat
fish, dietary supplementation with EPA and DHA is an important
approach to addressing this problem. Unfortunately, many
supplements of omega-3 fatty acids are sensitive to oxidation and
can be foul smelling and tasting. Further, compliance with dietary
supplement regimens requires discipline, which is often wanting. In
light of the health benefits of omega-3 fatty acids, the disclosed
formulations comprising microcapsules can be used to deliver
omega-3 fatty acids to a subject. In the disclosed methods of use,
the food articles that are administered can be any of the
formulations disclosed herein.
[0128] When used in the above described methods or other
treatments, an "effective amount" of one of the disclosed food
articles (or one of the loading substances therein) can be employed
in pure form or, where such forms exist, in pharmaceutically
acceptable salt form, foodstuff, or other form.
[0129] The specific effective dose level for any particular subject
will depend upon a variety of factors including the disorder being
treated and the severity of the disorder; the identity and activity
of the specific composition employed; the age, body weight, general
health, sex and diet of the patient; the time of administration;
the route of administration; the rate of excretion of the specific
composition employed; the duration of the treatment; drugs used in
combination or coincidental with the specific composition employed
and like factors well known in the medical arts. For example, it is
well within the skill of the art to start doses of a composition at
levels lower than those required to achieve the desired therapeutic
effect and to gradually increase the dosage until the desired
effect is achieved. If desired, the effective daily dose can be
divided into multiple doses for purposes of administration.
Consequently, single dose compositions can contain such amounts or
submultiples thereof to make up the daily dose.
[0130] The dosage can be adjusted by the individual physician or
the subject in the event of any counterindications. Dosage can
vary, and can be administered in one or more dose administrations
daily, for one or several days. Guidance can be found in the
literature for appropriate dosages for given classes of
pharmaceutical products.
[0131] Further, disclosed are methods for delivering a disclosed
composition to a subject by administering to the subject any of the
food articles disclosed herein.
EXAMPLES
[0132] The following examples are set forth below to illustrate the
methods and results according to the disclosed subject matter.
These examples are not intended to be inclusive of all aspects of
the subject matter disclosed herein, but rather to illustrate
representative methods and results. These examples are not intended
to exclude equivalents and variations of the present invention
which are apparent to one skilled in the art.
[0133] Efforts have been made to ensure accuracy with respect to
numbers (e.g., amounts, temperature, etc.) but some errors and
deviations should be accounted for. Unless indicated otherwise,
parts are parts by weight, temperature is in .degree. C. or is at
ambient temperature, and pressure is at or near atmospheric. There
are numerous variations and combinations of reaction conditions,
e.g., component concentrations, desired solvents, solvent mixtures,
temperatures, pressures and other reaction ranges and conditions
that can be used to optimize the product purity and yield obtained
from the described process. Only reasonable and routine
experimentation will be required to optimize such process
conditions.
Example 1
Microcapsule Preparation
[0134] 54.5 grams gelatine 275 Bloom type A (isoelectric point of
about 9) was mixed with 600 grams of deionized water containing
0.5% sodium ascorbate under agitation at 50.degree. C. until
completely dissolved. 5.45 grams of sodium polyphosphate was
dissolved in 104 grams of deionized water containing 0.5% sodium
ascorbate. 90 grams of a fish oil concentrate containing 30%
eicosapentaenoic acid ethyl ester (EPA) and 20% docosahexaenoic
acid ethyl ester (DHA) (available from Ocean Nutrition Canada,
Dartmouth, Nova Scotia) was dispersed with 1.0% of an antioxidant
(blend of natural flavour, tocopherols and citric acid available as
DURALOX.TM. from KALSEC.TM.) into the gelatine solution with a high
speed POLYTRON.TM. homogenizer. An oil-in-water emulsion was
formed. The oil droplet size had a narrow distribution with an
average size of about 1 .mu.m measured by COULTER.TM. LS230
Particle Size Analyzer. The emulsion was diluted with 700 grams of
deionized water containing 0.5% sodium ascorbate at 50.degree. C.
The sodium polyphosphate solution was then added into the emulsion
and mixed with a Lightning agitator at 600 rpm. The pH was then
adjusted to 4.5 with a 10% aqueous acetic acid solution. During pH
adjustment and the cooling step that followed pH adjustment, a
coacervate formed from the gelatine and polyphosphate coated onto
the oil droplets to form primary microcapsules. Cooling was carried
out to above the gel point of the gelatine and polyphosphate and
the primary microcapsules started to agglomerate to form lumps
under agitation. Upon further cooling of the mixture, polymer
remaining in the aqueous phase further coated the lumps of primary
microcapsules to form an encapsulated agglomeration of
microcapsules having an outer shell and having an average size of
50 .mu.m. Once the temperature had been cooled to 5.degree. C., 2.7
grams of 50% gluteraldehyde was added into the mixture to further
strengthen the shell. The mixture was then warmed to room
temperature and kept stirring for 12 hours. Finally, the
microcapsule suspension washed with water. The washed suspension
was then spray dried to obtain a free-flowing powder. A payload of
60% was obtained.
Example 2
Microcapsule Preparation
[0135] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that 0.25% sodium
ascorbate was used. A payload of 50% was obtained.
Example 3
Microcapsule Preparation
[0136] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that no ascorbate
was used. A payload of 60% was obtained.
Example 4
Microcapsule Preparation
[0137] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that 105 grams of
fish oil concentrate was used and a payload of 70% was
obtained.
Example 5
Microcapsule Preparation
[0138] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that it was applied
to triglyceride (TG) fish oil (available from Ocean Nutrition
Canada Ltd.) rather than ethyl ester fish oil.
Example 6
Microcapsule Preparation
[0139] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that gelatine (type
A) and gum arabic were used as polymer components of the shell
material.
Example 7
Microcapsule Preparation
[0140] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that 150 Bloom
gelatine (type A) and polyphosphate were used as polymer components
of the shell material and 105 grams of fish oil concentrate was
used to obtain a payload of 70%.
Example 8
Microcapsule Preparation
[0141] Encapsulated agglomerations of microcapsules were formed in
accordance with the method of Example 1 except that
transglutaminase was used to cross-link the shell material.
Example 9
Potato Chips
[0142] Microencapsulated omega-3 oil (MEG-3.TM. powder) was
provided by Ocean Nutrition Canada (Dartmouth, Canada). Unseasoned
potato chips and dry seasoning were provided by Kettle Chip Company
(Salem, Oreg.).
