U.S. patent application number 13/783969 was filed with the patent office on 2013-07-11 for vitamin powder composition and method of making.
This patent application is currently assigned to DSM NUTRITIONAL PRODUCTS, INC.. The applicant listed for this patent is CHYI-CHENG CHEN, BRUNO LEUENBERGER. Invention is credited to CHYI-CHENG CHEN, BRUNO LEUENBERGER.
Application Number | 20130177619 13/783969 |
Document ID | / |
Family ID | 8239562 |
Filed Date | 2013-07-11 |
United States Patent
Application |
20130177619 |
Kind Code |
A1 |
CHEN; CHYI-CHENG ; et
al. |
July 11, 2013 |
VITAMIN POWDER COMPOSITION AND METHOD OF MAKING
Abstract
A powder composition containing at least one fat-soluble vitamin
dispersed in a matrix of a natural polysaccharide gum or a mixture
of gums having an emulsifying capacity and/or a protein or a
mixture of proteins having an emulsifying capacity. The fat-soluble
vitamin in the powder compositions is in the form of droplets
having an average diameter in the range of about 70 to about 200
nm. Tablets, beverages and beverage concentrates, foods, cosmetics
and pharmaceuticals containing the powder composition can be
made.
Inventors: |
CHEN; CHYI-CHENG;
(Binningen, CH) ; LEUENBERGER; BRUNO; (Allschwil,
CH) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
CHEN; CHYI-CHENG
LEUENBERGER; BRUNO |
Binningen
Allschwil |
|
CH
CH |
|
|
Assignee: |
DSM NUTRITIONAL PRODUCTS,
INC.
Parsippany
NJ
|
Family ID: |
8239562 |
Appl. No.: |
13/783969 |
Filed: |
March 4, 2013 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
09726880 |
Nov 30, 2000 |
8409617 |
|
|
13783969 |
|
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Current U.S.
Class: |
424/401 ; 424/61;
424/63; 424/70.13; 426/72 |
Current CPC
Class: |
A61K 9/1652 20130101;
A61K 9/1658 20130101; A23L 33/15 20160801; A23V 2002/00 20130101;
A61K 8/42 20130101; A61Q 5/02 20130101; A23L 2/02 20130101; A61Q
3/02 20130101; A23L 2/52 20130101; A61K 8/678 20130101; A23V
2002/00 20130101; A61Q 5/12 20130101; A61Q 1/00 20130101; A23V
2250/5028 20130101; A23V 2250/154 20130101; A23V 2250/714 20130101;
A23V 2250/712 20130101; A23V 2250/712 20130101; A23V 2250/154
20130101; A23V 2250/5028 20130101; A23V 2250/5432 20130101; A23V
2250/5432 20130101; A23V 2250/11 20130101; A23V 2250/702 20130101;
A23V 2250/5028 20130101; A23V 2250/21 20130101; A23V 2250/61
20130101; A23V 2250/5424 20130101; A23V 2250/5028 20130101; A23V
2250/5432 20130101; A23V 2250/5028 20130101; A23V 2250/21 20130101;
A23V 2250/5432 20130101; A23V 2250/7106 20130101; A23V 2250/5432
20130101; A23V 2002/00 20130101; A23V 2250/5072 20130101; A61K 8/02
20130101; A23V 2002/00 20130101; A23V 2002/00 20130101; A23V
2002/00 20130101; A61P 3/02 20180101; A61K 8/67 20130101; A61K
47/36 20130101; A61K 8/73 20130101; A61K 9/0007 20130101; A61Q
19/00 20130101 |
Class at
Publication: |
424/401 ; 426/72;
424/63; 424/61; 424/70.13 |
International
Class: |
A61K 47/36 20060101
A61K047/36; A23L 2/52 20060101 A23L002/52 |
Foreign Application Data
Date |
Code |
Application Number |
Dec 9, 1999 |
EP |
991245192 |
Claims
1. An emulsion for preparing a powder composition comprising
fat-soluble vitamin droplets dispersed in a matrix component,
wherein the droplets are about 70 to about 200 nm in diameter.
2. A beverage comprising a liquid admixed with a powder composition
comprising at least one fat-soluble vitamin, wherein a vitamin is
dispersed in a matrix comprising an emulsion-forming composition
selected from the group consisting of a natural polysaccharide gum,
a mixture of polysaccharide gums, a protein, a mixture of proteins,
and mixtures thereof, wherein the fat-soluble vitamin is present in
the powder composition in the form of droplets having an average
diameter of about 70 to about 200 nanometers (nm).
3. A beverage according to claim 2, wherein the beverage has an
optical clarity of no more than 20 NTUs when the beverage contains
up to 6 mg of the vitamin in 100 g of liquid.
4. A skin care product comprising a powder composition having at
least one fat-soluble vitamin, wherein a vitamin is dispersed in a
matrix comprising an emulsion-forming composition selected from the
group consisting of a natural polysaccharide gum, a mixture of
polysaccharide gums, a protein, a mixture of proteins, and mixtures
thereof, wherein the fat-soluble vitamin is present in the powder
composition in the form of droplets having an average diameter of
about 70 to about 200 nanometers (nm).
5. A skin care product according to claim 4, which is selected from
the group consisting of balms, lotions, sticks, ointments, make-up
compositions, shampoos, conditioners, and nail polishes.
6. A method for producing a powder composition comprising: (a)
combining water with a matrix component for a period of time
sufficient for the matrix component to dissolve in the water to
form a solution; (b) adding a fat-soluble vitamin to the solution
to form a crude emulsion; (c) emulsifying the crude emulsion at a
temperature of about 5.degree. C. to about 75.degree. C. at a
pressure of about 10,000 psi (about 680 bar) to about 60,000 psi
(about 4080 bar), to obtain a vitamin supplement emulsion
consisting of droplets with average diameter sizes of 70-200 nm;
and (d) drying the emulsion to obtain a powder composition.
7. A method according to claim 6 further comprising mixing the
crude emulsion until the size of the droplets within the emulsion
is about 1500 nm in diameter or less before the emulsifying
step.
8. A method according to claim 6, wherein the emulsifying step
occurs at a pressure of about 25,000 psi (about 1700 bar).
Description
CROSS REFERENCE OF RELATED APPLICATIONS
[0001] This application is a Divisional of U.S. application Ser.
No. 09/726,880, filed Nov. 30, 2000, which claims priority to
European Application No. 99124519.2 filed Dec. 9, 1999, each hereby
incorporated by reference in their entireties.
FIELD OF THE INVENTION
[0002] The present invention relates to new compositions,
especially powder compositions and emulsion compositions, useful to
produce nutritious vitamin and mineral supplemented beverages that
contain vitamin E and other fat-soluble vitamins.
BACKGROUND OF THE INVENTION
[0003] Sports beverages such as GATORADE.RTM., and vitamin
supplemented waters, are beverages where the addition of vitamins
is of interest. Also of interest are beverages used to restore
electrolytes lost through diarrhea, for example, Pedialyte.RTM..
Also of interest are carbonated beverages such as flavored seltzer
waters, soft drinks or mineral drinks, as well as non-carbonated
fruit and vegetable juices, punches and concentrated forms of these
beverages. In supplementing such beverages, it is often desirable
to preserve the optical clarity of the beverage. Fat-soluble
vitamins for supplementation are available in many forms, but when
added to beverages, will tend to increase the visible turbidity.
Ringing, i.e. the formation of a separate fat-soluble vitamin layer
on the top of the liquid, is also a problem which is often
encountered in fat-soluble vitamin fortification in beverages. One
means of adding fat-soluble vitamins to beverages without
significantly increasing turbidity or ringing is to encapsulate the
vitamins in liposomes. However, this is a costly process, and the
concentration of active substance in the liposome tends to be
low.
SUMMARY OF THE INVENTION
[0004] One object of the present invention is to provide a powder
composition of fat-soluble vitamins which can be added to beverages
in a restorative or nutritionally supplemental amount, preferably
without affecting the optical clarity of the beverage and without
altering the sensory properties of the beverage to which it is
added. In particular, the powder composition does not cause ringing
and enhances the bioavailability.
[0005] Another object of the present invention is an emulsion
composition comprising a fat-soluble vitamin, a matrix component as
defined herein below, and water.
