Note: Descriptions are shown in the official language in which they were submitted.
~ACKGROUND O~ rllE INVENT:[ON
The present in-vention relates to beverages, especially
fruit flavored beverages wherein a clesired quality is opacity.
In the art oE the formu]ation of dry mix fruit juice
beverages, there is a continuing effort being made to
duplicate a counterpart natural fruit juice as closely as
possible. The imitation beverage must have the mouth-feel,
opacity, color and flavor characteristics of a natural juice.
These desirable characteristics must be evident from the time
of preparation of the aqueous beverage from the dry mix to
the time of consumption. In many cases the beverage is not
consumed for periods of time up to 48 hours subsequent to
preparation. While stability after reconstitution is critical,
it is equally important that the powderous dry beverage mix
be storage stable for extended periods of time (i.e., in
excess of 90 days) under adverse conclitions (i.e., temperature
100F and relative humidity 90%).
An attempt at achieving the desired property of opacity
or cloud inherent in natural fruit juice is described in U.S.
Patent No. 3,023,106 to Common. Therein is described a dried
emulsion incorporating a plastic fat which is added to a dry
beverage mix. The term "plastic fat" is described to cover
a fat which is semi-solid at room temperature, that is, a
product which is a mixture of fats and oils at temperat~lres
in the order of 60F. The plastic Eat may be compounde(l by
any one oE a number of means such as by hardening through
hydrogenation of vegetable oils or may comprise a blend of
such Eats and oils. Typically coconut oil may be hydrogenated
to give a semi-solid material having a Wiley melting point
of 98F, a capillary melting po:int of 104F, an iodine value
of 5.2, a saponification number of approximately 253 and a
solids content index of 43% at 20C. To this material is
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.dde(l 6~o stearin to yiel(l a partial:ly solidiEied Eat having
a Wiley meLting point of 111F, a capillary melting point
of 116F, an iodine value of 2.2, a saponification number
of approximately 25~ and a solids content index of from
48-50~ solids at a temperature of 20C.
Another attempt at producing a clouding agent was set
out in ~.S. Patent No. 3,658,522 to Carlson. The concept
of a plastic fat emulsion system of Common was improved upon
by providing for the incorporation of one or more inorganic
whitening pigments, typically titanium dioxide, in a clouding
system comprising a plastic fat and a hydrophilic colloidal
- material. Carlson typically spray dries a solution of gum
Arabic, hydrogenated coconut oil and titanium dioxide to obtain
a dry, flowable, powderous clouding agent which is subsequently
incorporated in a dry beverage mix.
A major drawback oE prior cloud systems relates to their
inclusion of the plastic fat itself in the cloud system.
Several detrimental effects are manifested due to the fat and
result ultimately in problems of clumping of the dry mix and
insolubility of the mix when reconstitution is attempted.
First, the oil may be poorly fixed, that is an excess of free
oil will be present in the cloud system. Second, in the
blending process when the cloucl is mixed with the other
ingreclients of the dry beverage mix ingredients, consiclerable
mechanical work is performed (typical:Ly in 2,000 pound
capacity ribbon blenders). The mechanical attrition and
grinding will liberate oil from its Eixative agent. A third
undesirable effect is caused by temperature which may be
due to both mechanical shear during mixing and ambient
conditions. A fourth effect ls provided by excessive moisture
which may be due to excessively humid ambient conditions and
the addition of liquid color to the dry mix. Thus, there
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are various influences which tend to liberate oil during
processing. Since the oil is water insoluble, aqueous,
reconstitution is incomplete.
~ nother problem associated with the use of oil in a
clouding agent is off-taste. The oxidated rancidity and
alkaline hydrolysis of the oil result in a undesirable soapy
taste. This type of problem i8 further compounded in that
discovery of the off-taste in many instances is not made
until after the product has been in the stream of commerce
for a considerable period of time.
In view oE the foregoing~ it would be highly desirable
if a simple method were devised whereby a cloud system for
dry beverage mixes could be obtained which does not contain
fat.