[0143] The dry seasoning (at ambient temperature) and microcapsules
(at minus 18.degree. C.) were placed in a plastic laboratory tub.
The tub was covered and the contents were shaken vigorously by hand
for about one minute until the mixture was homogeneous. A
commercial blender at low speed for a short period of time can also
be used. Since a dry blend can heat during the blending process, it
can be desired to keep the mixture cool. See Table 4.
[0144] In a stainless steel bowl, the unseasoned chips were sprayed
with oil (e.g., PAM; ConAgra Foods, Omaha, Nebr.), while tossing
the chips with a spatula until about 4% by weight of the oil was
sprayed on the chips. It is also possible to use freshly fried
chips, since the residual oil can serve as an adhesive for the dry
seasonings.
[0145] The dry seasoning was added to the PAM-sprayed chips while
tossing was continued until at least 950% of the dry seasoning had
adhered to the chips. In multiple trials, the amount of seasoning
pick up was from about 95% to about 99%. A standard tumbling drum,
where the chips are tossed with dry seasoning added at a
pre-determined rate, can also be used. See Table 4.
[0146] It can also be desired to minimize the time between dry
seasoning blending and application to the chips.
[0147] The chips were then placed in a gas-barrier pouch, which was
flushed with ambient nitrogen gas and sealed.
TABLE-US-00004 TABLE 4 Component 100 grams Weight (g) Percent
Seasoning Blend Classic Barbeque 77.52 10.00 77.52% Seasoning
Microencapsulated 22.48 2.90 22.48% Omega-3 Fatty Acid 100.00 12.90
100.00% Chip Unsalted Chip 283.70 83.10 83.10% Seasoning Blend
44.04 12.90 12.90% Oil 13.66 4.00 4.00% 341.40 100.00 100.00%
Example 10
Apple Sauce Baby Food
[0148] Applesauce containing microcapsules was prepared according
to the formulation shown in Table 5. Specifically, applesauce was
placed into a water-jacketed kettle preheated to 99.5.degree. C.
Microencapsulated omega-3 oil (MC601812TG or MC60DHA from Ocean
Nutrition Canada; Dartmouth, Canada) was added to the applesauce. A
high shear mixer with a rod attachment was positioned in mixture
and the mix speed was set at 800 rpm for the batch. The mixture was
covered to minimize evaporation and maintained at 90.5.degree. C.
for approximately 10 minutes. The hot mixture was then filled into
glass containers (125 g serving size). Foil seals were ironed onto
the containers and the containers were inverted for 2 minutes or
more. The containers were then cooled in an ice water bath and
stored refrigerated.
TABLE-US-00005 TABLE 5 Ingredients Weight (g) Real % Applesauce
with Vitamin 1000.00 99.68 C, 100% DV, aseptic Omega-3
microcapsules 3.210 0.32 Total 1003.210 100.00
[0149] No off-flavors were detected in the applesauce stored under
accelerated or ambient conditions. The samples had about 60 mg
EPA+DHA per 125 g serving.
Example 11
Apple Banana Baby Food
[0150] Apples and banana baby food containing microcapsules was
prepared by first blending bananas with citric acid to a target pH
of about 4.20-4.30. Then, in a water-jacketed kettle, the bananas
were combined with apples and the mixture was pureed to a desired
consistency. Microencapsulated omega-3 oil (MEG-3.TM. powder from
Ocean nutrition Canada; Dartmouth, Canada; 30-50 mg of EPA+DHA per
serving) was blended into the mixture with a hand mixer. The
mixture was covered to minimize evaporation and maintained at
91.degree. C. The hot mixture was then filled into glass containers
(125 g serving size). Foil seals were ironed onto the containers
and the containers were inverted for 2 minutes or more. The
containers were then cooled in an ice water bath and stored
refrigerated. Taste test revealed that lower levels of EPA+DHA were
preferred over higher levels.
Example 12
Breaded Shrimp
[0151] Shrimp containing microcapsules were prepared according to
the formulation shown in Table 6. Specifically, frozen shrimp were
dipped into a predust containing microencapsulated omega-3 oil
(MEG-3.TM. powder from Ocean Nutrition Canada; Dartmouth Canada).
The shrimp were shaken gently to remove the extra predust adhering
to the shrimp. The shrimp were then dipped into the batter and
coated with breadcrumbs. Each shrimp took up to about 0.3 g of
predust, 0.4 g batter and 1 g breading. The shrimp were then fried
in 177.degree. C. oil for approximately 4 minutes. The shrimp were
kept frozen in plastic bags until ready to test.
TABLE-US-00006 TABLE 6 Ingredients Weight (g) Real % Shrimp, frozen
81.00 72.58 Predust* 5.40 4.83 Batter Mix* 7.20 6.45 Bread Crumbs
18.00 16.12 Total: 111.60 100.00 Predust Batter Mix 56.67 56.67
Omega 3 powder 43.33 43.33 Total: 100.00 100.00 Batter Mix Batter
Mix 80.00 34.78 Water, filtered 150.00 65.22 Total: 230.00 100.00
*see formula below
[0152] The shrimp had 175 mg EPA+DHA (350 mg before frying) per
serving (about 18 shrimp). In taste test, the flavor was
acceptable. Since the microcapsules may interfere with adherence of
crust to the shrimp, care should be taken during battering and
breading processes.
Example 13
Pasteurized Process Cheese Food
[0153] Pasteurized process cheese containing microcapsules was
prepared according to the formulation shown in Table 7. All dry
ingredients were first blended. Then all wet ingredients were
gradually blended into the dry ingredients with a whisk. The
mixture was heated in a double boiler to about 60.degree. C. Cheese
was added to the mixture and melted by heating to about
79-82.degree. C. with mixing. The mixture was vacuum packaged in
plastic film pouches to form slices. The pouches were chilled to
form and stored refrigerated.
TABLE-US-00007 TABLE 7 Ingredients Weight (g) Weight % Cheese
257.50 52.34 Water 118.41 24.07 Corn oil 50.00 10.16 Starch, Mira
Clear 340 (Staley) 26.25 5.34 Starch, Tenderfil 8 (Staley) 21.25
4.32 Sodium citrate 10.00 2.03 Disodium Phosphate 5.00 1.02 Annatto
color 0.04 0.008 Omega-3 3.56 0.72 Total 492.01 100.00
[0154] Microencapsulated omega-3 oil (MEG-3.TM. powder from Ocean
Nutrition Canada; Dartmouth Canada) was added with the dry
ingredients or the wet ingredients. Both methods produced similar
results; although, adding them with the dry ingredients was easier.
