Note: Descriptions are shown in the official language in which they were submitted.
11717Z8
BACKGROUND OF THE INVENTION
The present invention relates to fruit juice-containing
products and, in particular, to a method for eliminating or
minimizing the separation of solids in such products.
Fruit juice-containing products, i.e., aqueous-based
beverages or preparations containing fruit juice (as well
as concentrates from which such beverages or products may
be prepared), are well-known in the art and have achieved
a relatively high degree of commercial acceptance. A known
difficulty with such products, however, is the separation
of the fruit juice solids (e.g., pulp) in the product, that
is, the difficulty in maintaining the fruit juice solids
in suspension or dispersion in the beverage or preparation
over a prolonged period of time. As a result, at the time
lS of purchase and consumption of the product, the fruit juice
solids often will have either settled toward the bottom of
the container or floated toward the surface, depending upon
the relative densities of the solids and the liquid product.
In either event, the product thus is non-uniform in composi-
tion throughout the container.
Although agitation of the fruit juice-containing product
in its container prior to use generally will provide the
requisite uniform drink or preparation, many consumers either
forget to take this measure or find it cumbersome or
difficult to do so, particularly where the product, e.g.,
beverage, is packaged for purchase in a large volume container
such that product will be poured therefrom on a periodic
basis, i.e., after being re-stored for a time sufficient to
result in re-separation of solids. In addition, for certain
fruit juice-containing products, once the fruit juice solids
have separated it is difficult to reinstate the desired
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11717;~8
suspension, even with agitation, owing either to the nature
of the solids ~ se or some interaction (e.g., agglomera-
tion) between separated particles which alters their
solubility or dispersibility in the product.
Fruit juice-containing products packaged in transparent,
e.g., glass or plastic, containers present an added
difficulty with respect to the aesthetically undesirable
visible presence of solids at the bottom or top thereof at
the time of purchase by the consumer.
Prior art attempts at overcoming these difficulties
typically make use of natural or synthetic additive materials
as stabilizers in an effort to maintain the juice solids in
suspension. Most such additive systems proposed simply are
ineffective for this purpose, particularly in highly acidic
products having a pH of about 3.0 or less. Moreover, the
additives proposed often rely ~ se on their ability to
increase the viscosity of the product in order to more
effectively maintain the solids in suspension, or contribute
this property incident to their stabilizing function. As a
result, the final product is undesirably thickened and often
exhibits an undesirable mouthfeel. Still further, known
additives typically generate difficulties in the juice
product manufacturing process. For example, many such
additives require elaborate and expensive mixing procedures
to effect their dissolution in the product. In certain cases,
stabilizer additives require some form of heat processing to
bring about their activation for this purpose. However, such
heat processing may be inconsistent or incompatible with the
processing necessary or desired for preparing the juice-
containing product per se.
11717~8
SUMMARY OF THE INVENTION
..
It is an object of the present invention to provide a
means for reducing separation of juice solids in fruit
juice-containing products.
Another object of the present invention is to provide
fruit juice-containing products, for example single-
strength products and concentrates, exhibiting reduced
separation of juice solids.
Yet another object of the present invention is to
provide both aqueous-based and substantially water-free
concentrates which, upon reconstitution with water, result
in fruit juice-containing products having reduced separation
of solids.
These and other objects are attained by the inclusion
in the fruit juice-containing product or concentrate of a
stabilizer system comprised of a mixture of low viscosity
propylene glycol alginate and sodium carboxymethylcellulose.
According to the present invention, the ultimate desire
is the provision of a fruit juice-containing product
exhibiting reduced solids separation, i.e., wherein the
fruit juice solids are more effectively maintained in
relatively uniform suspension throughout the product over
an extended period of time. Such products may include single-
strength fruit juice beverages or other products which are
packaged for immediate consumption or use by the consumer;
concentrated products which are not per se subject to solids
separation difficulties but which are ultimately utilized to
prepare reconstituted products which otherwise would be
subject to separation; and concentrated products which would
exhibit undesirable solids separation both in their
li7i7;~8
concentrated state and in their reconstituted form.
The stabilizer system of the present invention
comprises propylene glycol alginate, the water-soluble
propylene glycol ester of alginic acid, and sodium
carboxymethylcellulose, a synthetic water-soluble ether of
cellulose. These gums or hydrophilic colloids are either
pre-blended for addition to the fruit juice-containing product
or added to the product separately, e.g., either simultaneously
or sequentially, such that the product contains an effective
amount of each, typically from about 0.015~ to about 0.20
propylene glycol alginate and 0.01% to about 0.10% sodium
carboxymethylcellulose, percents by weight based upon the
total weight of single-strength product, to result in reduced
solids separation. At the levels of gum so utilized, it is
found that the product can be stabilized over a wide range
of conditions, e.g., temperature and pH, without substantially
affecting the viscosity or mouthfeel of the product.