SUMMARY OF THE I~VENTION
It is an object of the present in-vention to provide a
clouding agent for dry beverage mixes and particularly
imitation fruit juice mixes which have the opacity and mouth-
feel oE natural juices. Typically these imitation fruit
juices have a pH oE below about ~.5. It is another object
of this invention that the cloud system be storage stable
for extended periods of time. Still another object is to
provide a clouding agent which is readily soluble in cold
water. Generally this invention allows the use of titanium
diox:lde ln a cloud system which is Eree from o:il.
These and other objects are accomplished according to
the present invention by preparing a dry clouding agent Eor
dry beverage mixes by co-drying an aqueous mixture containing
a major amount of solubilized malto dextrin with minor amounts
of xanthan gum and dispersed titanium dioxide.
DETAILED DESCRIPTION OF TEE INVENTION
The term opacity as used in this invention relates to
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~he level of light transmittance of an aqueous solutlon.
A laboratory instrument such as a ~ausch and Lomb Spec 20
(TM) is used to measure such light transmittance levels.
The clouding agent of this invention is prepared by
dispersing and co-dry;ng solubilized malto dextrin, xanthan
gum and dispersed titanium dioxide to prodLIce a dry powder
which manifests a clouding effect when incorporated in an
artificial beverage.
Various malto dextrins (hydrolyzed cereal solids)
which are starch hydrolysates produced by converting pure
refined corn starch into nutritive saccharides through the
use of acids or specific enzymes. The carbohydrate
composition of malto dextrin is arranged to yield a DE
(dextrose equivalent) of less than 20. They are typically
bland in flavor and without appreciable sweetness. Preferably,
the malto dextrin as used in the instant invention will have
a dextrose equivalent of between 10 and 20. As used herein,
the malto dextrin sold under the trademark Fro-Dex(T )15 by
the American Maize-Products Company has been found most
preferable. It is a white free-flowing powder extremely
bland in taste with little or no sweetness. Additionally, it
has a quality of contributing a slight opacity to the clouding
composition.
TYPICAL CHEMICAL AND PHYSICAL DATA
OF FRO-DEX(TM)15
% Molsture 4.5
Dextrose Equivalent 18
SOz (M.W.) 40 ppm
pH (1:1) 4.5
Weight Per Cu. Ft. (approx.) 36 lbs.
Carbohydrate Composition
(Approx. % D.~.)
Monosaccharides 3
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Visaccharides 2
Trlsac:charlcles 2
Tetrasaccharide~ 2
Pentasaccharides ~
higher 91
Screen Analysis (average %)
On ~0 nil.
On 100 .~
On 200 1~.0
Thru 200 85.6
The xanthall gum as used in this invention is a high
molecular weight natural carbohydrate or more specifically
polysaccharide. Xanthan gum defines the exocellular bio-
polysaccharide which is produced in a pure culture fermentationprocess by the microorganism xanthomonas campestris.
An important functional quality of the xanthan gum is
its ability to control aqueous fluid rheology. Water solutions
of xanthan gum are extremely pseudoplastic; when shear stress
is applied, viscosity is reduced in proportion to the amount
of shear once the yield point has been exceeded. Upon
release of the shear, total viscosity recovery occurs almost
instantaneously. Another attribute of xanthan gum that makes
it useful as a suspension stabili~er is that it not only has
a yield value but also a viscosity which is almost independent
of temperature and pH. A particular xanthan gum found most
useful in the practice of this invention is sold under the
trademark Keltrol( )F available from Merck ~ Company.
TYPICAL PHYSIC,A_ PROPERT ES
KELTROL(TM)
Physical State Dry, cream-colored powder
~loisture Content 11
Ash 9%
Color 70
SpeciEic Gravity 1.5
Bulk Density (lbs./cu. Et.) 52.2
Browning Temperature, C165
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Charrirlg Temperature, C 2~0
Ashing Temperature, C 470
As a 170 Solution (distilled
water):
Heat of Solution (cal.~g.soln) 0.080
ReEractive Index (20C) 1.3338
pH 7.0
Surface Tension (dynes/cm) 75
Freezing Point, C 0.0
1% Viscosity (60 rmp, Brookfield LVF)
(with 1% electrolyte added) 1400 cps
- Mesh Size 200
10 Titanium dioxide as used herein is preferably a purified
inorganic white5 named by the 1971 Colour Index, pigment
white 6, C.I. 77891. It is available from H. Kohnstamm
Company and typically has the following characteristics.
