U.S. patent application number 13/058763 was filed with the patent office on 2011-06-16 for new polydextrose material.
This patent application is currently assigned to CARGILL, INCORPORATED. Invention is credited to Bruno Frederic Stengel.
Application Number | 20110143007 13/058763 |
Document ID | / |
Family ID | 40193696 |
Filed Date | 2011-06-16 |
United States Patent
Application |
20110143007 |
Kind Code |
A1 |
Stengel; Bruno Frederic |
June 16, 2011 |
NEW POLYDEXTROSE MATERIAL
Abstract
The present invention discloses a new type of water-soluble
polydextrose. This new type of polydextrose contains at least 75%
by weight of saccharide molecules having a degree of polymerisation
(DP) of 5 or more and characterised in that the non-digestible
fiber content is at least 80% by weight. Further, the present
invention relates to a process for preparing this new type of
polydextrose and to the use of this polydextrose in products such
as food products, pharmaceutical products and personal care
products.
Inventors: |
Stengel; Bruno Frederic;
(Auderghem, BE) |
Assignee: |
CARGILL, INCORPORATED
Wayzata
MN
|
Family ID: |
40193696 |
Appl. No.: |
13/058763 |
Filed: |
July 23, 2009 |
PCT Filed: |
July 23, 2009 |
PCT NO: |
PCT/EP2009/005332 |
371 Date: |
February 11, 2011 |
Current U.S.
Class: |
426/549 ;
426/580; 426/590; 426/658; 426/660; 536/112 |
Current CPC
Class: |
A23L 33/26 20160801;
A23L 2/02 20130101; A23L 2/52 20130101; A61Q 19/00 20130101; A61K
47/26 20130101; A61K 8/73 20130101; C08B 37/0009 20130101; A23G
3/42 20130101; A23L 29/212 20160801; A23V 2002/00 20130101; A23V
2002/00 20130101; A23V 2250/5116 20130101; A23G 1/40 20130101 |
Class at
Publication: |
426/549 ;
536/112; 426/658; 426/660; 426/590; 426/580 |
International
Class: |
C08B 37/02 20060101
C08B037/02; A23G 3/42 20060101 A23G003/42; A23L 2/60 20060101
A23L002/60; A21D 13/00 20060101 A21D013/00; A23C 9/152 20060101
A23C009/152 |
Foreign Application Data
Date |
Code |
Application Number |
Aug 20, 2008 |
EP |
08014774.7 |
Claims
1-19. (canceled)
20. A polydextrose comprising saccharide molecules, wherein at
least 80% by weight of the saccharide molecules have a degree of
polymerisation of 5 or more, and wherein less than 20% by weight of
the saccharide molecules have a degree of polymerisation of from 1
to 4, and wherein the non-digestible fiber content of the
polydextrose is at least 80% by weight.
21. The polydextrose according to claim 20, wherein at least 70% by
weight of saccharide molecules have a degree of polymerisation of
10 or more.
22. The polydextrose according to claim 20, wherein the molecular
weight dispersity of the polydextrose is below 2.0.
23. The polydextrose according to claim 20, wherein the molecular
weight dispersity of the polydextrose is below 1.8.
24. The polydextrose according to claim 20, wherein the
polydextrose has a volume mean diameter that is smaller than 60
.mu.m.
25. The polydextrose according to claim 20, wherein the
non-digestible fiber content of the polydextrose is at least 85% by
weight.
26. The polydextrose according to claim 20, wherein the
non-digestible fiber content of the polydextrose is at least 90% by
weight.
27. The polydextrose according to claim 20, wherein less than 15%
by weight of the saccharide molecules have a degree of
polymerisation of from 1 to 4.
28. The polydextrose according to claim 20, wherein less than 10%
by weight of the saccharide molecules have a degree of
polymerisation of from 1 to 4.
29. A process for preparing a polydextrose comprising the following
steps: a) providing a crude polydextrose, b) adjusting the pH of
the crude polydextrose to from 6 to 8 to yield a product, and c)
chromatographic separation of the product of step b) into at least
two fractions, wherein one fraction comprises a first polydextrose
comprising saccharide molecules, wherein the first polydextrose is
enriched in saccharide molecules having a degree of polymerisation
of from 1 to 4 compared to the product of step b); and a second
fraction comprises a second polydextrose comprising saccharide
molecules, wherein the second polydextrose is enriched in
saccharide molecules having a degree of polymerisation of 5 or more
compared to the product of step b).
30. The process according to claim 29, wherein the crude
polydextrose is provided by polycondensation of saccharides, and
optionally sugar alcohols in the presence of acid.
31. The process according to claim 29, wherein the chromatographic
separation of step c) comprises chromatographic separation on a
strongly acidic cation exchange resin.
32. A food product comprising the polydextrose according to claim
20 and further comprising food ingredients.
33. The food product according to claim 32, wherein the food
product is selected from the group consisting of confectionery,
bakery products, beverages, and dairy products.
34. The food product according to claim 32, wherein the food
product is an ice cream and the food ingredients are ice cream
ingredients.
35. The food product according to claim 32, wherein the food
product is a chocolate and the food ingredients are chocolate
ingredients.
36. The food product according to claim 32, wherein the food
product is a beverage and the food ingredients are beverage
ingredients.
Description
TECHNICAL FIELD
[0001] The present invention relates to a new type of water-soluble
polydextrose. This new type of polydextrose contains an increased
amount of saccharide molecules having a higher degree of
polymerisation (DP) and has a high non-digestible fiber content.
Further, the present invention relates to a process for preparing
this new type of polydextrose and to the use of this new
polydextrose in products such as food products, pharmaceutical
products and personal care products as well as to such products
containing this polydextrose.
BACKGROUND OF THE INVENTION
[0002] Acid-catalysed polymerisation of saccharides is a well-known
phenomenon which is described in numerous general articles, books
and patents.