The products had 32 mg of EPA+DHA oil per serving (30 g slice). At
these loading levels of EPA+DHA, the products tasted acceptable.
Products containing higher levels (50 mg EPA+DHA/serving and
higher) had detectable fish flavors, but the fish flavor dissipated
somewhat as the product aged.
Example 14
Chewy Granola Bar
[0155] A chewy granola bar containing microcapsules was prepared
according to the formulation shown in Table 8. Specifically,
microencapsulated omega-3 oil (MEG-3.TM. powder from Ocean
Nutrition Canada; Dartmouth, Canada) was pre-blended with honey. To
account for loss during transfer, a larger amount than needed was
prepared based on the following calculation (16.54% microcapsules
and honey mixture). The mixture was stirred well and allowed to sit
and hydrate. In a large mixing bowl, oats and crisp rice were
combined and gently mixed. Oil was drizzled into the mixture while
mixing continued. The microcapsules and honey mixture mixed into
the mixture and gently stirred for 1 minute. The mixture was spread
onto baking sheets coated with non-stick spray and baked at
121.degree. C. in a convection oven for 20 minutes, tossing after
10 minutes. After cooling, the product was stored in an airtight
foil package until ready to use.
TABLE-US-00008 TABLE 8 Ingredients Weight (g) Real % Rolled Oats
186.76 46.69 Honey, Clover (60.degree. C.) 92.95 23.24 Crisp Rice
84.89 21.22 Omega 3 18.42 4.61 Canola Oil 16.98 4.24 Total 400.00
100.00
[0156] The product contained 130 mg EPA+DHA per serving (40 g).
Fishy flavors were at were least noticeable when the
microencapsulated oil was baked with cereals. It appears that
cinnamon may have accentuated the fishy flavors. However, the
microcapsules baked and blended with honey (or syrup) produced an
acceptable flavor.
Example 15
Chicken Dinner Baby Food
[0157] A chicken dinner baby food containing microcapsules was
prepared according to the formulation shown in Table 9.
Specifically, the dry ingredients were blended and set aside.
Chicken was boiled, cooled, chopped into small pieces, and then
finely ground in a food processor. Egg noodles were cooked, cooled,
and set aside. Peas were cooked, cooled, pressed through a sieve,
and set aside. Carrots, split peas, chicken fat, oil, and the
noodles were blended in a food processor. While blending, the dry
ingredients and water were slowly added. The ground chicken was
then added and the mixture was blended until the mixture was
completely combined and smooth. The product was then filled into to
8 oz glass jars and retorted at 15 psi for 40 minutes. The product
was stored at ambient temperature.
TABLE-US-00009 TABLE 9 Ingredients Weight (g) Weight % Water 250.00
48.13 Carrots, IQF diced 205.00 39.45 Chicken breast 26.00 5.01
Peas, IQF 11.00 2.12 Egg noodles, cooked 10.00 1.93 Rice flour 9.00
1.73 Chicken fat 3.50 0.67 Onion powder 2.00 0.39 Soybean oil 1.50
0.29 Celery powder 0.05 0.01 Omega-3 1.40 0.27 Total 519.45
100.00
[0158] No off-flavors or odors were detected in the product. The
product contained about 60 mg EPA+DHA per serving (125 g). To avoid
shearing and damage of microcapsules, it was found that the baby
food base needed to be prepared prior to the addition of
microcapsules.
Example 16
Potato Chip Seasoning
[0159] A potato chip seasoning containing microcapsules was
prepared according to the formulation shown in Table 10.
Specifically, the ingredients were blended together. The flavors
tested included BBQ, sour cream and green onion, and salt and
pepper. Then the mixture was applied to potato chips at a level of
12.9%. If there was insufficient residual oil on the chips to allow
for the seasoning to properly adhere, oil was sprayed (about 4% by
weight) onto the chips to act as an adhesive. The chips were
packaged in a nitrogen flushed, metallized film and stored at
ambient temperature. The chips contained 130 g of EPA+DHA per
serving (30 g of seasoned chips).
TABLE-US-00010 TABLE 10 Ingredient Weight (g) Weight % Dry
Seasoning 75.00 77.52 Omega-3 Powder 21.75 22.48 Total 96.75
100.00
[0160] Under accelerated conditions (37.8.degree. C.) some
off-flavors were detected after 4 weeks. Under ambient conditions
(21.1.degree. C.), the flavors of the products were slightly muted
but similar to the controls at 6 weeks of storage
Example 17
Extruded Cereal Bar
[0161] An extruded cereal bar containing microcapsules was prepared
according to the formulation shown in Table 11. Specifically, fat
was creamed with sugar and liquids ingredients were added. Then the
microcapsules were blended with the dry ingredients. All
ingredients were combined and mixed to form dough. The dough was
extruded with a fruit filling center. The product was baked at
163.degree. C. for approximately 6-7 minutes.
TABLE-US-00011 TABLE 11 Ingredients Weight (g) Real % Fruit Filling
Granulated sugar 35.45 17.72 Strawberry puree, seedless 20.86 10.43
Water 18.25 9.12 Strawberry juice concentrate 17.73 8.86 Starch
(Rezista) 6.26 3.13 lemon juice 1.04 0.52 Salt 0.42 0.21 Dough
Pastry flour 43.86 21.93 Fructose 11.10 5.55 Unsalted butter 10.63
5.31 Molasses 5.13 2.56 Non fat milk 11.73 5.86 Egg white powder
4.35 2.17 Canola oil 3.54 1.77 Sugar 3.54 1.77 Salt 0.59 0.29
Lecithin 0.59 0.29 Baking powder 0.52 0.26 Baking soda 0.47 0.23
Emulsifier 0.24 0.12 Xanthan gum 0.18 0.09 Strawberry flavor 0.12
0.06 Vanilla flavor 0.08 0.04 Omega-3 Powder 3.33 1.66 Total 200.01
100.00
[0162] The product contained 50 mg of EPA+DHA per serving (40 g).
The product had acceptable flavor at time of manufacture. Further
the product flavor was acceptable after 4 months.
Example 18
Chicken Nuggets
[0163] Chicken nuggets containing microcapsules were prepared
according to the formulation shown in Table 12. Four batches were
prepared: a control, a batch containing 150 mg EPA+DHA per 100 g
serving, a batch containing 175 mg EPA+DHA per 100 g serving, and a
batch containing 300 mg EPA+DHA per 100 g serving.