The method of incorporating the gums into the fruit
juice-containing product is not critical per se so long as
effective dissolution of the gums is achieved. Thus, for
example, where the fruit juice-containing product is an
aqueous single-strength product or aqueous concentrate, the
gums, in a substantially dry state, may be added to the
liquid mixture of all other ingredients to achieve hydration,
dispersion and dissolution of the gums therein. Alternatively,
the dry gums may be added to only a portion of the liquid
mixture of other ingredients to effect hydration, dispersion
and dissolution of the gums, with the remaining ingredients,
e.g. additional water, being thereafter added.
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~i717;~8
In another method, the gums may be hydrated, dispersed
and dissolved in an appropriate amount of liquid medium in a
separate vessel and the thus prepared solution thereafter
added to a vessel containing the main body of ingredients.
Alternatively, the gums may be dry blended with one or more
dry ingredients of the fruit juice-containing product and the
thus prepared blend thereafter added to the liquid mixture of
the remaining ingredients. A dry-blending procedure obviously
is desirable where the fruit juice-containing product is a
substantially dry mixture intended to be reconstituted with
water for ultimate use.
As earlier noted, the fruit juice-containing products
to which the present invention is directed may assume a
variety of forms. According to one embodiment of the invention
the product may be one which is manufactured and sold at a
dilution or concentration suitable for immediate consumption
or use, in which case the product will comprise fruit juice
solids, water and the stabilizer system, typically in
conjunction with sweeteners, acidulants, colorants, pre-
servatives, flavorings, and the like. The fruit juice-
containing product also may be one which is manufactured and
sold in an aqueous-based concentrated form wherein the
consumer is required to add additional water for ultimate use.
Again, the product is comprised basically of water (in an
amount less than that appropriate for ultimate use), fruit
juice solids and the stabilizer system, with sweeteners,
acidulants, colorants, etc. added as necessary. Such a
concentrate may be one which is otherwise subject to
separation difficulties only when reconstituted to proper
dilution or which exhibits such problems both in the
concentrated and reconstituted state. Still further,
7~13
the fruit juice-containing product may be a substantially
water-free, reconstitutable product comprised of fruit juice
solids, stabilizer and other optional ingredients such as
those earlier noted. Such a product, of course, will
otherwise exhibit undesirable separation of solids only
after reconstitution.
The juice-containing product also may be a manufactured
concentrate which is intended to be further processed by the
same or a different manufacturer, typically at some different
location, to a prGperly diluted product which is then sold
to the ultimate consumer. In such a case, the stabilizer
system may be present in the concentrate, comprised of water,
juice solids and other optional ingredients, as it leaves
the first manufacturer, particularly if separation of solids
might occur in the concentrate per se; alternatively, it may
prove more economical to manufacture the concentrate free of
stabilizer whereby the stabilizer is added to the product
incident to the dilution and other steps performed by the
final processor.
In each of the products described, the water and juice
solids present in the product typically are derived from
water-containing fruit juice, either in natural or concentrated
form, and, particularly for products manufactured for immediate
use, additional water. For certain products, however, the
sole source of water in the fruit juice-containing product
may possibly be derived from the water present in the fruit
juice or alternatively, the sole source of water may comprise
added water.
As will be apparent from the more detailed description
and Examples given in the following section, the stabilizer
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. ,
ii717;~8
system employed in the present invention is uniquely and
surprisingly superior to known stabilizers in its ability
to reduce sedimentation in fruit juice-containing products.
Indeed, use of either of the individual components of the
stabilizer system alone is ineffective in accomplishing the
desired results.
DETAILED DESCRIPTION OF THE INVENTION
.
Further details regarding the present invention are
provided with reference to the following illustrative,
non-limiting Examples:
EXAMPLE I
_ .
An orange juice beverage is prepared from the following
ingredients:
Orange Juice Concentrate (65 Brix).......................... 14.50 gal.
Orange Oil.................................................... 0.20 gal.
Citric Acid.................................................. 20.00 lbs.
Sodium Citrate............................................... 10.00 lbs.
FD&C Yellow #6................................................ 0.25 lbs.
Sugar...................~................................... 915.00 lbs.
Water............................................... Approx. 914.11 gal.
TOTAL: 1000.00 gal.
To an agitated vessel containing this product are added from
about 1.31 to about 17.45 pounds of propylene glycol alginate
(Kelco Kelcoloid-0)* and from about 0.87 to ~.72 pounds of
sodium carboxymethylcellulose (Hercules CMC-7LF). The
product is then adjusted to 12.0 Brix and 0.30~ acid, heated
to a temperature of about 195 to 205F to effect sterilization
and filled into transparent glass bottles. The bottled
product is then cooled to room temperature.