[0006] Another object of the present invention is a tablet
containing the powder composition of this invention. The tablets of
this invention may be dissolved in a liquid without causing
ringing.
[0007] Another object of the present invention is a beverage, by
which is meant liquids intended for human or animal consumption,
containing the powder composition of this invention where the
fat-soluble vitamins are present in a nutritionally supplemental or
restorative amount. Another object of the present invention is a
method for producing the powder composition.
[0008] Another object of the invention is a food product containing
the powder composition of this invention.
[0009] Accordingly, one embodiment of the invention is a powder
composition containing at least one fat-soluble vitamin, wherein a
vitamin is dispersed in a matrix comprising an emulsion-forming
composition selected from the group consisting of a natural
polysaccharide gum, a mixture of polysaccharide gums, a protein, a
mixture of proteins, and mixtures thereof, wherein the fat-soluble
vitamin is present in the powder composition in the form of
droplets having an average diameter of about 70 to about 200
nanometers (nm).
[0010] Another embodiment is an emulsion for preparing a powder
composition that includes a fat-soluble vitamin droplets dispersed
in a matrix component, wherein the droplets are about 70 to about
200 nm in diameter.
[0011] A further embodiment is a beverage having a liquid admixed
with a powder composition containing at least one fat-soluble
vitamin, wherein a vitamin is dispersed in a matrix containing an
emulsion-forming composition selected from a natural polysaccharide
gum, a mixture of polysaccharide gums, a protein, a mixture of
proteins, and mixtures thereof, wherein the fat-soluble vitamin is
present in the powder composition in the form of droplets having an
average diameter of about 70 to about 200 nanometers (nm).
[0012] Another embodiment is a skin care product containing a
powder composition having at least one fat-soluble vitamin, wherein
a vitamin is dispersed in a matrix comprising an emulsion-forming
composition selected from a natural polysaccharide gum, a mixture
of polysaccharide gums, a protein, a mixture of proteins, and
mixtures thereof, wherein the fat-soluble vitamin is present in the
powder composition in the form of droplets having an average
diameter of about 70 to about 200 nanometers (nm).
[0013] Another embodiment is a method for producing a powder
composition, which method includes:
[0014] (a) combining water with a matrix component for a period of
time sufficient for the matrix component to dissolve in the water
to form a solution;
[0015] (b) adding a fat-soluble vitamin to the solution to form a
crude emulsion;
[0016] (c) emulsifying the crude emulsion at a temperature of about
5.degree. C. to about 75.degree. C. at a pressure of about 10,000
psi (about 680 bar) to about 60,000 psi (about 4080 bar), to obtain
a vitamin supplement emulsion consisting of droplets with average
diameter sizes of 70-200 nm; and
[0017] (d) drying the emulsion to obtain a powder composition.
[0018] Another embodiment is a composition to which a powder is
admixed to form a product containing a fat soluble vitamin, wherein
the powder has at least fat-soluble vitamin in the form of droplets
of about 70 to 200 nm in diameter, which is dispersed in a matrix
comprising an emulsion-forming material selected from the group
consisting of a natural polysaccharide gum, a mixture of natural
polysaccharide gums, a protein, a mixture of proteins, and a
mixture of a polysaccharide gum and a protein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 shows a flow diagram of the typical procedure for
preparation of a powder composition of this invention. 1-25 liter
Fryma process unit with integrated dissolve disc and colloid mill;
2--gear pump. max. 1,000 liters/hr. max. 100 bar. 3-microfluidizer,
M-210C-E/H, 100 liter/hr. max, 2,000 bar 4--heat exchanger with
cold water (ca. 10.degree. C.) 5--milk can 6--pump integrated to
Minor spray dryer 7--spray dryer Minor Model Hi-Tec.
[0020] FIG. 2 shows a graph of droplet size (nm) versus optical
clarity (NTU) for 15.75% (wt) vitamin E (circle) and 26.25% (wt)
vitamin E (square) in water dispersion.
DETAILED DESCRIPTION OF THE INVENTION
[0021] The present invention relates to a powder composition
containing at least one fat-soluble vitamin characterized in that
the vitamin is dispersed in a matrix of a natural polysaccharide
gum or a mixture of gums having an emulsifying capacity and/or a
protein or a mixture of proteins having an emulsifying capacity,
and wherein the fat-soluble vitamin is present in the powder
composition in the form of droplets having an average diameter
within the range of about 70 to about 200 nanometers (nm),
particularly about 70 to about 150 nm.
[0022] A preferred powder of this invention includes fat-soluble
vitamin droplets with an average diameter within the range of about
80 to about 120 nm. Most preferred is an average droplet size of
about 100 nm in diameter.
[0023] The powder composition may include a single vitamin, or more
than one vitamin. The vitamin may be in pure form, or it may be in
a diluent such as an edible oil. Powder compositions of this
invention contain vitamin droplets of a very small size. As a
result, the compositions can be added to a liquid without causing
ringing. In addition, bioavailability is improved. Also, preferred
compositions of this invention may be added to a clear liquid
without significantly increasing its turbidity.
[0024] The powder of this invention is made up of particles that
include at least one fat-soluble vitamin dispersed in a matrix
containing at least one natural polysaccharide gum or at least one
protein with emulsifying capacity. The natural polysaccharide gum
or the protein with emulsifying capacity, when used as matrix
materials in the present invention, are also referred to as
"matrix" or "matrix component(s)." These particles may be of
various sizes, but all of them are at least sufficiently large to
have a structure throughout which individual droplets of the
fat-soluble vitamin are distributed. These particles may be as
large as several hundred microns. The vitamin droplets have an
average size within the range of about 70 to about 200 nm in
diameter or even less. The droplets may contain a fat-soluble
vitamin in a pure form, or a fat-soluble vitamin in a suitable
medium or diluent such as an edible oil. The droplets may also
contain a mixture of two or more different fat-soluble vitamins.
When the powder is added to a liquid, the predominant structure of
the resulting droplets within the liquid is a vitamin core sheathed
by the matrix component interface between vitamin and the aqueous
medium.
[0025] Droplet size is conveniently determined by a light
scattering technique using an instrument such as Malvern ZetaSizer
3, which provides an average droplet size (the "Z" average). This
method is known in the art and described in various references, for
example in Particle Size Distribution, ACS Symposium Series 332,
Ed. T. Provder, American Chemical Society, Washington, D.C. (1987).
Thus, a powder composition of this invention contains droplets
consisting of the fat-soluble vitamin with an average droplet size
of about 70 to about 200 nm in diameter as measured by the
technique of light scattering.
[0026] As used herein, the terms "droplet size" and "particle size"
both refer to the diameter of the respective droplet or particle,
unless otherwise specifically noted.
[0027] Optical clarity may be estimated by a visual comparison,
such that if there is no significant visible added turbidity, the
liquid has retained its optical clarity. Optical clarity
(turbidity) can be accurately measured by a turbidimeter. To
determine the turbidity, a sample is dispersed, with stirring, in
water or a beverage. After complete dispersion, which usually takes
a few minutes or more (up to complete dispersion as determined
below), the turbidity of the resulting liquid is measured using a
turbidimeter as is available from Orbeco Analytical Systems, Inc.,
Farmingdale, N.Y. Complete dispersion is indicated when a constant
turbidity reading is obtained. Turbidity is measured by directing a
beam of light into a cell containing the test sample, measuring the
amount of light that is reflected at a 90 degree angle by any
droplets present in the sample and comparing it to the light
scattered by a standard reference suspension. The intensity of the
light reflected at 90 degrees is measured by a suitable
photodetector, amplified and displayed on a digital readout. The
amount of reflected light is directly proportional to the degree of
turbidity. NTU (Nephelometric Turbidity Unit) is customarily used
to describe the results from the turbidity measurement using a
turbidimeter. Higher NTU means higher turbidity.
[0028] Any standard turbidimeter will provide equivalent NTU
measurements. For purposes of this invention, an NTU of ten or less
is optically clear. For example, the NTU of most commercial apple
juices investigated is about 5. An optically clear liquid to which
a preferred powder composition of this invention has been added
will preferably have a resulting NTU of no more than forty NTUs,
and preferably ten to twenty NTUs. The compositions of this
invention may also be added to liquids that are not optically
clear. In this regard, increase in turbidity is not of concern.