Microencapsulated omega-3 oil (MEG-3.TM. powder from Ocean
Nutrition Canada; Dartmouth Canada) was added to soy protein, which
was then added to ground chicken meat. The mixture was stirred,
formed into nugget shapes, coated with a pre-dust, and then a
batter and breading was applied. The product was par-fried for 30
seconds at approximately 196.degree. C. to set the coating and the
color. The product was then transferred to the oven where it was
fully cooked at 177.degree. C. for approximately 3 minutes. For the
chicken nuggets containing the microcapsules the cider trim was
reduced to compensate for the added microcapsules. The final weight
of each batch was 400 kg. The final product was packaged in clear
plastic bags and stored frozen until consumption. The preparation
instructions for the product include reheating in the oven at
220.degree. C. for 10-15 minutes, microwaved, or deep-fried.
TABLE-US-00012 TABLE 12 Ingredients Quantity (kg) Cider trim 253.94
Skin and fat 14.50 Soy protein FX 213 20.25 Water 107.78 Salt 3.57
Total 400.00
[0164] The samples were evaluated monthly for sensory attributes,
color, and pH during a 12-month shelf life. The samples were
evaluated initially for difference from control and at the end of
shelf life for acceptability. The samples were also tested at the
beginning and end of shelf life for EPA+DHA and moisture
content.
[0165] The EPA+DHA and moisture contents of the nuggets remained
constant throughout the shelf life. No significant difference was
found between the nuggets containing 300 mg of EPA+DHA per serving
and the control, at the beginning of the shelf life. At the end of
the 12-month shelf life, panelists indicated that they "liked very
much" the nuggets containing 300 mg EPA+DHA per serving. The sample
nuggets had similar stability to the control nuggets. High levels
of EPA+DHA can be added per serving without affecting the sensory
and physical attributes of the nuggets or the overall
stability.
Example 19
Soymilk
[0166] Soymilk containing microcapsules was prepared using an
automatic soymilk maker. Two batches of soymilk were produced, one
control and one containing 250 mg EPA+DHA per 250 mL serving.
Specifically, 85 g of dry soybeans were soaked in tap water
overnight. The soaked beans were drained and rinsed. 1.5 L of water
was poured into the soymilk maker and the beans were placed in the
filter cup. The soymilk maker was then started. The soymilk was
collected and the spent beans discarded. The soymilk was cooled.
Microencapsulated omega-3 oil (MEG-3.TM. powder from Ocean
Nutrition Canada; Dartmouth Canada) was added and the soy milk was
pasteurized at 85.degree. C. for 5 sec. Pasteurization and addition
of MEG-3.TM. powder to plain soymilk helped to reduce beany
off-notes.
[0167] Three more batches of soymilk were produced as just
described: pasteurized soymilk, pasteurized soymilk with 1 cm.sup.3
salt and 30 cm.sup.3 sugar, pasteurized soy milk with
microencapsulated omega-3 oil, 1 cm.sup.3 salt and 30 cm.sup.3
sugar (the salt and sugar were added to the soymilk after
pasteurization). Pasteurized soy milk containing salt and sugar
tasted similar to commercial soymilks. The pasteurized soy milk
containing microcapsules, salt and sugar was slightly less sweet
but tasted better than the pasteurized soymilk containing no salt
and sugar.
[0168] Soymilk was an acceptable beverage for the addition of
microcapsules. No off-flavors or odors attributable to the powder
were observed, even at 250 mg EPA+DHA per serving. Some of the
typical soy beany flavor was masked by the microcapsules.
Example 20
Frozen Waffles
[0169] Frozen waffles containing microcapsules were prepared
according to the formulation shown in Table 13. Specifically, the
dry ingredients were blended together. Water, melted butter, and
vanilla were then added to the dry mix. After mixing the
ingredients together, the batter was placed onto oil brushed waffle
maker and baked for 70 seconds. The waffles were removed from the
waffle maker and placed into plastic pouches, separated by wax
paper, and frozen.
TABLE-US-00013 TABLE 13 Ingredients Weight (g) Real % Water 187.40
34.1965 All Purpose Flour 163.90 29.9082 Blueberry, low moisture
60.00 10.9487 Sugar 50.00 9.1239 Eggs, Fresh Liquid 47.00 8.5765
Butter, Unsalted 25.00 4.5620 Omega 3 4.36 0.7956 Vanilla Extract
3.35 0.6113 Blueberry Flavor, Natural 2.00 0.3650 Salt 2.00 0.3650
Baking Soda 2.00 0.3650 Sodium Aluminum 1.00 0.1825 Phosphate Total
1000.00 100.0000
[0170] The waffles had about 130 mg of EPA+DHA per 85 g serving.
Flavor in both levels were acceptable in first round tastings.
Plain and blueberry waffles were also prepared. An apple cinnamon
flavor was included in early development, but cinnamon seems to
enhance off flavors. Cinnamon should not be used as a flavor for
this type of product.
Example 21
Granola Cereal
[0171] Granola cereal containing microcapsules were prepared
according to the formulation shown in Table 14. Microencapsulated
omega-3 oil (MEG-3.TM. powder from Ocean Nutrition Canada;
Dartmouth, Canada) was blended with honey. The mixture was stirred
well and the mixture was allowed to hydrate. Vanilla was then added
to the mixture and mixed well. Brown sugar, flour, cinnamon, and
nonfat dry milk were slowly stirred for 1 minute. Oats, sunflower
seeds, almonds, and sesame seeds were then added. Raisins were
added at the end of baking to cooled granola. Oil was heated to
43.degree. C. and drizzled into a bowl while continuing to stir for
1 minute. The microcapsules, vanilla, and honey mixture were heated
to 60.degree. C. and drizzled into the mixture. After mixing for 2
minutes, the mixture was spread onto uncoated baking sheets. The
mixture was baked 121.degree. C. in a convection oven on low fan
for 30 minutes. The mixture was then tossed after 15 minutes. After
cooling, the granola was stored in an airtight container until
ready to use.