[0003] Polydextrose is commercially available and all of these
polydextrose products include a variety of residual compounds such
as glucose, sorbitol, citric acid and other compounds which
contribute to the taste, colour, and caloric value. Low molecular
weight compounds such as 1,6-anhydroglucose and
5-hydroxymethylfurfural contribute a bitter taste and
off-flavour.
[0004] U.S. Pat. No. 3,766,165 discloses that polymers useful as
low-calorie food ingredients can be prepared by heating dextrose or
maltose, optionally with a minor amount of a polyol, in the
presence of edible polycarboxylic acid catalysts under reduced
pressure. U.S. Pat. No. 3,876,794 discloses various kinds of foods
containing same.
[0005] In the wake of this important disclosure, further
development and research is concentrated on overcoming the sour
and/or bitter taste observed in the products according to U.S. Pat.
No. 3,766,165 and U.S. Pat. No. 3,876,794.
[0006] E.g., WO 98/41545 discloses methods for preparing
polysaccharides by reacting glucose or glucose containing materials
with a polyol in the presence of mineral acids such as phosphoric,
hydrochloric and/or sulphuric acid. According to this disclosure,
the low levels of catalyst as suggested therein lead to minimal or
no off-flavors and little color formed during the course of the
reaction. The methods disclosed in this document may comprise
further purification methods.
[0007] U.S. Pat. No. 5,831,082 describes a process for obtaining
highly pure water-soluble polydextrose by separation. The reported
over 99,2% water-soluble polydextrose contains considerable amounts
of di-, tri- and tetrasaccharides. The products according to this
disclosure are reported to not have a bitter aftertaste.
[0008] U.S. Pat. No. 5,051,500 describes a continuous method for
preparing a randomly-bonded polysaccharide.
[0009] US 2004/0038837 relates to the use of maltodextrin (named
here as well as polydextrose) in combination with sucrose to induce
biphasic liquid formation. The mentioned product has a
polymerisation degree of 4 to 22 and is brought on the market as
Maltrine.TM., which corresponds to maltodextrin type products.
[0010] EP 0 458 748 describes a polydextrose composition that is
substantially free of bitter tasting and colour. In example 1 the
polydextrose solution is added to an anion exchanger. The eluate
(containing polydextrose) is free from the citric acid, but lower
molecular weight contaminants such as 1,6- anhydroglucose, sorbitol
and glucose are still present.
[0011] U.S. Pat. No. 5,831,082 describes a process for obtaining a
highly pure water-soluble polydextrose. The crude polydextrose
which contains 0.5 to 3% of citric acid is purified by using a
simulated moving bed system applying a strong acidic gel. The
DP6+fraction is always around 56-58% by weight.
[0012] In view of the prior art, there is still a considerable need
for an improved water-soluble polydextrose material which contains
an increased amount of saccharide molecules with a higher degree of
polymerisation and a reduced number of digestible mono- and
oligosaccharides. With the present invention, such a new kind of
polydextrose is provided.
SUMMARY OF THE INVENTION
[0013] The current invention relates to a new water-soluble
polydextrose containing at least 75% by weight of saccharide
molecules having a degree of polymerisation of 5 or more. More
preferably, the polydextrose contains at least 80% by weight of
saccharide molecules having a degree of polymerisation of 5 or
more, and characterised in that the non-digestible fiber content is
at least 80% by weight, preferably at least 85% by weight, more
preferably at least 90% by weight. In addition, the present
invention provides a process for preparing such a polydextrose
comprising the steps of
[0014] a) providing crude polydextrose,
[0015] b) adjusting the pH to from 6 to 8 preferably about 7,
and
[0016] c) chromatographic separation into at least two fractions,
wherein one fraction is enriched in saccharide molecules having a
degree of polymerisation from 1 to 4 and one fraction is enriched
in said new water-soluble polydextrose according to the
invention.
[0017] Moreover, the present invention relates to the use of this
new polydextrose in the preparation of products such as food
products, pharmaceutical products and personal care products, as
well as to said food products, pharmaceutical products and personal
care products containing this polydextrose.
DETAILED DESCRIPTION OF THE INVENTION
[0018] Polydextrose as referred to herein, is a water-soluble,
bulking agent. It is a randomly cross-linked (branched) glucan
polymer (polysaccharide) characterised by having predominantly
(.beta.-1-6 and .beta.-1-4 linkage and which is produced through
acid-catalysed condensation of saccharides alone or in the presence
of sugar alcohols. Polydextrose is substantially different from
maltodextrin which is obtained through the hydrolysis of starch
materials and which is containing a majority of .alpha.-1-4
linkages.
[0019] The new polydextrose according to the present invention is a
polydextrose with an increased amount of saccharide molecules
having a degree of polymerisation (DP) of 5 or more. The degree of
polymerisation is applied as in polymer chemistry and refers to the
number of repeat units in the chain. The degree of polymerisation
is a measure of molecular weight and the molecular weight of the
monomer is calculated as about 162. This increased amount of
saccharide molecules with a DP of 5 or more is at least 75% by
weight and more preferably, at least 80% by weight. The new
polydextrose is further characterised in that the non-digestible
fiber content is at least 80% by weight, preferably at least 85% by
weight, more preferably at least 90% by weight. Non-digestible
fiber is neither digested nor absorbed in the small intestine. It
has at least one of the following properties: increase stools
production, stimulate colonic fermentation, reduce fasting
cholesterol levels, and/or reduced post-prandial blood sugar and/or
insulin levels. The non-digestible fiber is determined by applying
fresh dialysed rat small intestine powder at 37.degree. C. at pH
6.