Ringing will not occur. Also, bioavailability of the vitamin may be
increased. The invention contemplates powder compositions which,
when added to a liquid, provide vitamin droplets averaging about 70
to about 200 nm in diameter, preferably about 70 to about 150 nm,
more preferably about 80 to about 120 nm, and most preferably about
100 nm. When the liquid is optically clear, then the liquid remains
for all practical purposes optically clear after addition of a
powder composition according to this invention.
[0029] The natural polysaccharide gums and/or the proteins with
emulsifying capacity as used in this invention are defined herein
below. The polysaccharide gum and/or the protein, as used in this
invention both have sufficient emulsifying properties. This means
that they have sufficient emulsifying properties in an oil-in-water
context to emulsify the oil into a fine dispersion in an aqueous
medium and are capable of forming a stable emulsion of a desired
droplet size (for example 70-200 nm) under conditions of high
pressure homogenization. As used herein, "high pressure" means a
pressure of about 10,000 psi (about 680 bar) to about 60,000 psi
(about 4080 bar). Even higher pressures may be used, if required.
Natural polysaccharide gums with emulsifying capacity and proteins
to be used in the present invention are known and are commercially
available, or may be isolated by a skilled person using
conventional methods. Polysaccharide gums have been described for
example in Industrial Gums, (3.sup.rd Ed., Academic Press, Inc.,
1993).
[0030] Whether a selected polysaccharide gum or a protein to be
used according to the present invention has an emulsifying capacity
sufficient to be used for performing the present invention may be
easily determined by assaying whether or not the selected
polysaccharide gum and/or protein can maintain an emulsion as
defined above, and as further described herein below.
[0031] Briefly, one starts with a crude emulsion made by dissolving
the matrix component in a suitable aqueous solvent such as water
and during homogenization adding fat-soluble vitamins in such
proportions as to produce a crude emulsion with a solids content
(percent by weight of vitamin(s) and matrix component) of
preferably no more than 60%. A solids content of 70% is possible,
however it may be difficult to process due to the thickness of the
emulsion. The amount of lipid, or lipid content, is the lipid
component of the solids content. The lipid component may be pure
vitamin or vitamin in an appropriate diluent. The lipid content
preferably makes up 75% by weight or less of the solids content. If
the resulting emulsion has an average emulsion droplet size of
about 70 to about 200 nm, after one cycle up to about one hundred
cycles of emulsification (passes) at a pressure of about 10,000 to
60,000 psi (about 680 to about 4080 bar), then the matrix component
is suitable to be used in this invention. The matrix component
should also produce an emulsion that remains stable at least until
the performance of the next preparation step, which preferably is
spray drying.
[0032] Preferably, the matrix component should be at least
acceptable for animal consumption. For human consumption, preferred
matrix components should be GRAS (generally recognized as safe) or
are an approved material for food consumption as determined by the
various regulatory agencies worldwide.
[0033] As used herein, a "natural polysaccharide gum having an
emulsifying capacity" is a polysaccharide gum which originates from
plants, animals or microbial sources and which has not been
intentionally subjected to chemical modifications to alter its
chemical structure. All gums such as exudate gums, seaweed gums,
seed gums or microbial gums may be used to perform the present
invention provided they have an emulsifying capacity and, depending
on the use contemplated, are at least acceptable for animal
consumption or preferably are GRAS or are an approved material for
food consumption as determined by the various regulatory agencies
worldwide.
[0034] Examples of natural polysaccharide gums include gum arabic,
flaxseed gum, ghatti gum, tamarind gum and arabinogalactan.
Preferred are gum arabic, gum ghatti and arabinogalactan. Most
preferred is gum arabic. These gums have a sufficient emulsifying
action for use in the present invention. These gums lower the
interfacial tension in oil-in-water emulsions and, at the same
time, increase the viscosity of the aqueous phase.
[0035] Generally, it is difficult to handle aqueous solutions of
polysaccharide gums at higher concentrations than 5%. There are,
however, exceptions. Gum arabic, for example, dissolves rather
quickly when stirred into water at concentrations higher than 5%.
Quality grade of gum arabic yields colorless, bland-tasting
solutions.
[0036] Industrial gums useful for carrying out the present
invention may contain varying amounts of added substances such as
inorganic salts. Product specifications often vary according to
plant origin, production method or intended application. For the
expert in the art, such variations are normal and present no
problem in applying such gums according to the present
invention.
[0037] The matrix component of the present invention may be a
natural polysaccharide gum with emulsifying capacity. The natural
polysaccharide gum may be mixed with a protein having emulsifying
capacity or, alternatively, a protein alone having emulsifying
capacity may be used as a matrix component wherein the fat-soluble
vitamin is present in the form of droplets having an average
diameter within the range of about 70 to about 200 nanometers
(nm).
[0038] Proteins as used in the present invention are defined as
polypeptides, which originate from plant or animal sources and
possess emulsifying capacity, e.g. gelatine, plant proteins and
milk proteins. Such proteins are known in the art. The proteins may
be of vegetable (plant) or animal origin. Examples of such proteins
include sunflower proteins, soy-bean proteins, cotton seed
proteins, peanut proteins, rape seed proteins, milk proteins, blood
proteins, egg proteins, and acetylated derivatives thereof, and
gelatine or crosslinked gelatine. Preferred are gelatine and milk
proteins. Gelatines may be extracted from skins or bones by acid or
base hydrolysis, and therefore herein are not named "natural." In
this sense, the term "gelatine" includes also suitable chemical
derivatives thereof such as acetylated gelatine or crosslinked
gelatine.
[0039] The matrix component may include a natural polysaccharide
gum with emulsifying capacity or a mixture of different natural
polysaccharide gums having emulsifying capacity without the
admixture of any proteins. Alternatively, the matrix may include a
protein with emulsifying capacity or a mixture of such proteins of
different origins without the admixture of any natural
polysaccharide gum.
[0040] The matrix may further include a mixture of (i) a natural
polysaccharide gum with emulsifying capacity or a mixture of such
natural polysaccharide gums of different origins together with (ii)
a protein with emulsifying capacity or a mixture of such proteins
of different origins. In this case, the ratio of component (i) to
component (ii) is not critical and is a matter of optimization.
Therefore, the ratio of component (i) to component (ii) may be
within the ratio of 1:99 to 99:1. It is, however, preferred that
the matrix include either a natural polysaccharide gum or a mixture
of gums only as described or a protein or a mixture of proteins
only as described. Potentially, interactions between
polysaccharides and proteins may occur and, depending on the
processing conditions, especially on the processing pH, may reduce
or even destroy the emulsifying property. This is easily determined
by one skilled in the art, who is able to choose the correct
mixture and the optimized processing conditions when using such a
mixture.
[0041] As fat-soluble vitamins, vitamin E or its esters (for
example vitamin E acetate), vitamin A or its esters (for example
vitamin A acetate and vitamin A palmitate), vitamin K
(phytomenadione) and vitamin D.sub.3 (cholecalciferol) are
contemplated in the present invention. Vitamin E or its esters is
the preferred fat-soluble vitamin, with vitamin E acetate being
most preferred. Such vitamins are readily available from commercial
sources. Also, they may be prepared by conventional methods by a
skilled person. Vitamins may be used in pure form, or in a suitable
diluent such as a fat or edible oil (e.g. soybean oil). Thus the
droplets in the powder of this invention may contain one or more
vitamins in a pure state or in an appropriate diluent.
[0042] Thus, a preferred powder composition includes droplets of a
fat-soluble vitamin which are dispersed in a matrix component as
described above, wherein
[0043] (i) the droplets have an average diameter within the range
of about 70 to about 200 nm, preferably about 70 to about 150 nm,
more preferably about 80 to about 120 nm, most preferably about 100
nm;
[0044] (ii) the fat-soluble vitamin is selected from the group
consisting of vitamin E or its esters, vitamin A or its esters,
vitamin K, and vitamin D.sub.3; and
[0045] (iii) the matrix component includes a natural polysaccharide
with emulsifying capacity gum or a protein with emulsifying
capacity.
[0046] Most preferably, the fat-soluble vitamin is vitamin E
acetate and the matrix is selected from gum arabic, gum ghatti, and
gelatine, preferably from gum arabic or gelatine, and preferably
from gum arabic.
[0047] The composition of this invention may include from about
0.5% to 75% by weight of fat-soluble vitamin (the "potency" of the
composition) and from about 99.5% to 25% by weight of a matrix
component, on a dry weight basis, the total weight of the
components adding up to 100% by weight.