TABLE-US-00014 TABLE 14 Ingredients Weight (g) Real % Rolled Oats
240.97 48.19 Honey, Clover (60.degree. C.) 75.00 15.00 Canola Oil
(43.degree. C.) 40.00 8.00 Brown Sugar, granulated 30.00 6.00
Sunflower seeds 25.00 5.00 Whole Wheat flour 21.25 4.25 Almonds,
raw, sliced 20.00 4.00 Non fat dry milk 15.00 3.00 Sesame Seeds
12.50 2.50 Raisins, midgets 10.00 2.00 Vanilla Extract, 2X 3.75
0.75 Cinnamon, ground 3.75 0.75 Omega 3 2.78 0.56 Total 500.00
100.00
[0172] The granola cereal contained about 50 mg EPA+DHA per serving
(55 g). While fishy flavors were noticeable when the cereal was
fresh, this dissipated over 10-12 days. The cinnamon may have
accentuated the fishy flavors. Samples tasted in milk did not have
any off flavors.
Example 22
Gummy Candies
[0173] Gummy Candies containing microcapsules were prepared
according to the formulation shown in Table 15. Specifically,
sugar, corn syrup, microencapsulated omega-3 oil (MEG-3.TM. powder
from Ocean Nutrition Canada; Dartmouth Canada) and water were mixed
together in a cooking vessel. The mixture was brought to a boil at
118.degree. C. The mixture was removed from heat and cooled to
96.degree. C. Gum mucilage was vigorously stirred into the syrup to
create a homogenous blend. Gum mucilage was prepared by adding
gelatin to water and holding in a water bath at 60.degree. C. for
one hour or until the solution was clear. The solution was kept
warm (above 54.degree. C.) until ready for use in gummy candies.
Flavor, color and acid solution was added and the mixture was
blended well. The mixture was then placed in starch molds and
allowed to set for 48 hours at room temperature. The resulting
gummy were removed from the molds and lightly oiled with a 1:3
blend of mineral/coconut oil. The product was allowed to age for 2
days before packaging in a nitrogen purged, metallized film.
TABLE-US-00015 TABLE 15 Ingredient Quantity (g) Weight % Corn syrup
390.00 40.50 Sugar 300.00 31.15 Water 80.00 8.31 *Gum mucilage
Gelatin, 225 Bloom 55.00 5.71 Water 100.00 10.38 Apple flavor 5.00
0.52 Malic acid, 50% solution 25.00 2.60 Green food color 0.43 0.04
Omega-3 Powder 7.50 0.78 Total 962.93 99.99 *prepare separately
[0174] Gummy candies containing about 50, 100, and 130 mg EPA+DHA
per serving (40 g) were tried. Lower levels gave favorable results.
Also, different methods of addition of the microcapsules were
tried, such as soaking with gelatin in mucilage, boiling with
syrup, and boiling in water for 5 minutes prior to addition of
syrup. Addition of the microcapsules to the mucilage produced a
grainy texture and soft gel. Boiling of the microcapsules in water
prior to addition of syrup actually provided the best results.
Example 23
Pasta Sauce
[0175] Pasta sauce containing microcapsules were prepared according
to the formulation shown in Table 16. Specifically, the wet
ingredients were mixed together and the dry ingredients were mixed
together. The dry band wet mixtures were then combined. The mixture
was heated to 88.degree. C. and held at that temperature for 1
minute. The mixture was then poured into glass jars.
TABLE-US-00016 TABLE 16 Ingredients Weight (g) Weight % Tomatoes,
3/8'' diced 196.28 28.28 Water 230.00 33.13 Tomato puree 160.00
23.05 Sugar 39.00 5.62 Extra virgin olive oil 17.00 2.45 Onions,
diced 14.00 2.02 Beef base 8.00 1.15 Modified food starch 6.85 0.99
Basil, IQF 4.30 0.62 Salt 6.50 0.94 Onion powder 3.00 0.43 Garlic
puree 4.00 0.58 Citric acid, anhydrous 1.00 0.14 Black pepper 0.40
0.06 Omega-3 3.72 0.54 Total 694.05 100.00
[0176] Samples containing about 100 mg, 120 mg, and 130 mg EPA+DHA
per serving (125 g) were prepared. No fishy flavors were detected
at any levels initially or after 3 months of storage.
Example 24
Strawberry Yogurt Smoothie
[0177] A Strawberry Yogurt Smoothie (serving size of 8 fl oz; about
226 g) incorporating microencapsulated omega-3 fatty acids (1812TG
Omega-3 powder from Ocean Nutrition Canada, Ltd., Dartmouth,
Canada) was prepared according to the formulation in Table 17. The
product had a 130 mg dosage of EPA+DHA per serving.
TABLE-US-00017 TABLE 17 Ingredients Weight (g) Weight % Plain
Yogurt 438.24 43.82 Strawberry Puree, Seedless 110.62 11.06 Water
299.78 29.98 Liquid Fructose 143.81 14.38 Strawberry Flavor 0.93
0.093 Red Color 0.02 0.002 Dipotassium Phosphate 1.33 0.133 Omega-3
3.83 0.383 Pectin 1.44 0.144 Total 1000.00 100.00
[0178] Specifically, strawberry puree, water, liquid fructose,
strawberry flavor, and red color were mixed together in a pot.
Dipotassium phosphate, pectin, and the microcapsules were then
added to the wet ingredients. The mixture was heated to 88.degree.
C. and then cooled to room temperature. Yogurt was added next and
the mixture was again heated to 88.degree. C. The mixture was then
homogenized at a total pressure of 2,500 psi (first stage at 2,000
psi and second stage at 500 psi). The formulation was then placed
into bottles and stored refrigerated until use.
[0179] A second smoothie was prepared according to the formulation
in Table 6. Specifically, 1% milk, starch, gelatin, and whey
protein were mixed together. The microcapsules were then sprinkled
over the surface and allowed to hydrate for 5 minutes. The mixture
was then heated to 55.degree. C. and homogenized at a total
pressure of 2,300 psi (first stage at 1,800 psi and second stage at
500 psi). The homogenized formulation was then pasteurized at
86.degree. C. for 30 minutes and cooled to 38.degree. C. Yogurt
culture mixed with 2% milk was added to the homogenized/pasteurized
formulation and incubated at 38.degree. C. for approximately 10
hours, or until the mixture reached a pH of 4.5. The resulting
mixture was then mixed with a fruit preparation and heated to
88.degree. C. Then, the mixture was again homogenized at a total
pressure of 2,500 psi (first stage at 2,000 psi and second stage at
500 psi). The mixture was chilled and stored refrigerated until
ready to use.