* Trademark
-- 7 --
11717~8
EXAMPLE II
An orange juice syrup concentrate intended to be
diluted with 5 parts water for each part of concentrate to
form a suitable beverage is prepared from the following
ingredients:
Orange Juice Concentrate (65Brix)............... 87.0 gal.
Orange Oil........................................ 1.2 gal.
Citric Acid..................................... 120.0 lbs.
Sodium Hexametaphosphate......................... 52.0 lbs.
Sodium Benzoate.................................. 52.0 lbs.
FD&C Yellow #6.................................... 1.5 lbs.
Sugar.......................................... 5435.0 lbs.
Water................................... Approx. 488.7 gal.
TOT~L: 1000.0 gal.
15 To an agitated vessel containing this product are added from
about 7.85 to about 104.69 pounds of propylene glycol
alginate (Kelco Kelcoloid-0) and from about 5.23 to about
52.34 pounds sodium carboxymethylcellulose (Hercules CMC-7LF).
The product is adjusted to 72 Brix and 1.80~ acid (resulting
in a product which, upon dilution at 5:1, has 0.30% acid and
a soluble solids content of 12.0 Brix) and filled into
suitable containers at room temperature.
Sequestrants such as sodium hexametaphosphate employed
above or calcium disodium ethylenediaminetetraacetate
dihydrate are found to enhance product stability, particular-
ly in concentrates.
EXAMPLE III
A grapefruit drink is prepared by first preparing
a beverage base from the following ingredients:
li'717i~8
Grapefruit Concentrate (65 Brix).................... 760.0 gal.
Grapefruit Oil........................................ 12.5 gal.
Sodium Citrate....................................... 625.0 lbs.
Sodium Hexametaphosphate............................. 545.0 lbs.
FD&C Yellow #5......................................... 3.0 lbs.
Citric Acid.......................................... 155.0 lbs.
Water........................................ Approx. 148.5 gal.
TOTAL: 1000.0 gal.
This base is adjusted to 48.3 Brix and 5.4~ acid and stored
in a frozen condition. The base is thereafter thawed and
16~0 gallons thereof mixed with 800 pounds of sugar and
920 gallons of water to produce a grapefruit drink. To
this drink are added from about 1.30 to 17.38 pounds of
propylene glycol alginate (Kelco Kelcoloid-0) and about
0.87 to 8.69 pounds sodium carboxymethylcellulose (Hercules
CMC-7LF). The resultant product is adjusted to 11.0 Brix
and 0.60% acid and packed into containers at a temperature
of from 195F to 205F after which the containers are
cooled to room temperature.
EXAMPLE IV
A control fruit punch beverage was prepared from the
following ingredients:
Sucrose............................................ 693.97 grams
High Fructose Corn Syrup (68.5Brix)............... 385.01 grams
Citric Acid......................................... 12.86 grams
Fruit Punch Concentrate............................ 219.74 grams
Water............................................. 7430.42 grams
TOTAL: 8742.00 grams
(8.32 liters)
30 The beverage has a fruit juice content of 10~ (orange and
pineapple), a pH of about 3.0 (I 0.2), 0.30% acid and 12.5 Brix
,....
li~l7;~8
and was heated to about 195-205F to effect sterilization
and packed into four 64 ounce glass bottles. The bottled
product was then brought to ambient conditions and stored.
A sample fruit punch beverage for comparison to the
control was prepared from the following ingredients:
Sucrose...................................... 689.99* grams
High Fructose Corn Syrup (68.5 Brix)......... 385.01 grams
Citric Acid.................................... 12.86 grams
Water........................................ 7429.83 grams
10 Kelcoloid-0} ........................... ... , 3.26 grams
(Dry Blended with Sucrose)
CMC-7LF................................... ...... 1.31 grams
Fruit Punch Concentrate................... .... 219.74 grams
TOTAL: 8742.00
(8.32 liters)
*The sucrose content of the sample beverage was adjusted to
take into account the solids contributed by the gum blend.
This product had a pH of about 3.0 (+ 0.2), 0.30~ acid and
12.5 Brix and was packaged in a manner identical to that
employed for the control beverage.
Initial sampling of control and sample indicated that
neither possessed a gummy or slimy mouthfeel. After 18
hours storage at ambient conditions, the control exhibited
a light to medium degree of precipitation of solids and
a moderate to heavy degree of precipitation after four days.
The sample beverage, however, exhibited no sedimentation
of solids even after five days of ambient storage.
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~i717;~3
EXAMPLE V
Three sample powdered lemonade beverage mixes were
prepared by first dry blending a mixture of dried lemon
juice powder, sucrose, tricalcium phosphate and powdered
lemon flavor to form a base mixture. This base then was
used to prepare the three samples by mixing additional dry
ingredients therewith according to the following table:
INGREDIENTSAMPLE 1 SAMPLE 2 SAMPLE 3
Base 957.00 gms 957.00 gms 957.00 gms
Sucrose*(dry) 3.98 gms 1.22 gms ---
~elcoloid-0 --- --- 3.26 gms
CMC-7LF --- 3.15 gms 1.31 gms
960.98 gms 961.37 gms 961.57 gms
*The sucrose content of the samples was adjusted to take into
account the solids contributed by the gum blend.