[0048] A preferred percent of fat-soluble vitamin is from about 15%
to about 40%, most preferably about 25% by weight, based on the
total weight of all the components present in the composition,
whereby the composition as a final powder product usually has a
moisture content of about 1-3% by weight.
[0049] The composition may contain only vitamin and matrix
components in percentages that add up to 100%. The composition may
also contain a small amount of residual water. The amount of
residual water depends on the drying technology used, which will be
evident to a skilled practitioner. A typical amount of residual
water is up to about 4.0% by weight. Alternatively, other
ingredients standard to a vitamin powder composition may be added.
For example, vitamin protectors such as sucrose or maltodextrin
alone or in combination, and/or antioxidants may be added. The
amounts of vitamin and matrix component may then be adjusted
accordingly. Part of this invention therefore is also a composition
where the ratio of fat-soluble vitamin to matrix component is from
about 1:99 to about 3:1. A preferred composition includes from
about 15% to about 40% by weight of fat-soluble vitamin and from
about 60% to 85% by weight of a matrix component. A preferred ratio
of fat-soluble vitamin to matrix component is about 1:8 to 1:1,
preferably about 1:5.7 to 1:1.5. In a particularly preferred
composition, the fat-soluble vitamin is vitamin E or vitamin E
acetate and the matrix component is gum arabic or gelatine,
especially gum arabic.
[0050] Another embodiment of this invention is an emulsion
composition which includes a fat-soluble vitamin; a matrix
component as defined above, optionally a preservative and water,
wherein the droplets of the emulsion are no more than about 70 to
about 200 nanometers in diameter.
[0051] A preferred emulsion of 5% to about 20% by weight of the
fat-soluble vitamin, preferably about 7.5% to about 20%; about 30%
to 40% by weight of the matrix component, and about 50% to about
55% of water, wherein the weight-% of all the components add up to
100%.
[0052] This emulsion is useful for preparing the powder composition
of the present invention. The preferred matrix component is as
defined above. A preferred vitamin is vitamin E and its acetate.
When other components such as preservatives are included, the
percent vitamin, matrix component, and water is adjusted
accordingly.
[0053] Tablets, in particular effervescent tablets, are part of the
present invention. Such tablets include a fat-soluble vitamin and
the matrix component as defined above, and are preferably obtained
from a powder composition according to this invention and as
described herein by formulating the composition into effervescent
tablets by conventional tabletting means. When added to a liquid
such as water, mineral water, or a beverage, the tablet dissolves
and provides a liquid whose fat-soluble vitamin contents do not
cause ringing, by which is meant separation of a top fat-soluble
vitamin layer on the liquid. The tablets of this invention may be
produced from any powder composition described herein, for example
compositions wherein the preferred matrix is a gum as defined
above, especially gum arabic, arabinogalactan, gum ghatti, or
gelatine, preferably gum arabic and a preferred vitamin is vitamin
E and its acetate.
[0054] This invention is also directed to a beverage containing a
powder composition or an emulsion as described above. The present
invention is also directed to beverages containing a mixture
of:
[0055] (i) a matrix component as defined above, and a nutritionally
supplemental amount of a fat-soluble vitamin in the form of
droplets which average from about 70 to about 200 nm in diameter,
preferably about 70 to about 150 nm in diameter; and
[0056] (ii) a liquid containing juice and/or water, and,
optionally, a flavor, to bring the beverage weight to 100%.
[0057] Preferred are beverages as described above, wherein
[0058] (i) the fat-soluble vitamin is selected from the group of
vitamin E or its esters, vitamin A or its esters, vitamin K, and
vitamin D.sub.3; and
[0059] (ii) the matrix is a gum or a protein as described above,
especially gum arabic, arabinogalactan, gum ghatti, or gelatine,
preferably gum arabic or gelatine.
[0060] Most preferred is a beverage wherein the fat-soluble vitamin
is vitamin E acetate and the matrix is gum arabic or gelatine. A
preferred amount of the vitamin in such a composition is from about
2 to 12 mg of vitamin E per 100 grams of liquid. An especially
preferred amount is 3.2 to 8.0 mg of vitamin E per 100 grams. Most
preferred is about 6.0 mg per 100 grams.
[0061] The liquid for a typical beverage may be about 3% (wt) fruit
juice and 97% (wt) water, or 0.05% (wt) flavor, 1.95% (wt) fruit
juice, and 98% (wt) water. Sweeteners, preservatives, stabilizers,
and other known beverage components may be included in the
beverage. When these components are included, the percentage of
juice, flavor, and water are adjusted accordingly.
[0062] In the case of clear beverages, the preferred beverage
should have an optical clarity which does not differ significantly
from its optical clarity before addition of the powder, for
example, which does not appear significantly more turbid on visual
inspection.
[0063] This invention is also directed to a beverage including a
mixture of:
[0064] (i) a nutritionally supplemental amount of a fat-soluble
vitamin, and a matrix component as defined herein above,
[0065] (ii) a liquid containing juice and/or water, and,
optionally, a flavor, to bring the beverage weight to 100%, and
[0066] (iii) which beverage has an optical clarity of no more than
20 NTUs when containing up to 6 mg of vitamin per 100 g of
liquid.
[0067] The beverages of this invention are preferably obtained by
adding to a beverage a powder composition of this invention. Adding
a powder composition of this invention to a liquid requires no
special procedure or extensive mixing. The powder may simply be
added to the liquid and mixed by shaking or stirring until the
powder particles are no longer visible to the naked eye. One or
more of the powder compositions of this invention may be added to a
beverage as described herein, to obtain a beverage, e.g. a
fortified beverage. For example, the fat-soluble vitamin may be one
or more of vitamin E or its esters, vitamin A or its esters,
vitamin K, and vitamin D.sub.3, especially vitamin E and vitamin E
acetate. The matrix may be as defined above including the preferred
matrix components.
[0068] Fat-soluble vitamins may be added in a restorative amount,
i.e. in an amount sufficient to replace the vitamin naturally
present in a beverage such as juice or milk, which vitamin has been
lost or inactivated during processing. Fat-soluble vitamins may
also be added in a nutritionally supplemental amount, i.e. in an
amount considered advisable for a child or adult to consume based
on RDAs and other such standards, preferably from about one to
three times the RDA (Recommended Daily Amount). A nutritionally
supplemental amount of fat-soluble vitamin may be readily
determined by a skilled person to obtain the desired amount of
fortification in a liquid, e.g. a beverage, and based on RDAs and
other such standards. A preferred amount of vitamin E is from about
2 to 12 mg of vitamin E per 100 grams of liquid. An especially
preferred amount is 3.2 to 8.0 mg per 100 grams of liquid. Most
preferred is about 6.0 mg per 100 grams of liquid. Thus, the powder
compositions of this invention may be added to a beverage to
provide a vitamin E concentration of from about 2 to 12 mg or 3.2
to 8.0 mg per 100 grams of liquid. In the case of fat-soluble
vitamins which have greater potency than vitamin E, it is preferred
to formulate the powder composition such that 2 to 12 mg of such a
vitamin per 100 grams in diluent (e.g. edible oil) may be added.
This means that the vitamin is diluted in diluent so that 2 to 12
mg of vitamin per 100 g in diluent provides a suitable
nutritionally supplemental amount, for example a multiple of the
RDA, preferably 1 to 3 times the RDA. For example, the RDA for
vitamin D.sub.3 is 400 IU. Thus, a vitamin D.sub.3 composition of
this invention would preferably contain 15% to 40% by weight of 400
IU of vitamin D.sub.3 in diluent. The same would apply to other
fat-soluble vitamins. Alternatively, the vitamin itself in
undiluted form may be used to make the powder composition. Whether
or not dilution is necessary will depend on the potency of the
vitamin.
[0069] The amount of powder composition to be added depends on the
potency of the powder, i.e. the amount of vitamin in the powder,
which in this invention can range from about 0.5% to about 75% by
weight. Preferred powders have a potency of about 25% (wt) to about
40% (wt). Powders with smaller droplet sizes will in general
generate less turbidity in liquid. Based on the droplet size and
the desired level of fortification and turbidity, the skilled
person should be able to determine the amount of powder to add,
depending on its potency, to attain desired optical clarity. If a
beverage to be supplemented is already turbid, then an increase in
NTUs is less likely to be of concern, and a higher range of added
turbidity can be accommodated.