TABLE-US-00018 TABLE 18 Ingredients Weight (g) Weight % Milk, 1%
milk fat 428.87 42.89 Starch 5.71 0.57 Whey Protein Isolate 1.99
0.20 Milk, 2% milk fat 1.64 0.16 Gelatin 1.19 0.12 Yo-Fast 17,
yogurt culture 0.13 0.01 Strawberry fruit prep 556.64 55.66 Omega-3
3.83 0.383 Total 1000.00 100.00
[0180] Both processes produced smoothies with acceptable flavor,
odor, and texture.
Example 25
Orange Juice
[0181] A batch of orange juice (18 servings; each serving size
being 250 g) incorporating microencapsulated omega-3 fatty acids
(1812TG Omega-3 powder from Ocean Nutrition Canada, Ltd.,
Dartmouth, Canada) was prepared according to the formulation in
Table 19. Specifically, the microcapsules were sprinkled on the
surface of orange juice in a blend tank equipped with an agitator
providing a minimum of 30 rpm. The juice was blended for 5 minute.
Afterwards, the juice was pasteurized at 91.degree. C. for 17
seconds with a flow rate of 212 L/minute. The pasteurized juice was
filled into gable top containers and stored refrigerated.
TABLE-US-00019 TABLE 19 Ingredients Weight (g) Weight % Orange
Juice 4500.00 99.74 Omega-3 Powder 11.88 0.26 Total 4511.88
100.00
[0182] The orange juice contained 100 mg of EPA+DHA (120 mg of
total omega-3 fatty acids) per serving. In taste tests there was no
perceptible difference in taste, texture, or quality between the
omega-3 orange juice and the control.
Example 26
Chocolate Frozen Dairy Dessert
[0183] A chocolate frozen dairy dessert (serving size of 1/2 cup;
about 118 mL) incorporating microencapsulated omega-3 fatty acids
(MEG-3 powder from Ocean Nutrition Canada, Ltd., Dartmouth, Canada)
was prepared according to the formulation in Table 20. The product
had a 100 mg dosage of EPA+DHA per serving.
TABLE-US-00020 TABLE 20 Ingredients Weight (g) Percent Chocolate
Ice Cream Non Fat Milk 750.00 59.88% Sugar 200.00 15.97% Heavy
Cream 150.00 11.98% MPC 80 70.000 5.59% Corn Syrup, Regular 42 DE
40.000 3.19% Cocoa Powder 24.000 1.92% Omega-3 Powder 7.00 0.56%
Chocolate Flavor 3.410 0.27% Stabilizer 3.00 0.24% Tricalcium
Phosphate 2.000 0.16% Probiotic Blend, 150 B/gm (from 3.000 0.24%
DSM; L10/L26 (50/50 Ratio)) Total 1252.41 100.00%
[0184] Specifically, all dry ingredients were blended except the
calcium phosphate and probiotic blend. The mixture of dry
ingredients was then combined with milk, cream, and corn syrup. The
mixture was stirred until smooth. Next, the mixture was heated to
72.degree. C. for 30 seconds. After cooling to about 4.degree. C.,
the mixture was aged for 24 hours under refrigeration. Chocolate
flavor and the remaining ingredients were then added and the
resulting mixture was placed in an ice cream freezer to the desired
overrun (target 70%). The ice cream was ejected from the freezer
and packed into individual containers, which were hard frozen
overnight.
[0185] The ice cream had a start weight per 4 fl. oz of 150, end
weight per 4 fl. oz of 90, and overrun of 67.00%. The ice cream had
100 mg of EPA+DHA per 118 mL serving. Further, each serving of the
ice cream contained 200,000,000 colony forming units (CFU) of
probiotic per serving.
[0186] The nutritional facts of the ice cream are as follows: 150
calories (45 from fat); 5 g of total fats (3 g from saturated fat;
0 g from trans fat); 20 mg of cholesterol; 40 mg of sodium; 19 g of
total carbohydrates (less than 1 g of dietary fiber; 18 g from
sugar); and 7 g of protein. The ice cream also contained 6% vitamin
A, 15% vitamin C, 15% calcium, and 4% iron, which are percent daily
values based on a 2000 calorie diet.
Example 27
Strawberry Frozen Dairy Dessert
[0187] A strawberry frozen dairy dessert (serving size of 1/2 cup;
about 118 mL) incorporating microencapsulated omega-3 fatty acids
(MEG-3 powder from Ocean Nutrition Canada, Ltd., Dartmouth, Canada)
was prepared according to the formulation in Table 21. The product
had a 100 mg dosage of EPA+DHA per serving.
TABLE-US-00021 TABLE 21 Ingredient Weight (g) Percent Non Fat Milk
750.00 54.21% Sugar 200.00 14.46% Strawberry, Sliced, Sweetened
155.000 11.20% Heavy Cream 150.00 10.84% MPC 80 70.000 5.06%
Strawberry Syrup 42.000 3.04% Omega-3 Powder 8.00 0.58% Stabilizer
3.00 0.22% Tricalcium Phosphate 2.000 0.14% Probiotic Blend, 150
B/gm (from 3.500 0.25% DSM; L10/L26 (50/50 Ratio) Total 1383.50
100.00%
[0188] Specifically, all dry ingredients were blended except the
calcium phosphate and probiotic blend. The mixture of dry
ingredients was then combined with milk and cream. The mixture was
stirred until smooth. Next, the mixture was heated to 72.degree. C.
for 30 seconds. After cooling to about 4.degree. C., the mixture
was aged for 24 hours under refrigeration. Strawberry syrup and the
remaining ingredients were then added and the resulting mixture was
placed in an ice cream freezer to the desired overrun (target 70%).
The ice cream was ejected from the freezer and packed into
individual containers, which were hard frozen overnight.
[0189] The ice cream had a start weight per 4 fl. oz of 150, end
weight per 4 fl. oz of 95, and overrun of 65.00%. The ice cream had
100 mg of EPA+DHA per 118 mL serving. Further, each serving of the
ice cream contained 200,000,000 colony forming units (CFU) of
probiotic per serving.
[0190] The nutritional facts of the ice cream are as follows: 150
calories (40 from fat); 4.5 g of total fats (2.5 g from saturated
fat; 0 g from trans fat); 20 mg of cholesterol; 35 mg of sodium; 21
g of total carbohydrates (0 g of dietary fiber; 18 g from sugar);
and 6 g of protein. The ice cream also contained 6% vitamin A, 20%
vitamin C, 15% calcium, and 0% iron, which are percent daily values
based on a 2000 calorie diet.