[0020] In a preferred embodiment, the polydextrose according to the
invention further contains less than 20% of saccharide molecules
having a DP from 1 to 4 (mono- and oligomers), and preferably the
amount of these mono- and oligomers is less than 15% by weight,
more preferably less than 10% by weight. With respect to the
present invention, the terms "oligomer" and "oligosaccharide" are
used to describe those products of a polymerisation reaction which
have a DP from 1 to 4, i.e. they contain 1 to 4 moieties
corresponding to a saccharide or sugar alcohol unit, e.g. 4
saccharide units or 3 saccharide and 1 sugar alcohol unit, each
linked via covalent bonds such as glycosylic bonds. In contrast,
those molecules resulting from the polymerisation reaction which
have a degree of polymerisation of 5 or more are referred to as
"polymers" or "polysaccharides". If, glucose or other hexose
containing reactants are used in the polymerisation reaction, these
polymers have a molecular weight of about 828 g/mol or higher.
[0021] Furthermore, the polydextrose according to the invention has
a molecular weight dispersity below 2.0, or preferably, below 1.8,
describing the dispersions of distributions of molar masses. The
equivalent terminology is polydispersity. This is the ratio of
weight average molecular weight to number average molecular
weight.
[0022] The current invention further relates to a polydextrose
according to the invention characterized by a volume mean diameter
smaller than 60 .mu.m, preferably smaller than 55 .mu.m, and more
preferably smaller than 50 .mu.m. The calculation of the volume
mean diameter is based on the definition of moments of a
distribution and an example is given in ISO/FDIS 9276-2.
[0023] Finally, according to the present invention, the
polydextrose is low caloric, and non-cariogenic. Its
non-cariogenicity is measured with an in-vitro test.
[0024] Another embodiment of the invention is directed to a process
for preparing the new polydextrose as defined above, which
comprises the following steps:
[0025] a) providing a crude polydextrose;
[0026] b) adjusting the pH of the crude polydextrose of step a) to
from 6 to 8, preferably about 7, e.g. by adding alkaline compounds;
and
[0027] c) chromatographic separation of the product of step b) into
at least two fractions, wherein one fraction is enriched in
saccharide molecules having a DP from 1 to 4, and one fraction
which is enriched in polydextrose containing at least 75% of
molecules, which have a DP of 5 or more.
[0028] In one embodiment, this process according to the invention
provides the crude polydextrose in step a) by acid-catalysed
polymerisation of saccharides.
[0029] The saccharides used in the first step of the process are
preferably glucose and glucose containing saccharides. These
saccharides can be glucose (dextrose), maltose, starch
hydrolysates, or the like, wherein a fraction of the saccharide
moieties might also be esterified with carboxylic acids. These
saccharides could be used in an anhydrous or in hydrated state, or
they could be used in an aqueous solution.
[0030] Optionally, the saccharides used as starting material may
further contain sugar alcohols.
[0031] Preferably, the amount of sugar alcohols used in the
starting material is from 0 to 20% by weight of polymerisation
reactants (saccharides). These sugar alcohols can comprise one or
more of glycerol, erythritol, threitol, pentitols such as xylitol,
and hexitols such as sorbitol, mannitol or galactitol. Preferred
sugar alcohols comprise one or more hexitols and, particularly,
sorbitol.
[0032] A large range of acids could be used for catalysing the
polymerisation to obtain the crude polydextrose in step a).
Preferably, these catalysts are acids which are allowable for
consumption in order to reduce the otherwise necessary controls and
costs to check for the presence of and, if necessary, remove the
catalyst acids from the final product. In particular, the preferred
acids are edible acids (food grade acids) such as phosphoric acid,
citric acid, malic acid, succinic acid, adipic acid, gluconic acid,
tartaric acid, fumaric acid and mixtures thereof. Particularly
preferred are citric acid and/or phosphoric acid. The amount of
acid to be used as catalyst should be below 10 mol % relative to
the amount of saccharide (and polyol, if present) starting material
used in the polymerisation reaction. Preferably, this amount should
be clearly below this level, such as e.g. at most 3, at most 1, at
most 0.5, at most 0.1 mol % or lower.
[0033] The crude polydextrose is still containing the residual acid
which is used in the polymerisation reaction.
[0034] In step b), the pH of the crude polydextrose is increased to
6 to 8, preferably about 7, by adding alkaline compounds.
Surprisingly, it was found that by increasing the pH any formation
of degradation products such as furans, furfural and
5-hydroxymethyl furfural (5HMF) was prevented during the subsequent
separation step. The pH is increased preferably by adding liquid
alkaline compounds, such as sodium hydroxide dissolved in water or
other suitable alkalising compounds known in the art.
[0035] The chromatographic separation according to step c) leads to
at least two fractions, wherein one fraction is enriched of mono-
and oligosaccharide molecules, i.e. this fraction is enriched in
dextrose, maltose and other oligomers (up to DP4) in comparison
with the crude polydextrose after step b); and the other fraction
is enriched in polysaccharides (preferably with polymerisation
degree of 5 and higher) compared to the crude polydextrose after
step b).
[0036] Preferably, the chromatographic separation is performed on a
cation exchange resin, such as a strongly acidic cation (SAC)
exchange resin.
[0037] Finally, the polydextrose of the current invention is free
from degradation products such as furans, furfural and
5-hydroxymethyl furfural (5HMF) and through the chromatographic
separation a new profile of polymerisation degree is obtained and
the final product is low-caloric, non-cariogenic and has a
non-digestible fiber content of at least 80%.
[0038] Another aspect of the invention is directed to the use of
polydextrose containing at least 75% by weight of saccharide
molecules having a DP of 5 or more and characterised in that the
non-digestible fiber content is at least 80% by weight, in the
preparation of products selected from the group consisting of food
products, pharmaceutical products and personal care products. Still
another aspect of the invention is directed to food products,
pharmaceutical products and personal care products which contain
such a new polydextrose. In these products, the polydextrose
containing at least 75% by weight saccharide polymers and
characterised in that the non-digestible fiber content is at least
80% by weight, can be used in addition or instead of conventional
polydextroses.