[0070] The beverages of this invention may be carbonated beverages,
e.g. flavored seltzer waters, soft drinks or mineral drinks, as
well as non-carbonated juices, punches and concentrated forms of
these beverages. Beverages, especially juice and cola beverages,
which are carbonated in the manner of soft drinks, as well as
"still" beverages, nectars, and full-strength beverages or beverage
concentrates which contain at least about 45% by weight of juice
are also contemplated.
[0071] The fruit juices and fruit flavors used herein include
grape, pear, passion fruit, pineapple, banana or banana puree,
apricot, orange, lemon, grapefruit, apple, cranberry, tomato,
mango, papaya, lime, tangerine, cherry, raspberry, carrot, and
mixtures thereof. Additionally, artificial flavors, e.g. cola, or
natural flavors derived from these juices may be used in the
beverages. Chocolate flavors and other non-fruit flavors may also
be used to make beverages containing the vitamin and mineral
supplement. Additionally, milk, obtained from cows or synthetic, is
a contemplated beverage to to which the powder compositions of this
invention may be added. The milk may itself include other beverage
components, in particular flavors such as chocolate, coffee, or
strawberry. As used herein, the term "juice product" refers to both
fruit and vegetable juice beverages, and fruit and vegetable juice
concentrates which comprise at least about 45% (wt) fruit juice. As
used herein, the term "vegetable" means both nonfruit, edible plant
parts, such as tubers, leaves, rinds, and also, if not otherwise
indicated, any grains, nuts, beans, and sprouts which are provided
as juices or beverage flavorings.
[0072] Sport beverages are also contemplated as beverages which can
be supplemented by the powder compositions of the present
invention. Typical sport beverages contain water, sucrose syrup,
glucose-fructose syrup, and natural or artificial flavors. These
beverages may also contain citric acid, sodium citrate, and
monopotassium phosphate, as well as other materials which are
useful in replenishing electrolytes lost during perspiration.
[0073] As used herein, the term "juice beverage" refers to a fruit
or vegetable juice product which is in a single-strength,
ready-to-serve, drinkable form. Juice beverages of the present
invention may be of the "full-strength" type which typically
contain at least about 95% (wt) juice. Full strength juice
beverages also include those products of 100% (wt) juice such as,
for example, orange, lemon, apple, raspberry, cherry, apricot,
pear, grapefruit, grape, lime, tangerine, carrot, pineapple, melon,
mango, papaya, passion fruit, banana and banana puree, cranberry,
tomato, carrot, cabbage, celery, cucumber, spinach, and various
mixtures thereof. Juice beverages also include extended juice
products which are referred to as "nectars." These extended juice
products typically comprise from about 50% (wt) to about 90% (wt)
juice, preferably from about 50% (wt) to about 70% (wt) juice.
Nectars usually have added sugars or artificial sweeteners or
carbohydrate substitutes. As used herein, the term "citrus juice"
refers to fruit juices selected from orange juice, lemon juice,
lime juice, grapefruit juice, tangerine juice, and mixtures
thereof.
[0074] As used herein, the term "juice materials" refers to
concentrated fruit or vegetable juice, plus other materials such as
juice aroma and flavor volatiles, peel oils, and pulp or pomace. As
used herein, the term "juice concentrate" refers to a fruit or
vegetable juice product which, when diluted with the appropriate
amount of water, forms drinkable juice beverages. Juice
concentrates within the scope of the present invention are
typically formulated to provide drinkable beverages when diluted
with 3 to 5 parts by weight water.
[0075] As used herein the term "beverage concentrate" or "bottling
syrup" refers to a mixture of flavors, water and from about 10%
(wt) to about 60% (wt) sugar or carbohydrate substitute, i.e.
sucrose, dextrose, corn syrup solids, fructose, dextrins,
polydextrose, and mixtures thereof.
[0076] The flavor component of the beverages and beverage
concentrates contains flavors selected from fruit flavors,
vegetable flavors, botanical flavors and mixtures thereof. As used
herein, the term "fruit flavor" refers to those flavors derived
from the edible reproductive part of a seed plant, especially one
having a sweet pulp associated with the seed, and "vegetable
flavor" refers to flavors derived from other edible parts of the
seed and other plants. Also included within the term "fruit flavor"
and "vegetable flavor" are synthetically prepared flavors made to
simulate fruit or vegetable flavors derived from natural sources.
Particularly preferred fruit flavors are the citrus flavors
including orange, lemon, lime and grapefruit flavors. Besides
citrus flavors, a variety of other fruit flavors may be used, such
as apple, grape, cherry, pineapple, mango, papaya flavors, and the
like. These fruit flavors may be derived from natural sources such
as juices and flavor oils, or may be synthetically prepared. As
used herein, the term "botanical flavor" refers to flavors derived
from parts of a plant other than the fruit, i.e. derived from nuts,
bark, roots and leaves, and beans such as coffee, cocoa, and
vanilla. Also included within the term "botanical flavor" are
synthetically prepared flavors made to simulate botanical flavors
derived from natural sources. Examples of such flavors include
cola, tea, coffee, chocolate, vanilla, almond, and the like.
Botanical flavors may be derived from natural sources such as
essential oils and extracts, or may be synthetically prepared.
[0077] The flavor component may include a blend of various flavors,
e.g. lemon and lime flavors, cola flavors and citrus flavors to
form cola flavors, etc. If desired, juices such as orange, lemon,
lime, apple, grape, carrot, celery, and like juices may be used in
the flavor component. The flavors in the flavor component are
sometimes formed into emulsion droplets which are then dispersed in
the beverage concentrate. Because these droplets usually have a
specific gravity less than that of water and would therefore form a
separate phase, weighting agents (which may also act as clouding
agents) are typically used to keep the emulsion droplets dispersed
in the beverage. Examples of such weighting agents are brominated
vegetable oils (BVO) and rosin esters, in particular the ester
gums. See L. F. Green, Developments in Soft Drinks Technology, Vol.
1, (Applied Science Publishers Ltd. 1978), pp. 87-93, for a further
description of the use of weighting and clouding agents in liquid
beverages.
[0078] Besides weighting agents, emulsifiers and emulsion
stabilizers may be used to stabilize the emulsion droplets. The
particular amount of the flavor component effective for imparting
flavor characteristics to the beverages and beverage concentrates
("flavor enhancing") may depend upon the flavor(s) selected, the
flavor impression desired, and the form of the flavor component.
The flavor component may include at least 0.05% by weight of the
beverage composition, and typically from 0.1% to 2% by weight for
carbonated beverages. When juices are used as the flavor, the
flavor component may include, on a single-strength basis, up to 25%
fruit juice by weight of the beverage, preferably from 5% to 15%
juice by weight for carbonated beverages.
[0079] Carbon dioxide may be introduced into the water which is
mixed with the beverage syrup or into the drinkable beverage after
dilution to achieve carbonation. The carbonated beverage may be
placed into a container, such as a bottle or can, and is then
sealed. Any conventional carbonation methodology may be used to
make the carbonated beverages of this invention. The amount of
carbon dioxide introduced into the beverage will depend upon the
particular flavor system used and the amount of carbonation
desired. Usually, carbonated beverages of the present invention
contain from 1.0 to 4.5 volumes of carbon dioxide. The preferred
carbonated beverages contain from 2 to about 3.5 volumes of carbon
dioxide.
[0080] The present invention is also particularly suited for the
supplementation of beverages and beverage concentrates, including
citrus juices. The beverages may contain from 3% (wt) to 100% (wt)
juice or from about 0.05% (wt) to about 10% (wt) of an artificial
or natural flavor, particularly orange juice. The concentrated
orange juice, orange juice aroma and flavor volatiles, pulp and
peel oils used in the method of the present invention may be
obtained from standard orange juice. See Nagy et al, Citrus Science
and Technology, Volume 2, (AVI Publishing Co. 1977), pp. 177-252
for standard processing of oranges, grapefruit and tangerines. (See
also Nelson et al, Fruit and Vegetable Juice Processing Technology
(3rd Ed., AVI Publishing 1980), pp. 180-505 for standard processing
of noncitrus juices such as apple, grape, pineapple, etc. to
provide sources of juice and juice materials for noncitrus juice
products).