TITANI~M DIOXIDE TECHNICAL DATA
Crystal Type Anatase
Speclfic Gravity 3.9
Pounds per Solid Gallon 32.5
1 Pound Bulks, Gals. .0308
Minimum TiO2 99%
20 Spatula Water Absorption 30 lbs. water/100 lbs. Pigment
Spatula Oil Absorption 20-22 lbs. oilllOO lbs. Pigment
Average Particle Diameter 0.3 Microns
Screen Test 99% Through 325 Mesh Screen
100% Through 200 Mesh Screen
(CTFA Method C 6-1, Wet
Screening)
(ASTM D-185-~5)
The cloud composition oE the instant invention is
preferably added to constituent ingredients necessary to
formulate a dry beverage mix. ThereEore, unless otherwise
indicated all percentages herein referred to will be in
relation to the total dry mix (as in the instant example)
composition. Thus, the malto dextrin may be present in
the range of 0.5% to 5.0% by weight of the total dry mix
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composition. Preferably the range will be 1.5% to about 2~0~o~
The xanthan gum will be present in the range between .01% and
about 0.1% by weight of the dry mix composition. Preferably
the xanthan will be present in the amollnt of .015% to about
.035,0 by weight of the dry weight mix composition. The
titanium dioxide will be present in amounts between ~Ol~o and
between ~025% and .075%. Preferably the titanium dioxide
will be finely divided say .1 micron to about .7 microns in
particle size.
A number of unexpected results arise from the combination
of the three components of the instant clouding composition.
Most importantly it has been found that it is critical that
the titanium dioxide be added to an aqueous solution of malto
dextrin and xanthan gum and the resultant suspension be dried
concurrently or co-dried. The combination oE each component
by mixing in its dry form does not have utility. The titanium
dioxide immediately begins to precipitate when the mix is
put in a beverage. Likewise, co-drying titanium dioxide
with either malto dextrin or xanthan gum separately does not
work. The titanium dioxide again immediately beings to
precipitate when the mix is put in a beverage. Likewise~
co-drying titanium dioxide with either malto dextrin or
xanthan gum separately does not work. The titanium dioxide
again immediately precipitates when used in a beverage.
Surprisingly the co-dried combination permits a c:Loud which
; is useful in a beverage for periods of at least 24 hours and
preferably at least 48 hours when the beverage is stored at
50F.
~nother unexpected result of the instant invention
relates to the amount of xanthan gum necessary to contribute
the desired mouth-feel (viscosity) in an artificial fruit
beverage. Conventionally, carboxy methyl cellulose is used
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n the amount of .46% by weight of the dry be-verage mix
composition to impart the desired effect. Direct replacement
of carboxy methyl cellulose has been found to require the
xanthan gum in the amount of about .13% by weight of the dry
mix. It has been found that on a comparative basis when
xanthan gum is contained within the composition of the instant
invention that only about one-third the amount by weight of
the dry mix of xanthan gum is needed for equivalency of the
desired viscosity/mouth-feel characteristics. Another
unexpected result is that two particular levels of malto
dextrin have been identified as being most effective. Those
lev~ls are 1.75% and 3.00~O of malto dextrin by weight of the
dry beverage mix. Thus, while levels oE malto dextrin of
between .5 and 5.0% by weight of the dry mix are effective,
the unexpected benefits displayed by this invention are most
evident at the two specific levels identified.
In the preparation of the product of this invention, it
is preferable to use a vessel which has provision for mixing
under high shear. Additionally, the malto dextrin and xanthan
- 20 gum will solubilize more quickly if the aqueous system is
heated preferably to about 150F. The higher temperatures
may be used, but in no case should they exceed the boiling
point of the composition. The resultant solution or
suspension is then maintained at an elevated temperature in
preparation Eor drying. Most advantageous due to process
cost and volume considerations is the uti:Lization of a spray
i dryer to evaporate the water from the aqueous mixture and
thus obtain a powderous clouding agent from the co-dried
ingredients. Those skilled in the art will recognize that
other methods of drying may be employed such as freeze drying,
vacuum drying, etc. Typically in spray drying, the product
will be fed to the drying tower by means of a pump such as a
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lanton-G,aulin under working pressures of between 500 psi
and 3,000 psi. Sucll pressures inEl:ict additional shearing
force on the mixture and further serve to homogenize and
reduce the particle size oE the product.