Example 28
Microwave Popcorn
[0191] Microwave popcorn (serving size of 30 g) incorporating
microencapsulated omega-3 fatty acids (MEG-3 powder from Ocean
Nutrition Canada, Ltd., Dartmouth, Canada) was prepared according
to the formulation in Table 22. The product had a 32 mg dosage of
EPA+DHA per serving.
TABLE-US-00022 TABLE 22 Ingredient Weight (g) Percent Popcorn 70.11
70.11% Hydrogenated Soybean Oil 25.50 25.50% Salt 3.00 3.00% Omega
3 Powder 0.75 0.75% Butter Flavor 0.60 0.60% Annatto 0.04 0.04%
Total 100.00 100.00%
[0192] Specifically, fat was melted at about 49.degree. C. While
stirring and maintaining heat, annatto color was then added to the
melted fat. In a separate container, all dry ingredients were
blended together. The dry ingredients were then added to the melted
fat. Popcorn was then placed into a microwave popcorn bag. The
fat-dry ingredient slurry, which contained the microencapsulated
omega-3 oil, was deposited into the bag (30 g per bag). The bag was
sealed and folded into thirds. The fat was allowed to harden.
Example 29
Country Style Baked Beans
[0193] Country style baked beans (serving size of 1/2 cup, about
130 g) incorporating microencapsulated omega-3 fatty acids (1812TG
powder from Ocean Nutrition Canada, Ltd., Dartmouth, Canada) was
prepared according to the formulation in Tables 23 and 24. The
product had a 32 mg dosage of EPA+DHA (0.2133 g powder) per
serving.
[0194] Basically, beans were rinsed well and soaked at ambient
temperature overnight in water (3.times. volume of beans). Next, a
large pot of water was brought to a boil. The beans were drained
and then added to the boiling water. The beans were boiled for 5
minutes. The boiling water was drained and the beans were rinsed
with cold water. The beans were then drained in a colander for 15
minutes before transferring to the cans.
[0195] The country style sauce was prepared according to the
formulation in Table 23.
TABLE-US-00023 TABLE 23 Ingredient Weight (g) Percent Water 721.00
75.700% Sugar 162.00 17.009% Modified Food Starch 20.00 2.100% Salt
15.00 1.575% Molasses 16.00 1.680% Pork Base 8.00 0.840% Onion
Powder 4.00 0.420% Omega 3 Powder 2.90 0.304% Caramel Color 1.50
0.157% Yellow Mustard Flour 1.00 0.105% Garlic Powder 1.00 0.105%
Cloves, ground 0.04 0.004% Yield: 100% 952.44 99.999%
[0196] The dry ingredients were weighed and then pre-blended in a
saucepan. Water was added to the dry ingredients in the saucepan
and the mixture was blended well. Molasses and pork base was added
next and the mixture was blended. The sauce was brought to a simmer
(>91.degree. C.) for 5 minutes to thicken the starch. The
saucepan was cooled in an ice water bath and brought to a 100%
yield. The sauce had a pH of 5.6 and brix of 22.5.
[0197] The beans were then prepared according to the formulation in
Table 24.
TABLE-US-00024 TABLE 24 Ingredient Weight (g) Percent County Style
Sauce (described in Table 23) 121.80 53.70% Navy Beans, soaked, 6
min blanch 92.00 40.56% Salt Pork, 1/2'' .times. 1'' chunk 13.00
5.73% Total 226.80 99.99%
[0198] Specifically, the beans were weighed into a can. The sauce
was also weighed into the can. The mixture was topped with a piece
of salt pork and the can was sealed. Water was added to a retort
and the cans were layered into the retort. The water was brought to
a boil and the retort lid was sealed. The retort vented with steam
escaping through a vent for 15 minutes and then a temperature gauge
was placed on top. Once the temperature reached 121.degree. C. (15
psi), the beans were retorted for 60 minutes. Heat was then removed
and the gauge was vented until ambient pressure was reached. The
lid was removed and the cans were transferred to an ice water bath.
After samples were cold, they were dried and stored under
refrigeration.
Example 30
Gummy Bears
[0199] Gummy bears (serving size of 2 g per gummy bear)
incorporating microencapsulated omega-3 fatty acids (MEG-3 powder
from Ocean Nutrition Canada, Ltd., Dartmouth, Canada) was prepared
according to the formulation in Table 25. The product had a 15 mg
dosage of EPA+DHA per 2 g serving.
TABLE-US-00025 TABLE 25 Ingredient Weight (g) At Deposit Percent At
Deposit Corn Syrup 30.000 24.300 31.14% 27.97% Sugar 26.000 26.000
26.98% 29.93% Water 10.000 6.217 10.38% 7.16% Gelatin - Gum
Mucilage 4.500 4.500 4.67% 5.18% (250 Bloom) Sorbitol 1.000 1.000
1.04% 1.15% Water - Gum Mucilage 16.000 16.000 16.61% 18.42% Omega
3 Fish Oil 4.650 4.650 4.83% 5.35% Blood Orange Flavor 0.800 0.800
0.83% 0.92% Blood Orange Oil Flavor 0.200 0.200 0.21% 0.23% Citric
Acid, 50% 1.800 1.800 1.87% 2.07% Solution Lactic Acid, 88% 1.200
1.200 1.25% 1.38% Orange Color 0.150 0.150 0.16% 0.17% Red Color
0.050 0.050 0.05% 0.06% Total 96.35 86.87 100.00% 100.00%
[0200] Specifically, the omega-3 powder was dispersed in water and
stirred until completely dissolved. Gelatin was added and melted in
a water bath at 77.degree. C. Next, sugar, corn syrup, and water
were weighed together in a cooking vessel. The mixture was brought
to a boil and the sides of the pot were washed of any crystals.
Boiling was continued until 90% solids (118.degree. C.). The pot
was removed from the heat and cooled to 96.degree. C. Gum mucilage
was added to and blended with the cooked syrup. Flavor, color, and
acid solution were added next and blended well. The resulting
mixture was deposited into dry starch molds and allowed to set for
48 hours at room temperature. The gummies were removed from the
molds and excess starch was brushed off. The gummies were brushed
lightly with capol and allowed to age for 2 days before packaging.
The cooked yield was 90.16%.
Example 31
Natural Lemon Chew
[0201] A natural lemon chew (serving size of 5.6 g) incorporating
microencapsulated omega-3 fatty acids (MEG-3 powder from Ocean
Nutrition Canada, Ltd., Dartmouth, Canada) was prepared according
to the formulation in Table 26. The product had a 100 mg dosage of
EPA+DHA per 5.6 g serving.