[0081] Juices from different sources are frequently blended to
adjust the sugar-to-acid ratio of the juice. Different varieties of
oranges may be blended or different juices may be blended to get
the desired flavor and sugar-to-acid ratio. A sugar-to-acid ratio
of from about 8:1 to about 20:1 is considered acceptable for fruit
juices. However, preferred sugar-to-acid ratios are typically from
about 11:1 to about 15:1, especially for citrus juices.
[0082] Sweeteners include the sugars normally present in juice
products, for example glucose, sucrose, and fructose. Sugars also
include high fructose corn syrup, invert syrup, sugar alcohols,
including sorbitol, refiners syrup, and mixtures thereof. In
addition to sugar, extended juice beverages of the present
invention may contain other sweeteners. Other suitable sweeteners
include saccharin, cyclamates, acetosulfam, and
L-aspartyl-L-phenylalanine lower alkyl ester sweeteners (e.g.
aspartame). A particularly preferred sweetener for use in such
extended juice products is aspartame. For single-strength juice
beverages, the sugar content may range from about 2.degree. to
about 16.degree. Brix (16.degree. Brix means the juice contains
about 16% soluble solid, and so on). Typically, the sugar content
of such beverages depends upon the amount of juice contained
therein. For full-strength beverages containing at least about 95%
(wt) juice, the sugar content is typically from about 5.degree. to
about 14.degree. Brix. For extended juice beverages which contain
from about 50% (wt) to about 90% (wt) juice, the sugar content is
typically from about 5.degree. to about 13.degree. Brix (no other
sweetener) or from about 2.degree. to about 8.degree. Brix (other
sweetener containing). For juice concentrates according to the
present invention, the sugar content may range from about 6.degree.
to about 75.degree. Brix. Typically, the sugar content of these
juice concentrates is from about 20.degree. to about 50.degree.
Brix. For orange juice concentrates, the sugar content is
preferably from about 35.degree. to about 50.degree. Brix.
[0083] The amount of the sweetener effective in the beverages of
the invention depends upon the particular sweetener used and the
sweetness intensity desired. For noncaloric sweeteners, this amount
varies depending upon the sweetness intensity of the particular
sweetener. For sugar, this amount can be from 1% to 14% (typically
from 6% to 14%) by weight for carbonated beverages. Preferred
beverages contain from 9% to 13% by weight sugar. In determining
the amount of sugar for beverages of the present invention, any
sugar or other sweetener present in the flavor component, such as
in juice, is also included. Low-calorie sweetener combinations
containing a noncaloric sweetener, such as aspartame, and a sugar,
such as high fructose corn syrup, may also be used in beverages.
For beverage syrups, the amount of sugar in a beverage syrup is
from about 10% (wt) to about 60%, (wt) and preferably from about
40% (wt) to about 60% (wt). In addition to sweeteners, beverages
may also already be fortified with water soluble or fat-soluble
vitamins. The composition of this invention may be added to
beverages that already contain or to which are later added vitamin
compositions that are not of this invention.
[0084] The various beverage and beverage concentrates may be
packaged in conventional packages for the particular beverage or
beverage concentrates which are nutritionally supplemented by the
optically clear composition of fat-soluble vitamins. In some
instances, the concentrates are frozen.
[0085] The powder compositions of this invention may also be added
to cosmetics, if it is desired, to blend fat-soluble vitamins such
as vitamin E into a cosmetic. If the cosmetic is optically clear,
preferred compositions of this invention may be used to avoid
increasing the turbidity of the cosmetic. Cosmetics include any
materials designed for application to the skin, hair, or nails, for
example skin care products such as balms, lotions, or sticks,
various ointments, make-up compositions for use on the face, eyes,
or lips, shampoos and conditioners, nail polishes, and the like.
The cosmetic may contain other active ingredients as used in the
cosmetics industry. Pharmaceutical compositions intended for
topical application in the form of ointments, lotions, and the like
are also contemplated. Cosmetic formulations will be well known to
the skilled person. The powder composition of this invention is
added at an appropriate time in the production process such as to
be thoroughly blended into the cosmetic.
[0086] The powder composition of this invention which contains
droplets of a fat-soluble vitamin that average about 70 to about
200 nanometers in diameter (preferably about 70 to about 150 nm,
more preferably about 80 to about 120 nm, and most preferably about
100 nm), and which are dispersed in a matrix as defined herein
above may be made by:
[0087] (a) combining water with a matrix as defined herein above
for a period of time sufficient for the matrix component to
dissolve in the water;
[0088] (b) adding a fat-soluble vitamin to the solution of step (a)
to form a crude emulsion, preferably a crude emulsion having a
solids content as described above, preferably of from about 30%
(wt) to about 50% (wt), more preferably of about 45% (wt);
[0089] (c) mixing the crude emulsion of step (b) until the size of
the droplets within the emulsion is determined to be about 1500 nm
or less;
[0090] (d) emulsifying the crude emulsion of step (c) at a
temperature of about 5.degree. C. to about 75.degree. C. at a
pressure of about 10,000 to about 60,000 psi (about 680 to about
4080 bar), preferably of about 25,000 psi (about 1700 bar) to
obtain a vitamin supplement emulsion consisting of droplets with
average sizes of about 70 to about 200 nm in diameter; and
[0091] (e) drying the emulsion of step (d) to obtain a powder
composition which contains droplets of a fat-soluble vitamin that
average about 70 to about 200 nanometers in diameter, and which are
dispersed in the matrix component.
[0092] Step (a) may be done at any reasonable temperature to ensure
a rapid dissolution of the matrix component in water and to fully
utilize its functionality. To ensure complete dissolution of the
matrix component within a reasonable amount of time (i.e.,
sufficient for the matrix component to dissolve), heating to about
70.degree. C. or to 80.degree. C. is preferable, after which the
resulting solution may be conveniently cooled to about room
temperature or a little higher (about 30.degree. C.).
[0093] In order to attain the desired droplet size, the emulsion
step (d) may be repeated through one or more passes as necessary to
obtain the desired droplet size, i.e. the crude emulsion is passed
into the homogenization vessel, emulsified, passed out of the
homogenization vessel, and passed through the homogenization vessel
again until the desired droplet size is attained. Usually at least
five to twenty passes will be required. These passes are usually
all performed at the same pressure and the same system parameters,
but different pressures may be used for different passes (other
system parameters could also be varied for different passes).
[0094] The period of time for one pass is not critical. The amount
of time per pass will depend on system parameters including
emulsion viscosity, batch size, flow rate and pressure. These
parameters will depend on the precise processing format selected,
and may be varied by the skilled person to obtain the desired
results. Emulsification passes should continue until testing shows
that the desired droplet size is achieved as determined by particle
size analysis (for example, by light scattering as described
above).
[0095] It is important that the homogenization step be performed at
an ultra-high pressure as described above to effectively reduce the
droplet size of the emulsion to a desirable size. The
homogenization temperature as measured at the exit of the
homogenizer is preferably below 70.degree. C. The emulsion is then
converted to a powder, by a known technology such as freeze-drying,
fluid-bed drying, beadlet formation, but preferably by
spray-drying, to obtain a powder composition which includes
droplets of a fat-soluble vitamin which droplets average about 70
to about 200 nm in diameter (preferably about 70 to about 150 nm,
more preferably about 80 to about 120 nm, and most preferably 100
nm), and which are dispersed in a matrix of natural polysaccharide
gum or of protein. A powder composition produced by this process is
part of this invention.
[0096] The final emulsion yields a powder which, upon redispersal
in a liquid, yields an emulsion droplet (diameter) size generally
about 5-15 nm larger than the droplet size of the emulsion before
spray drying. A powder so produced will contain vitamin droplets
e.g. of 200 nm diameter or less. Such a powder when added to a
liquid, will provide droplets with average droplet size of about 70
to about 200 nm in diameter, preferably about 70 to about 150 nm in
diameter, most preferably about 100 nm in diameter. Such droplet
sizes are convenient for adding to beverages at fortification
levels of up to about 2 to about 12 mg, preferably about 3.2 to
about 8 mg and especially about 6 mg of vitamin per 100 g of
beverage. As discussed above, vitamin E may be added in pure form
(i.e. 6 mg of vitamin E per 100 g). However, the more potent
fat-soluble vitamins will preferably be diluted, so that what is
added would be 6 mg of vitamin in diluent, rather than 6 mg of pure
vitamin. When added, the resulting beverage should display no
ringing. In addition, the added vitamin may be provided with
superior bioavailability.