The dried cloud ingredients are typically mixed with
other beverage materials such as tartaric acid~ citric acid
or other food acids, sugars such as sucrose, dextrose,
fructose and the like, artificial sweeteners, suitable co:Loring
agents such as orange coloring, cherry coloring, grape
coloring and the like, fruit flavors such as orange, grape,
lemon, lime and the like and other art recognized beverage
additives.
The invention is more fully described but not limited
by the following examples.
EXAMPLE 1
To prepare the cloud according to the preferred
embodiment of this invention, the following procedure is
follows:
To a high shear planetary-type mixture is added a
pre-blended dry mix of 953.9 pounds of malto dextrin sold
under the trademark Fro-Dex(TM)15 available from ~merican
Maize-Products Company and 13.7 pounds of xanthan gum sold
under the trademark Keltrol( )F available from Merck and
Company and 290 gallons oE water with constant mixing. To
the resulting solution is added 27.~ pounds of food grade
titanium dioxide. During the mixing the temperature of the
solution is elevated to about 150F. Next the mixer speed
is increased to maximum speed ancl shear and is maintained
for a 15 minute period. The product is then transferred to
a separate holding tank preparatory to spray drying. The
mixture enters the spray drying tower by means oE passage
through a two stage Manton-Gaulin positive displacement pump.
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The first stage and second stage are operated at 2000 psi
pressure and 3000 psi pressure, respectively. The solution
enters the upper portion of the drying tower through a series
of spray nozzles. The inlet air temperature of the drying
tower is about 400. The exit air temperature in the lower
portion of the tower is about 190F. The product exiting
the bottom of the tower is a dry flowable powder having a
moisture content below about 5~O.
_XAMPLE 2
A fruit flavored beverage mix is prepared employing
the cloud prepared as in Example 1 and in accordance with
the following formulation:
B erage Mix A
Ingredient Percent
Sugar 88.522
Citric Acid 5.318
Cloud* 1.825
Flavor and Flavor Enhancers 1.143
Monocalcium Phosphate 1~137
Potassillm Citrate0.780
Dry Calcium Phosphate 0.66~
Vitamin C 0.511
Carboxymethylcellulose 0.460
Vitamin A 0.036
Color 0.028
100.000
*Cloud
Malto Dextrin (Fro-Dex 15 ( )) 95.89
Xanthan Gum (Keltrol ( ))1.37
Titanium Dioxide _.74
100.000
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For compar:ison, a conventiona:L fruit flavored beverage
mix i8 prepared in accordance with the following formulation:
Bever~ B
Ingredient Perce t
Sugar 88.309
Citric Acid 5.381
Cloud~ 1.574
Monocalcium Phosphate1.137
Potassium Citrate 0.780
Tricalcium Phosphate0.664
Vitamin C 0.511
Flavor and Flavor Enhancers 1.143
Carboxymethylcellulose0.500
Vitamin A 0.036
; Color 0.028
~, 100.000
*Cloud
Modified Starch 76.440
~Iydrogenated Coconut Oil19.600
20 Titanium Dioxide 1.960
Tricalcium Phosphate 2.000
1~0.000
Thirty-three grams of Beverage ~lix B is reconstituted
; in 8 ounces of water and produced a beverage with an opacity
readlng of 60 on a Bausch Lomb Spec 20 opacity meter.
Thirty-three grams of the above Beverage Mix A is
reconstituted in 8 ounces of water. The opacity is the same
as that of the Beverage Mix B. Additionally the body and
mouth feel of the beverage of A and that of B are judged
equivalent by an expert panel.
The prodLIct of Beverage Mix B after being reconstituted
in 50F water and held at that temperature Eor 24 hours
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~Lisplayecl precipitation of the cloud system. Titanium
dioxide came out of so:Lution and settled at the bottom of
the sample flask with an attendant reduction in opacity.
The product of Beverage Mix A has no apparent precipitation
or change in opacity after 24 hours at 50F. Additionally
the product of Beverage Mix A is readily dispersible in cold
water and does not display the clumping or streaking problems
associated with beverages mixes which have oil.
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