TABLE-US-00026 TABLE 26 Start End Finished Ingredients Wt (g) Wt
(g) Starting % % Dried Whipping Egg Whites 33.00 33.00 1.54% 1.61%
Water 55.50 55.50 2.59% 2.71% Invert Sugar 150.00 150.00 7.01%
7.33% Corn Syrup, 42 DE 75.00 75.00 3.51% 3.67% Sugar 690.00 690.00
32.25% 33.74% Corn Syrup, 42 DE 500.00 410.00 23.37% 20.05% Water
100.00 95.65 4.67% 4.68% Palm Oil, 102 mp 225.00 225.00 10.52%
11.00% Omega 3 Oil 250.00 250.00 11.69% 12.22% Malic Acid, Fine
Powder 24.00 24.00 1.12% 1.17% Citric Acid, Fine Powder 6.00 6.00
0.28% 0.29% Nat Lemon/Lime Flavor 18.00 18.00 0.84% 0.88% Lemon Oil
9.00 9.00 0.42% 0.44% Tumeric Powder 3.90 3.90 0.18% 0.19% Total
2139.40 2045.05 100.00% 100.00%
[0202] Specifically, in a mixer bowl with a whip attachment, egg
protein was solubilized in the first measure of water. In a
separate container, sugar and the first measure of corn syrup was
brought to a boil. The boiled syrup was slowly added to the mixer
bowl while mixing on low speed. After all syrup had been added, the
speed was increased to maximum speed and the mixture was whipped
until the volume was at maximum.
[0203] In another container, palm oil was melted to clarity and
combined with 80% of the omega-3 powder, until thickening began.
The resulting paste was stirred until all dry ingredients were
evenly coated with fat.
[0204] Sugar, the second measure of corn syrup, and water were
brought to a boil (126.degree. C.). Syrup was slowly poured into
the mixer bowl while mixing slowly. The omega-3 paste was added and
mixed until even. Acid, the remaining dry omega-3 powder, and
flavors were added next and mixed until even. The resulting mixture
was poured and formed as a slab on a cool surface. The product was
cut and wrapped. The product had a cooked yield of 95.59%.
Example 32
Orange Chew
[0205] An orange chew (serving size of 5.6 g) incorporating
microencapsulated omega-3 fatty acids (MEG-3 powder from Ocean
Nutrition Canada, Ltd., Dartmouth, Canada) was prepared according
to the formulation in Table 27. The product had a 100 mg dosage of
EPA+DHA per 5.6 g serving.
TABLE-US-00027 TABLE 27 Start End Finished Ingredient Wt (g) Wt (g)
Starting % % Dried Whipping Egg Whites 33.00 33.00 1.53% 1.60%
Water 55.50 55.50 2.57% 2.69% Invert Sugar 150.00 150.00 6.96%
7.27% Corn Syrup, 42 DE 75.00 75.00 3.48% 3.64% Sugar 690.00 690.00
32.00% 33.46% Corn Syrup, 42 DE 500.00 410.00 23.19% 19.88% Water
100.00 95.65 4.64% 4.64% Hydrogenated Palm Kernel 225.00 225.00
10.43% 10.91% Oil, 100 mp Omega 3 powder 250.00 250.00 11.59%
12.12% Malic Acid, Fine Powder 24.00 24.00 1.11% 1.16% Citric Acid,
Fine Powder 6.00 6.00 0.28% 0.29% Orange Flavor 27.00 27.00 1.25%
1.31% Oil of Orange Water Soluble 9.00 9.00 0.42% 0.44% Orange
Color, Liquid 12.00 12.00 0.56% 0.58% Total 2156.50 2062.15 100.00%
100.00%
[0206] Specifically, in a mixer bowl with a whip attachment, egg
protein was solubilized in the first measure of water. In a
separate container, sugar and the first measure of corn syrup was
brought to a boil. The boiled syrup was slowly added to the mixer
bowl while mixing on low speed. After all syrup had been added, the
speed was increased to maximum speed and the mixture was whipped
until the volume was at maximum.
[0207] In another container, palm oil was melted to clarity and
combined with 80% of the omega-3 powder, until thickening began.
The resulting paste was stirred until all dry ingredients were
evenly coated with fat.
[0208] Sugar, the second measure of corn syrup, and water were
brought to a boil (126.degree. C.). Syrup was slowly poured into
the mixer bowl while mixing slowly. The omega-3 paste was added and
mixed until even. Acid, the remaining dry omega-3 powder, and
flavors were added next and mixed until even. The resulting mixture
was poured and formed as a slab on a cool surface. The product was
cut and wrapped. The product had a cooked yield of 95.62%.
Example 33
Pasta
[0209] Pasta (serving size of 150 g) incorporating
microencapsulated omega-3 fatty acids (1812 TG powder from Ocean
Nutrition Canada, Ltd., Dartmouth, Canada) was prepared according
to the formulation in Table 28. The product had a 32 mg dosage of
EPA+DHA per 140 g serving.
TABLE-US-00028 TABLE 28 Ingredient Weight (g) Percent Durham Wheat
Flour 453.60 69.70% Whole Eggs 120.00 18.44% Water 75.00 11.52%
Omega 3 2.20 0.34% Total 650.80 100.00%
[0210] Flour and omega-3 powder were mixed together in one
container. Eggs and water were combined in a separate container.
The wet ingredients were slowly poured into the dry ingredients as
they were mixed in a mixer equipped with a dough hook. The
resulting dough was kneaded for about 30 seconds. The dough was
then covered with plastic wrap and allowed to stand for 45 minutes.
The dough was then sheeted into fettuccini sized noodles and dried
for from 20 minutes to 1 hour. To cook the noodles, water was
brought to a rolling boil and the noodles were added. After 3.5
minutes, the water was drained and the cooked noodles were rinsed
under cold water.
[0211] Other advantages which are obvious and which are inherent to
the invention will be evident to one skilled in the art. It will be
understood that certain features and sub-combinations are of
utility and may be employed without reference to other features and
sub-combinations. This is contemplated by and is within the scope
of the claims. Since many possible embodiments may be made of the
invention without departing from the scope thereof, it is to be
understood that all matter herein set forth or shown in the
accompanying drawings is to be interpreted as illustrative and not
in a limiting sense.
* * * * *