[0097] With regard to an originally optically clear beverage, in
order to maintain optical clarity, a preferred composition of this
invention may be added. The NTU of the resulting beverage should be
no more than 30, and preferably around 10 to 15, especially at
lower levels of fortification. In general, at the desired levels of
fortification a droplet size of about 120 nm in diameter is
acceptable with regard to optical clarity, and does not contribute
substantial NTUs. In general, a droplet of smaller size may be
preferable for use at a higher level of fortification. Thus, with
regard to minimizing turbidity in an optically clear beverage, a
powder with a higher average vitamin droplet size would be more
useful at a lower level of fortification, while a powder with a
lower average vitamin droplet size would be preferable at a higher
level of fortification. In this regard, FIG. 2 provides guidance on
the relationship between droplet size and optical clarity. As can
be seen by this best fit approximation, this relationship is
roughly linear such that as droplet size increases, NTU increases
for the same level of fortification. Thus, optical clarity (NTU) is
a function of the droplet size of the composition.
[0098] To obtain the emulsion and powder of this invention, the
parameters of the above process may be varied within the limits
provided. The pertinent variables are pressure and temperature in
the emulsification step, solids content, which is percent by weight
of the vitamin(s) plus the matrix component in the crude emulsion,
the lipid component of the solids content, which is the percent by
weight of the solids content which is vitamin(s), including any
edible diluent such as oil, and the number of passes through the
emulsification step. Within the guidance of this invention, these
parameters may be varied to obtain a powder composition which
contains vitamin droplets of e.g. 200 nm or less in diameter, and
which has a potency (which is percent by weight of vitamin) of from
about 0.5% to 75%, especially about 25% to about 40%, and which
provides fortification levels of multiple RDAs of the vitamin,
preferably about 1-3 RDA of vitamin, most preferably in the form of
5 to about 30 mg of vitamin (pure, or as processed in a diluent)
per 8 ounces of liquid.
[0099] The potency of the powder of this invention is determined by
the amount of fat-soluble vitamin in the crude emulsion. For
example, an emulsion which is about 5% to about 15% by weight
vitamin (pure vitamin or vitamin in diluent) will in rough estimate
provide a powder with a potency of about 10% to 30% by weight.
However, a skilled person will be able to vary the emulsion content
with the guidance provided by this invention to obtain a desired
potency in the resulting powder.
[0100] In general, the lower the pressure, the more passes will be
required to obtain an emulsion with a given droplet size. Also, the
higher the lipid content, the more passes will be required to
obtain the given droplet size. As discussed above, the droplet size
of the emulsion determines the droplet size in the resulting
powder, and the droplet size in the liquid to which the powder is
ultimately added is about 5-15 nm greater than the droplet size of
the original emulsion. The potency of the powder is roughly twice
the lipid content (for pure vitamin) of the emulsion. The emulsion
is processed as described above, and in more detail below, to
obtain the desired droplet size. If a high level of fortification
is desired, then it is preferable to obtain a powder with droplet
sizes at the low end of the range. Lower droplet sizes can be
obtained by increasing the processing pressure, or the number of
passes. If it is possible to increase the processing pressure, then
a given number of passes at the higher pressure will provide
smaller droplets. However, if the pressure cannot be increased (if
for example 15,000 psi (1020 bar) is the upper limit for the
equipment being used), then the same result can be obtained by
increasing the number of passes.
[0101] With regard to obtaining a powder containing droplets of a
size which provide an acceptable turbidity for the desired
fortification level, the droplet size resulting from addition of
the powder is the most important variable. It is possible to add
less of a higher potency powder than of a lower potency powder to
get the same level of fortification, but if the higher potency
powder has a larger droplet size, then the fact that less of this
powder is added will not negate the effect of the droplet size and
higher turbidity will result.
[0102] To obtain powder compositions of this invention, the above
parameters may be varied within the following limits: The pressure
range is from about 10,000 psi (about 680 bar) to about 60,000 psi
(about 4080 bar), preferably from about 20,000 psi (about 1360 bar)
to about 35,000 psi (about 2380 bar), and especially about 30,000
psi (about 2040 bar). The solids content is preferably no more than
60% (wt). A preferred crude emulsion has a solids content of from
about 30% (wt) to about 50% (wt), preferably about 45% (wt), a
preferred lipid content is from about 10% (wt) to about 50%.(wt) A
preferred potency is from about 25% (wt) to about 40% (wt). The
number of passes that will be required to attain a droplet size in
the emulsion of about 70 to about 200 nm may be adjusted depending
on the parameters.
[0103] The various steps in the above method may be performed by
known methods using conventional reagents and equipment. A skilled
person given the guidance provided herein will be able to adjust
the emulsion, solids and lipid content (for potency), pressure,
temperature, and number of passes, within the limits of this
invention, to readily obtain a powder composition of this
invention.
[0104] In more detail, the powder is prepared by emulsifying a
crude emulsion of fat-soluble vitamin and matrix component (for
example the emulsion of this invention). Once the emulsion has
reached the desired emulsion droplet size, it is spray dried into a
powder. The potency of the powder is the weight percent of vitamin
which the powder contains.
[0105] The crude emulsion is prepared by homogenizing the
fat-soluble vitamin with the aqueous matrix component in suitable
amounts which will provide a powder to product having a droplet
size when dissolved in liquid of about 70 to about 200 nm,
preferably about 70 to 150 nm, more preferably about 80 to about
120 nm and most preferably about 100 nm. An emulsion containing
about 5-15% by weight of fat-soluble vitamin, 30-40% by weight of
matrix component, and 50-55% by weight water is an example. The
emulsion may be prepared in a standard vessel of a convenient
capacity where heating and cooling can take place. The water and
matrix component are added to the vessel. The mixture may be heated
to about 80.degree. C., but this is not required. The mixture
should be stirred until the matrix component has dissolved.
[0106] The solution is then left at or cooled to room temperature,
i.e., to about 30.degree. C., and the fat-soluble vitamin is slowly
added. The mixture is homogenized to a crude emulsion in the vessel
(for example by using a colloid mill or any other conventional
mixing means) until the droplet size is less than 1500 nm. Droplet
size may be measured by any conventional particle size analyzer. A
preferred measuring technique is the laser light scattering
technique. The Malvern ZetaSizer 3 or Autosizer Iic (Malvern
Instruments, Southborough, Mass.) is an example of a laser light
scattering measuring device that is used to measure particle size
according to the present invention.
[0107] The crude emulsion is then further emulsified using standard
equipment and vessels for this purpose. The device selected should
provide a sufficiently high pressure. Microfluidizer devices are
useful, models such as M-210C-E/H, M-110ET, M-610-C, and M-140K,
may be obtained from Microfluidics International Corporation,
Newton, Mass. It is also possible to use a water jet (such as those
produced by Jet Edge Inc., Minneapolis, Minn.). The crude emulsion
may be transferred from the holding vessel to the emulsifying
device through a suitable sieve in order to prevent clogging of the
microfluidizer. The temperature at which the homogenization (by
which is meant further emulsification) takes place is best kept
between room temperature (about 20-25.degree. C.) or about
30.degree. C. up to about 75.degree. C. with a cooling system such
as an ice water bath to control the temperature of the emulsion.
The pressure pump of the emulsifying device should be set at a
suitable pressure. Note that pressure in the device may fluctuate
over a wide range, depending on the number of pistons in the high
pressure pump. A two-piston Microfluidizer may vary, e.g. from
7,250 to 14,500 psi (500 to 1000 bar). A three-piston pump is
preferable.
[0108] Homogenization continues for a sufficient number of passes
to obtain an emulsion of the desired droplet size. In general, the
more stable the process pressure, the fewer number of passes should
be required to achieve the same droplet size. The emulsion is then
dried to obtain the powder of this invention. Drying may be
accomplished by any standard method, for example spray-drying in a
suitable spray dryer, such as a Yamato Mini-Spray Dryer.
[0109] The following examples are provided to further illustrate
the compositions and processes of the present invention. These
examples are illustrative only and are not intended to limit the
scope of the invention in any way.