[0039] The pharmaceutical products according to the invention
comprise tablets, excipients for preparing tablets, viscosity
agents for use in syrups or other liquid or viscous fluids,
solutions, emulsions or suspensions.
[0040] The personal care products according to the invention are
selected from fluid, semifluid or solid products such as tooth
paste, mouth wash and the like.
[0041] The polydextrose according to the invention is useful as a
humectant. Humectant is a substance used primarily in foods and
cosmetic products to help retain moisture.
[0042] The polydextrose according to the invention is particularly
useful for the preparation of food products. These food products
comprise in particular confectionary, bakery products, beverages
and diary products.
[0043] Confectionery compositions within the scope of the present
invention include chocolate, crystalline and non-crystalline
products. Non-crystalline products within the scope of the present
invention include hard candies, brittle, caramel, toffee, licorice,
jellies, chewing gums and gums, preferably soft gums. Crystalline
products within the contemplation of the confectionery compositions
of the present invention encompass fondants and creams, fudge,
nougats, marshmallows, pralines, pressed candies such as tablets,
marzipan and pastes, and panned candies (dragees). Combinations of
these products are also within the scope of confectionery
compositions. For example, chocolate coated crystalline or
non-crystalline products.
[0044] Chocolate, an important confectionery composition within the
contemplation of the present invention, encompasses sweet
chocolate, semi-sweet chocolate, bitter-sweet chocolate, which as a
group are often also referred to as dark chocolate, milk chocolate,
buttermilk chocolate, skim milk chocolate and white chocolate. In
addition, any of the aforementioned chocolates filled with nuts,
fruits, rice and other fillings used in the chocolate arts are also
within the scope of the current invention. Chocolate also includes
any confectionery product having qualities sufficient to impart
chocolate taste, chocolate flavour and any other material that
performs as a chocolate analogue obtaining a tender cake. By
applying the new polydextrose of the current invention, the
chocolate, milk and/or dark chocolate, is low caloric. Furthermore
in combination with erythritol, the final chocolate is
non-cariogenic and the cooling effect of erythritol is reduced by
the new polydextrose of the current invention.
[0045] The current invention further relates to bakery products
comprising the polydextrose of the current invention and additional
bakery ingredients.
[0046] The additional bakery ingredients will be apparent to a
person skilled in the art. They may include, e.g.: flour, raising
agents (such as baking powder and/or yeast), water and/or
water-miscible liquids (such as milk, alcohols, etc.), sweeteners
(e.g. sugar or artificial sweeteners), flavourings (e.g. synthetic
or natural flavours such as vanilla, caramel and/or almond
flavours; fruit juices such as orange, grapefruit, pear, cherry,
raspberry and/or blackcurrant juices; vegetable extracts such as
tomato, carrot, onion and/or garlic extracts;
[0047] spices; herbs; etc.) and/or one or more natural or synthetic
colorants. Optionally, vitamins (such as vitamins A, D3, E, K1, C,
B1, B2, B5, B6, B12 and PP, folic acid and biotin) and minerals
(such as sodium, potassium, calcium, phosphorus, magnesium,
chloride, iron, zinc, copper, manganese, fluorine, chromium,
molybdenum, selenium and iodine) can also be added.
[0048] The flour used in the bakery products may be from any source
(e.g. corn flour, soy flour or wheat flour). Most preferably,
however, it will be wheat flour. It is the protein of wheat flour,
gluten, which distinguishes it from other flours and makes it of
particular value in the baking industry. In hard, high-protein
wheat, there is more gluten in the endosperm and the starch cells
are firmly cemented together. In soft, low-protein wheat the
bonding is not so firm. For to most cakes a soft, low-protein flour
is needed for. Flours used for pan bread production will generally
be milled from hard wheat of high protein content, although soft
wheat can give optimum quality in the type of bread that is most
popular in some countries. Ideally, the flour will be
non-chlorinated.
[0049] The choice of additional bakery ingredients will depend, of
course, on the bakery product being produced. Indeed, the
polydextrose according to the present invention can be used in the
manufacture of bakery products such as cakes, biscuits, cookies,
waffles, donuts, muffins, bread, fat-filling and bakery cream.
[0050] Dairy products of the invention can be selected from the
group consisting of milk, whey, yoghurts and drinks based on them;
dairy cocoa based drinks, fermented desserts (such as fresh cheese
preparations, drinkable products), ice cream, neutral dairy
desserts (such as puddings, flans, vlas, crime desserts, whipped
desserts) and flavoured yoghurt preparations (e.g. fruit yoghurt
without fruit). Ice cream prepared with the new polydextrose of the
current invention, has a more full texture, is less watery, and
shows a more fat-like creaminess and is very much appreciated for
its rich taste and texture. The texture is better than the texture
of ice cream using commercial polydextrose.
[0051] Beverage can be any medical or non-medical syrup or any
drinkable solution including iced tea, and fruit juices, vegetable
based juices, lemonades, cordials, and nut based drinks. It further
encompasses beverage concentrates and drink powders. Beverage
concentrate refers to a concentrate that is either in liquid form
or in essentially dry mixture form. The liquid concentrate can be
in form of a relatively thick, syrupy liquid. The essentially dry
mixture can be in the form of either a powder or a tablet. The
beverage concentrate is usually formulated to provide a drinkable
beverage composition or a final beverage when constituted or
diluted with water, either carbonated or non-carbonated. Drink
powders are suitable for constituting with water, carbonated or
non-carbonated, or milk, a final beverage for oral
administration.
[0052] Said beverage can further comprising additional
carbohydrates, proteins, peptides, amino s acids, antioxidants,
fats, vitamins, trace elements, electrolytes, intense sweeteners,
edible acids, flavours and/or mixtures thereof.
[0053] Said additional carbohydrates are selected from the group
consisting of monosaccharides, disaccharides, gelling starches,
starch hydrolysates, dextrins, fibers such as low-caloric fibers,
polyols and mixtures thereof.
[0054] The monosaccharides to be used as additional carbohydrates
include tetroses, pentoses, hexoses and ketohexoses.
[0055] is Typical disaccharides to be used as additional
carbohydrates include sucrose, maltose, trehalulose, melibiose,
kojibiose, sophorose, laminaribiose, isomaltose, gentiobiose,
cellobiose, mannobiose, lactose, leucrose, maltulose, turanose and
the like.
[0056] Starch hydrolysates to be used as additional carbohydrates
are produced by the controlled acid or enzymatic hydrolysis of
starch. They can be subdivided into two specific categories,
maltodextrins and glucose syrups, and are characterized by their DE
number (dextrose equivalent). In fact, the DE number is a
measurement of the percentage of reducing sugars present in the
hydrolysate and calculated as dextrose on a dry weight basis.
Maltodextrins have a DE number up to 20, whereas glucose syrups
have a DE number greater than 20.
[0057] Dextrins to be used as additional carbohydrates are prepared
according to the dextrinisation method. Dextrinisation is a heat
treatment of dry starch in presence or absence of acid.
[0058] Gelling starches to be used as additional carbohydrates may
include emulsified starches such as starch n-octenyl succinate.
[0059] The low-caloric fibers can be arabinogalactan, chitosan,
chitin, xanthan, pectin, cellulosics, konjac, gum Arabic, soy
fiber, inulin, modified starch, hydrolysed guar, guar gum,
beta-glucan, carageenan, locust bean gum, alginate, polyglycol
alginate.
[0060] Among the vitamins one can mention vitamin A, vitamin C,
vitamin D, vitamin E, vitamin B.sub.12, and the like.
[0061] The edible acids can be selected from phosphoric acid,
citric acid, malic acid, succinic acid, adipic acid, gluconic acid,
tartaric acid, fumaric acid and mixtures thereof. Preferably the pH
range of the beverage is from about 2 to about 6.5. These acids can
be the same or different from the ones used in the crude
polydextrose provision step.
[0062] The flavours are selected from fruit flavours, botanical
flavour and mixtures thereof. Preferred flavours are cola flavour,
grape flavour, cherry flavour, apple flavour and citrus flavours
such as orange flavour, lemon flavour, lime flavour, fruit punch
and mixtures thereof. The amount of flavour depends upon the
flavour or flavours selected, the flavour impression desired and
the form of flavour used.
[0063] If desired, coloring agents can also be added. Any
water-soluble coloring agent approved for food use can be utilized
for the current invention.
[0064] When desired, preservatives such as potassium sorbate and
sodium benzoate can be added.
[0065] Gums, emulsifiers and oils can also be added in the beverage
for texture and opacity purposes. Typical ingredients include
carboxymethylcellulose, mono- and/or di-glycerides, lecithin, pulp,
cotton seed oil and vegetable oil. It further can comprise foam
stabilizing agents such as yucca, or yucca/quillaia extracts.
[0066] The invention will hereunder be illustrated in the form of a
series of non-limiting examples.
EXAMPLES
Example 1
[0067] A separation test was performed with a chromatographical
system (ISMB unit from Mitsubishi) composed of four chromatographic
columns connected in series that had a bed volume (BV) of 300
liters. The column were packed with a strongly acidic cation (SAC)
exchange resin (Mitsubishi UBK550 in Natform), which was
conditioned by passing deionized water through the column at
60.degree. C. for 15 hours. The resin used was a copolymer made
from styrene and divinylbenzene (DVB) with a cross-linking of 8%.
The crude polydextrose (1.71 kg dry substance, composition: 1.5%
contaminants including acid, 5.3% DP1, 8.4% DP2, 9.3% DP3, 9.0%
DP4, 8.3% DP5, 7.5% DP5-DP10, 18.3% DP10-DP20, 22.4% DP20-DP30,
9.7% DP30-DP36 and 0.5% DP36+ by weight) was neutralised with an
aqueous solution (30%) of sodium hydroxide to a pH close to 7.
[0068] The heated (55.degree. C.) neutralised polydextrose solution
(33.5.degree. Brix) was then injected at the top of the column. The
sample was then eluted with deionized water at a predetermined flow
rate of 0.15 BV/hr and at a constant temperature of 50.degree. C.
Samples were collected at regular intervals, and 2 fractions have
been isolated: one fraction containing the low molecular s weight
fraction and a second fraction containing the polydextrose (0.8 kg)
with the desired molecular weight profile (see table
1--refined).
[0069] Results of the GPC analysis of the polydextrose (0.8 kg)
with the desired molecular weight profile is shown in Table 1.
[0070] The GPC analysis was performed with two columns in series:
Ultrahydrogel.TM. 500 (Waters Corp., USA) at ambient temperature
and Rezex RSO Oligosaccharide (Phenomenex, USA) at 80.degree.
C.
[0071] The eluent is demineralised, degassed, sterile filtrated
water, applied at a flow Rate of 0.2 ml/min
[0072] Detector: Differential Refractometer and molecular Weight
Calibration is done with Pullulan Standard Kit P-82 (Shodex, Japan)
for MW 780.000-5.900, Cargill Polyol (e.g. Maltidex 163A6) for MW
828-180, and quantification is Electronical Integration.
TABLE-US-00001 TABLE 1 GPC analysis showing the composition of the
combined fractions before and after applying the chromatographic
step. Polymerisation Molecular degree % DP+ fractions Weight Crude
Refined 22800-11800 0.0 0.04 11800-5900 0.5 2.1 DP36-DP30 5900-4878
9.7 17.5 DP30-DP20 4878-3258 22.4 33.5 DP20-DP10 DP20+: 74.74
3258-1638 18.3 21.6 DP10-DP5 DP10+: 82.24 1638-828 7.5 7.5 DP5
DP5+: 90.74 828 8.3 8.5 DP4 666 9.0 6.7 DP3 504 9.3 2.3 DP2 342 8.4
0.2 DP1 180 5.3 0.1 Contaminants + 180* 1.5 0.0 acid contaminants +
residual acid DP: degree of polymerization expressed in
anhydroglucose units.