EXAMPLES
Example 1
[0110] Gum arabic (Example 1a), and gelatine (Example 1b) in an
amount of 10 kg was dissolved in 23.3 kg distilled water at a
temperature up to 80.degree. C. The solution was then cooled to
about 30.degree. C. Vitamin E acetate (1.87 kg) was gradually added
and, at the same time, homogenized until the droplet size of the
emulsion was below 1500 nm. The crude emulsion was then homogenized
with a high pressure homogenizer (Microfluidics International
Corporation, Newton, Mass.). The emulsion was recycled through the
homogenization process until the droplets of the emulsion reached
an average size of below 140 nm. During the homogenization, the
temperature of the emulsion was maintained at about 35.degree. C.
with a cooling system.
[0111] The emulsion was then spray-dried with a spray dryer to
yield a powder containing about 15% (wt) of vitamin E acetate. When
the powder was used in beverage fortification, the turbidity of the
beverages did not increase significantly and also no phase
separation occurred, that is, the vitamin E acetate lipid phase did
not separate from the aqueous phase and form a layer on the
surface.
[0112] The amount of powder to be added to a beverage depends on
the amount of fortification desired. It is important to determine
the optimal particle size for the desired level of
fortification.
[0113] The beverage or beverage concentrates supplemented with the
compositions or tablets of fat-soluble vitamins of the present
invention may be made by conventional means well known to those of
ordinary skill in the art. In general, the optically clear
composition of fat-soluble vitamins may be simply added and gently
mixed into the beverage or beverage concentrates or syrups. The
effervescent tablet is generally dropped into the beverage and
allowed to dissolve (tablets do not generally yield an optically
clear beverage due to other tabletting ingredients, but do yield a
beverage without ringing, provided that other ingredients do not
themselves cause ringing). The beverage concentrates and syrups to
which the powder composition of fat-soluble vitamins has been added
may be used to make a final single strength beverage by blending
the concentrate or syrup with an appropriate amount of water,
usually about 1 part concentrate or syrup to about 3 to 4 parts of
water. The water may be carbonated or non-carbonated.
[0114] Examples of other beverages, to which the powder
compositions of fat-soluble vitamins as produced in Examples 1a) or
1b) may be added in nutritionally supplemental amounts,
include:
[0115] (c) "sparkling" orange juice containing 55% (wt) orange
juice and 45% (wt) carbonated water;
[0116] (d) pear-grapefruit nectar containing 25% (wt) pear juice,
20% (wt) grapefruit juice, the balance containing 10% (wt)
sucrose-water;
[0117] (e) kiwi-grapefruit drink containing 20% (wt) kiwi fruit
juice, 15% (wt) grapefruit juice, the balance containing water;
[0118] (f) mixed fruit "cocktail" containing 10% (wt) each of the
juices of passion fruit, mango, guava, pineapple, papaya, banana,
apricot, mandarin orange, pear and lime juices;
[0119] (g) yogurt/fruit beverage containing 20% (wt) milk products,
1% (wt) pectin, 20% (wt) pineapple juice, 10% (wt) shredded
pineapple fruit pulp, 16% (wt) corn syrup, the balance containing
water;
[0120] (g) cola beverage containing 0.35% (wt) cola flavor
emulsion, 11% (wt) sugar, 0.1% (wt) phosphoric acid, 0.1% (wt)
citric and malic acids, caramel coloring, the balance containing
carbonated water;
[0121] (i) full-strength orange juice;
[0122] (j) full-strength apple juice; and
[0123] (k) full-strength flavored cow's milk.
Example 2
Effervescent Tablets
[0124] Tablets were produced from the powder of Examples 1a) at
26.24% (wt) and Example 1b) at 42.5% (wt) and compared with tablets
produced from a current 50% (wt) vitamin E powder product (see
Table 1). The 50% (wt) vitamin E powder used for comparison was
obtained from Roche Vitamins and Fine Chemicals, Nutley, N.J.
[0125] The formulation shown in Table 1 was chosen for the test. In
this formula, after the dissolution of the tablets (from dry
Vitamin E 50% (wt) powder, Type CWS/F), very small oil droplets of
vitamin E may be seen on the surface of the water, if the surface
is observed against reflected light.
TABLE-US-00001 TABLE 1 Effervescent Tablet Label Overage E 26.25% E
42.1% E 50.0% Claim % Quantities Quantities Quantities Composition
Mg (wt) mg/Tabl. mg/Tabl. mg/Tabl. 1 Beta-Carotene 6.00 20 as Beta
Tab 10% E 72.00 72.00 72.00 2 Vitamin C 200.00 10 as Ascorbic Acid,
Fine 220.00 220.00 220.00 Granular 3 Vitamin E 50.00 10 as Dry
Vitamin E 26.25% 209.52 SD Lot 16/96-8 as Dry Vitamin E 42.1%
130.64 <110 SD Lot 27903-076 4 Citric Acid Anhydrous, 1300.00
1300.00 1300.00 Medium Granular 5 Sodium bicarbonate 800.00 800.00
800.00 6 Sodium carbonate 80.00 80.00 80.00 7 Mannitol MG.sup.1
1138.48 1217.36 1238.00 8 Aspartame 20.00 20.00 20.00 9 Sodium
cyclamate 30.00 30.00 30.00 10 Polyethylene Glycol 6000 100.00
100.00 100.00 Fine Powder.sup.2 11 Orange flavor Permaseal 20.00
20.00 20.00 74016-71.sup.3 12 Tangerine flavor Permaseal 10.00
10.00 10.00 74740-31.sup.3 Total Tablet Weight 4000.00 4000.00
4000.00 Suppliers .sup.1Mannitol medium granular, Roquette Freres,
4 rue Patou, F-59022 Lille Cedex, France .sup.2Hoechst AG, Postfach
800320 Frankfurt/Main 80, F.R. Germany .sup.3Givaudan Dubendorf AG,
CH-8600 Dubendorf, Switzerland
Procedure
[0126] I. Pass 3-12 through 1.00 mm sieve and mix with 1 and 2 for
15 minutes. II. Compress into effervescent tablets.
Results
[0127] Both samples tested gave tablets from the 26.25% (wt) and
42.5% (m) vitamin E powders of this invention with acceptable
hardness and disintegration characteristics. Their compression
profiles are very close to that of E 50% CWS/F. Sample 27903-076
containing 42.5% (wt) vitamin E showed better hardness and slightly
shorter disintegration time than the other.
[0128] On visual inspection of the surface of the water after the
disintegration of the tablets made from the 26.25% (wt) and 42.5%
(wt), vitamin E powders of this invention did not show any oily
droplets. In contrast, oily droplets were visible on the surface of
the water with the vitamin E 50% CWS/F product not made from a
composition of this invention.
Example 3
[0129] A vitamin conditioning shampoo is produced using standard
ingredients and methods as follows using a powder composition or
this invention. Vitamin E acetate powder as produced in Example 1a)
and Example 1b) is used as follows: Disperse the vitamin E acetate
powder as produced in Example 1a) or Example 1b) into water. Add
the vitamin E acetate powder of Example 1a) or Example 1b) to a
mixture of Monamid and phytantriol. Add the panthenol and etyl
panthenol. Add Part 2 to Part 1 and mix until clear. Add the Kathon
CG and perfume. Adjust the pH with citric acid 50% solution to pH
6.0 to 6.8. Adjust the viscosity with sodium chloride.
TABLE-US-00002 % by Ingredients CTFA designation weight Part 1
Deionized water Water 57.05 Monamid 716 Lauramide DEA 5.00 liquid
DL-panthenol-50% Panthenol and water 2.00 25% vitamin E acetate
powder Tocopheryl acetate 0.80 Phytantriol Phytantriol 0.10% Part 2
Standapol ES-2 sodium laureth sulfate 30.00 Mirataine CBS
Cocamidopropyl 3.00 hydroxysultaine Part 3 Sodium chloride sodium
chloride 1.00 Citric acid 50% solution citric acid 0.30 Perfume
Fragrance 0.20 Kathon CG Methylchloroisothia- 0.05 zolinone (and)
methylisothiazolinone Total: 100
[0130] The invention being thus described, it will be obvious that
the same may be varied in many ways. Such variations are not to be
regarded as a departure from the spirit and scope of the invention
and all such modifications are intended to be included within the
scope of the following claims.
* * * * *