[0073] The neutralisation of the citric acid present in the
unrefined polydextrose prior to the chromatographic separation step
resulted not only in the removal of by-products like 5 HMF,
furfural, etc. but also prevented their formation.
Example 1B
[0074] Determination of Non-digestible Fiber Content
[0075] The fiber content of the `refined` polydextrose was measured
by an in-vitro digestion system using rat intestinal enzymes. As a
reference, isomaltulose was included.
[0076] The intestinal enzymes were purchased as rat intestinal
acetone powder from Sigma. (Sigma catalogue # 11630, Sigma-Aldrich,
St. Louis, Mo., USA). The crude powder was further purified as
described below:
[0077] 10 g rat small intestinal acetone powder was added to 200 ml
phosphate buffer pH 6.0, 0.1 M and was mixed for 3 h at 4.degree.
C. The mixture was centrifuged at 10000 rpm for 10 minutes at
4.degree. C. (Sorval RC5CPLUS--Kendro Laboratory Products, Newtown,
Conn., USA). The supernatant was filtered on filter paper with
vacuum followed by dialysis with membrane MWCO: 25000 (Spectra/Por
Biotech Cellulose Ester (CE) Dialysis Membranes, Spectrum
Laboratories, CA, USA) in buffer pH 6.0, 0.1 M, 0.01% NaN3 (10 L
and replace with fresh buffer every day) for 3 days at 4.degree. C.
while stirring gently with magnetic stirring bar. The obtained
solution was lyophilized.
[0078] An activity check was done on the purified small intestinal
rat powder. This was done with 0.06 g purified rat powder that was
incubated with 5.4 ml 0.1 M phosphate buffer and addition of 0.6 ml
0.1% isomaltulose (final 0.01% isomaltulose). This was performed in
a glass test tube at 37.degree. C. and stirred with a small
magnetic stirrer bar. Dextrose release was measured with a
Glucose-Test kit (Reflectoquant 1.16720--Merck KgaA, Darmstadt,
Germany Purified rat powder that gave a minimum of 40 ppm dextrose
after 60 minutes was used for fiber determination.
[0079] The polydextrose was incubated with intestinal enzymes under
the following conditions
[0080] 0.15 g purified rat intestinal powder was dissolved in 5.4
ml phosphate buffer pH 6.0, 0.05 M. Subsequently, 0.6 ml sample at
0.1% was added. The reaction mixture was stirred gently and
incubated at 37.degree. C.
[0081] 1 ml samples were taken after several time intervals and the
amount of glucose present in each sample was determined immediately
by Glucose-Test (Reflectoquant 1.16720--Merck KgaA, Darmstadt,
Germany).
[0082] 93% of non-digestible fiber was measured for the
polydextrose sample whereas isomaltulose was fully hydrolysed after
2.3 hrs.
Example 2
[0083] Chocolate:
[0084] The polydextrose of Example 1 was used to prepare dark
chocolate and milk chocolate according to Tables 2 and 3,
respectively.
TABLE-US-00002 TABLE 2 Dark chocolate composition % maltitol 10.00
polydextrose 19.00 erythritol 21.00 cocoa mass 45.44 cocoa butter
4.00 sucralose 0.013 vanilla 0.100 lecithine 0.450 total 100.00
[0085] The ingredients were mixed in a Z blender at 45.degree. C.
at a rate of 35 rpm for mixing and 50-60 for conching.
[0086] For producing dark chocolate, first, the sweetener
(=maltitol, polydextrose, erythritol and sucralose) was put in the
Z blender. Subsequently, part of the cocoa mass and the part of the
cocoa butter was added. Refining was done with 3 rolls refiner. The
powder obtained after the refining was put again into the Z blender
for 1-3 h. The temperature of the Z blender was increased to
70.degree. C. and the second part of the cocoa mass was added.
After 14 h the second part of the cocoa butter was added. The
temperature of the mixture was decreased to 50.degree. C. One hour
before the end of the process lecithin was added.
[0087] The chocolate is low caloric.
TABLE-US-00003 TABLE 3 Milk chocolate compositions 3-Way blend
maltitol 10.00 polydextrose 18.50 erythritol 14.39 cocoa mass 13.50
cocoa butter 16.00 Milk fat 5.00 Skimmed milk powder 22.00
sucralose 0.020 vanilla 0.020 lecithine 0.570 total 100.00 fat
content 29.1 caloric value 397.5
[0088] Table 3 shows a milk chocolate product comprising
erythritol, maltitol and the polydextrose according to the
invention (the 3-way blend)
[0089] The milk chocolate is low caloric. The final chocolate is
non-cariogenic and the cooling effect of erythritol is reduced by
the new polydextrose of the current invention.
Example 3
[0090] Ice Cream
[0091] In Table 4, three ice cream compositions comprising the
polydextrose of example 1 are given.
[0092] Creamy ice cream can be prepared by applying the
polydextrose according to example 1.
TABLE-US-00004 TABLE 4 Ingredients Fat-free Sugar-free Sugar-free
Maltitol syrup (Cargill C Maltidex M -- 9.9% 9.9% 16311)
Polydextrose (example 1) 4.5% 10.0% 10.0% Isomaltulose (Cargill
Xtend 16420) 10.0% -- -- Whey powder (WPC 30) 3.0% 3.0% 3.0%
Skimmed milk powder 2.0% 2.0% 2.0% Cocoa fat -- 3.0% -- Potato
starch (Cargill, C DryLight 2.5% -- -- 01970) Fructose 3.0% -- --
Sucralose -- 0.01% 0.01% Stabilizer (Danisco, Creamline 816) 0.65%
0.65% 0.65% Flavors n.d. n.d. n.d. Skimmed milk (<0.3% fat) add
add add to 100% to 100% to 100%
[0093] The dry ingredients (apart from the fat) were mixed
together. Everything was brought to a temperature of 40-45.degree.
C., followed by mixing in the water.
[0094] The fat was added and heating was started to pasteurize at
85.degree. C. for 5 minutes, followed by homogenization at
80-85.degree. C. in a two-step homogenizer at 150/50 bar. Product
was brought through an in-line tubular heat exchanger(water cooled)
to 25-30.degree. C. and it was collected in a tank. Rapid cooling
to 4.degree. C. while stirring was continued and it was kept at
4.degree. C. for a minimum of 4 hours (maturation).
[0095] The ice cream was extruded in a continuous freezer, outlet
temperature -6 to -6.5.degree. C. 1 L boxes were filled and put in
a freezer at -35.degree. C. for 16 hours and storage was done at
-18.degree. C.
[0096] The ice cream had a pleasant fat-like creaminess and was not
watery, in comparison to the ice cream containing commercial
polydextrose.
Example 4
[0097] Beverages
[0098] Carbonated Cola Beverages
[0099] Mid-calorie cola with 4% fructose, 3% polydextrose of
Example 1 and high intense-sweetener
TABLE-US-00005 TABLE 5 Recipe Polydextrose 188.1 g Aspartame 466.2
mg Acesulfame K 239.4 mg Caffeine anhydrous (ZX0116) 0.57 g
Fructose 240 g Sodium benzoate 10% (w/v) 9.5 g Cola emulsion AK
0610 (Duckworth) 12.5 g Ortho-phosphoric acid 85% 6.8 g add Spa
.TM. water to make 1 ltr
[0100] Procedure:
[0101] The amount of Spa.TM. water was put in a beaker, the
necessary amount of polydextrose was added and stirred until
dissolution. The total mixture was heated up to max 50.degree. C.
Afterwards, the other ingredients were added until dissolution and
heated up to max. 50.degree. C.
[0102] Afterwards, 35 ml of this basic syrup was put into bottles
and diluted with carbonated water to give a volume of 210 ml.
[0103] Evaluation:
[0104] The samples containing the polydextrose according to the
invention got a specific density of approx. 7.degree. Brix and a pH
of approx. 2.7.
[0105] When compared to mixtures containing equivalent amounts of
conventional polydextrose (Litesse.RTM.) instead, both had a good
cola odor, but the one containing polydextrose according to the
invention was less intense than conventional Litesse.RTM.
polydextrose containing cola.
[0106] Color is not an issue within the cola formulations.
[0107] Taste:
[0108] The cola products containing the polydextrose according to
the invention had a better cola taste than other conventional
polydextrose cola drinks. The inventive products were judged to
have a less artificial taste and no powdery taste.
[0109] Fruit Juice Containing Beverages
[0110] Low-calorie orange soft drink with 7% polydextrose of
Example 1 and high intense sweetener
TABLE-US-00006 TABLE 6 Recipe Polydextrose 72.68 g Aspartame 225.5
mg Acesulfame-K 112.24 mg Orange Compound JBA O11105-11 18 g Sodium
benzoate 10% (w/v) 1.5 g Citric acid monohydrate 50% (w/v) 4.3 g
Ascorbic acid 10% (w/v) 0.8 g Add Spa .TM. water to make 1 ltr
[0111] Procedure:
[0112] The amount of Spa.TM. water was put in a beaker, the
necessary amount of polydextrose was added and stirred until
dissolution. The total mixture was heated up to max 50.degree. C.
Afterwards, the other ingredients were added until dissolution and
heated up to max. 50.degree. C.
[0113] Odor:
[0114] All samples had a good orange odor--no real difference
[0115] Taste:
[0116] Good orange perception, somewhat artificial aftertaste
[0117] Mid Calorie orange soft drink with 4% polydextrose of
Example 1, 3% erythritol, and high intense-sweetener
TABLE-US-00007 TABLE 7 Recipe Polydextrose 41.5 g Erythritol 30 g
Aspartame 157.5 mg Acesulfame-K 77.5 mg Orange Compound JBA
011105-11 18 g Sodium benzoate 10% (w/v) 1.5 g Citric acid
monohydrate 50% (w/v) 4.3 g Ascorbic acid 10% (w/v) 0.8 g Add Spa
.TM. water to make 1 ltr
[0118] All samples had a dry matter of approx. 7.6.degree. Brix and
a pH of approx. 3.1.
[0119] Procedure:
[0120] The amount of Spa.TM. water was put in a beaker, the
necessary amount of polydextrose was added and stirred until
dissolution. The total mixture was heated up to max 50.degree. C.
Afterwards, the other ingredients were added until dissolution and
heated up to max. 50.degree. C.
[0121] Taste:
[0122] Good orange perception, nearly no artificial aftertaste
Example 5
[0123] Soft Gums
[0124] Soft gum recipes comprising no polydextrose (reference
material), and polydextrose according to example 1
TABLE-US-00008 TABLE 8 RECIPE Reference Polydextrose RAW MATERIALS
Part A Maltitol Cargill 3.5 -- C*16313 Polydextrose -- 5 Water --
2.14 d.s. 2.89 4.8 Part B Gelatine 220 bl 0.295 0.295 Water 0.421
0.421 PROCESS Part A Brix (after 86.degree. 83.degree. heating)
Part B Brix 37.01 37.01 d.s. 0.265 0.265
[0125] Part A was dissolved in hot water (temperature 80-90.degree.
C.). It was kept at this temperature until the desired Brix was
obtained.
[0126] Part B was dissolved in hot water of temperature of
90.degree. C.
[0127] Part A and B (ratio A:B: 83/17) were mixed and citric acid
was added to the blend.
[0128] Depositing was occurring at temperature 78-84.degree. C.
[0129] This method gave satisfactory results for the soft gums
prepared with polydextrose of example 1
Example 6
[0130] In-vitro assessment of the cariogenicity of polydextrose of
example 1.
[0131] Experimental
[0132] The method used was an in-vitro cariogenicity test. In this
test `in-vitro` fermentability of carbohydrates by the oral cavity
bacterium Streptococcus mutans, was investigated under defined
conditions. The test was set up as follows: In a medium, consisting
of a simple nitrogen source with the test substance as sole carbon
source, buffered with a physiological buffer, organic acid
production was recorded over time.
[0133] a. Medium Constituents
[0134] Carbohydrate: 0.85 M stock solution. Final concentration in
test volume was 170 mM. Nitrogen source: 6.7% d.s. Yeast Nitrogen
Base (YNB from Difco). Final concentration in test was 0.67%
d.s.
[0135] Buffer: 1.25 M MES (morpholino-ethane-sulfonic acid)
suspension was adjusted to pH=7.2 with concentrated NH4OH (MES is
solubilised during pH adjustment). Final concentration in test was
0.25 M.
[0136] The solutions were sterilized by filtration (0.22.mu.).
[0137] Each sterile `in vitro` test tube (15.times.150 mm, metal
stopper) contained the following ingredients (for a 10 ml
test):
[0138] 2 ml carbohydrate stock solution (0.85 M)
[0139] 2 ml MES-buffer
[0140] 1 ml YNB-solution
[0141] 4.5 ml sterile distilled water
[0142] 0.5 ml inoculum
[0143] A 5 ml test was generally used when low cariogenic
substrates were tested, because of the high inoculum density, which
was needed for these substrates; for cariogenic substrates (as
sucrose, dextrose) the test was performed in 10 ml.
[0144] b. Inoculum Preparation
[0145] A stock culture was prepared by transferring Streptococcus
mutans--TCV264 (ATCC25175) from TBAbase (Tryptose Blood Agar base)
slants to TSB (Tryptic Soy Broth)--MES buffer (3% TSB-0.06 M) in 1L
flask, pH7.2, and grown at 37.degree. C. For 16 hours,
100strokes/min shaking. Bacteria were concentrated by
centrifugation (10 minutes at 3000 g). Cells were washed with
physiological buffer (0.04% NaCl, 0.3 KH2PO4, 0.7% Na2HPO4.2H2O,
+0.5% Tween 80) and centrifuged again.
[0146] The final precipitate was re-suspended in a minimal volume
(25 ml) of the same buffer, to contain approx. 2-5.times.10e10
cells/ml.
[0147] This stock culture was transferred into sterile REVCO-vials
(1 ml/vial), immediately frozen in liquid nitrogen and stored at
-70.degree. C.
[0148] A vial with frozen S. Mutans cells was used to inoculate a
sterile 0.5L flask with 500 ml TSB-MES buffer, slightly agitating
in a water-bath to disperse the cells. The culture was grown under
the same conditions, as described above, during 5-7 hours
(pH=6.3-6.4 and O.D. 660=0.8-0.9).
[0149] Cells were then harvested and re-suspended in 10 ml
physiological buffer (=50.times.concentrated). Control platings on
slants with Bile Esculin Agar were performed to check the purity
and concentration of this cell-suspension.
[0150] Because of practical reasons and of the difficulty of viable
cell count with Streptococci, the cell density was estimated
several times by incubation of the inoculum on dextrose as
substrate, with three different amounts of cells, and the acid
production rate was observed. As inoculum for the test 1.0 ml of
the above obtained suspension was used to inoculate the test tubes
of the in vitro test.
[0151] All manipulations are carried out in a sterile
environment.
[0152] c. In-vitro Test Conditions and Sampling
[0153] Inoculated test tubes were incubated, without shaking, at
37.degree. C. Test tubes were agitated on a Vortex, just before
sampling. At appropriate time intervals, sterile samples (1.2 ml)
were taken, centrifuged for 5' at 3000 g and supernatant was
filtered through 0.45.mu. filter (non-sterile). The pH was
measured. 0.75 ml samples were transferred.
[0154] Depending on the type of carbohydrate under investigation,
different inoculum concentrations and different time intervals for
sampling were chosen.
[0155] For polyols and alternative sweeteners, acid evolution was
followed in a 16 to 40 hour interval, using approx. 5.times.10e9
cells/ml inoculum in the test tube.
[0156] For glucose, fructose, sucrose and other fermentable
carbohydrates, the faster acid production requires an interval from
1 to 24 hours and a 10 times lower inoculum in the test tube.
[0157] Analysis and Calculation of Results
[0158] Organic acids were determined by HPLC on a Sodex
KC811-column in H+ form, at 65.degree. C. And eluted with 0.01%
H2SO4 at 0.8 ml/min and an injection volume of 25.mu.; detection
with UV at 210 nm.
[0159] Areas of lactic, formic and acetic acid peaks were recorded
and corrected with butyric acid as internal standard. HPLC results
were expressed in micromol acid/ml or in mM.
[0160] The inoculum concentration used is 3.5.times.108 cells/ml.
The release of organic acids was measured and ADR (total acidity/hr
after a certain incubation period, mM/hr, total acidity is defined
as the sum of lactic , formic and acetic acid).
[0161] The results are given in the next table:
TABLE-US-00009 TABLE 9 ADR after ADR after ADR after Sample 3 h 5 h
28 h Polydextrose of example 1 3 3 1 Mannitol 0 0 0 Isomaltulose 4
5 5 Commercial polydextrose 6 5 2 Litesse Ultra (commercial 4 4 2
hydrogenated polydextrose)
[0162] The in-vitro cariogenicity data indicate that the
polydextrose of example 1 is essentially non-cariogenic and is even
less cariogenic than the commercial polydextrose.
* * * * *