The three sample mixes were reconstituted in separate
beakers to identical degrees (11.0 Brix) to provide single-
strength beverages having a pH of 3.1 and 0.45-0.51% acid.
None of the so-prepared beverages exhibited a gummy or slimy
mouthfeel or off-flavors. Within one hour of preparation and
storage at ambient conditions, Sample 1 exhibited separation
of solids as did Sample 2 to a slightly lesser degree. Sample
3 showed no such separation. After an additional 96 hours
refrigerated storage, Sample 1 displayed a heavy precipitation
of solids at the bottom of the beaker while Samples 2 and 3
5 exhibited only a slight precipitation.
EXAMPLE VI
A lemon based single-strength beverage was prepared
from the following ingredients:
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Lemon Concentrate (30.8% lemon acid)............ 154.45 gms
Lemon Oils...................................... 1.06 gms
Ascorbic Acid................................... 3.84 gms
Sodium Citrate.................................. 1.30 gms
High Fructose Corn Syrup (70.6 Brix)........... 517.05 gms
Kelcoloid-0..................................... 3.26 gms
CMC-7LF......................................... 1.31 gms
Sucrose......................................... 547.57 gms
Water........................................... 7477.16 gms
TOTAL: 8707.00 gms
(approx. 8.32 liters)
The beverage had a pH of 2.70, 0.57% acid and 11.5 Brix and
was hot-packed into four 64 oz. glass bottles. After over-
night storage at ambient conditions, the beverage displayed
acceptable flavor, mouthfeel and stability.
Utilizing the identical ingredients, amounts, pro-
cedure and testing shown above, two additional beverages
were prepared wherein the CMC-7LF, a low viscosity sodium
carboxymethylcellulose, was replaced with CMC-7MF (medium
viscosity) and CMC-7HF (high viscosity) respectively. The
beverages prepared from these formulations exhibited sub-
stantially the identical properties noted for the sample
prepared with CMC-7LF, with the exception that the CMC-7HF
containing beverage possessed a very slightly thicker mouth-
feel than the other beverages.
In the foregoing examples, the manufacturing procedure
employed, as earlier noted, is not critical provided the
ingredients of the product are suitably mixed and dispersed
and the gum system is added in a manner to achieve suitable
hydration, dispersion and dissolution in the product. A number
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~171728
of procedures for insuring adequate dispersion of gums in
aqueous systems are known and may be employed in the present
invention. Preferred among these methods is the use of an
eductor (e.g., Hercules Model 141 Mixing Device) wherein
gums are wetted by a high velocity stream of water in the
throat portion of the eductor and discharged directly into a
receiving vessel containing the remaining liquid mixture of
ingredients.
A considerable benefit of the present invention is
the ability to stabilize juice-containing products with a
gum system without appreciably adversely affecting (i.e.,
increasing) the viscosity of the product as perceived by the
ultimate user. In one experiment, the viscosity of identically
prepared lemonade beverages (containing 10% lemon juice, corn
and sugar sweeteners) with and without the gum stabilizer
system (0.0375% Kelcoloid*-0; 0.015% CMC-7LF; percents by
weight of total weight single-strength beverage) was measured
at 20C and 25C using a Brookfield* Viscometer (Model LVF
with U.L. adapter) at two different spindle speeds. At 30
R.P.M. spindle speed, the sample without gums had a viscosity
of 1.60 cp at 20C and 1.43 cp at 25C as compared to 1.71 cp
and 1.54, respectively, for the gum-containing sample. At a
spindle speed of 60 R.P.M., the measurements at 20C and 25C
for the gum-free sample were 1.54 cp and 1.36 cp as compared
to 1.73 cp and 1.51 cp for the gum-containing sample. Such
measured differences are imperceptible using sensory means.
*Trademarks
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t~-
117~7;~8
The propylene glycol alginate utilized in the present
invention is a low viscosity variety thereof. Such products
are commercially available and generally are characterized by
viscosity values of between about 50 and 175 centipoise for
2~ w/w aqueous solutions thereof measured at 25C with a
Brookfield LVF Viscometer (No. 2 spindle, 60 R.P.M.). The
sodium carboxymethylcellulose employed may, as shown in the
Examples, vary more widely in its viscosity. However, low
viscosity types are preferred, for example, those characterized
by viscosity values of between about 25 to 50 centipoise for
2% solids w/w aqueous solutions thereof measured at 25C with
a Brookfield LVF Viscometer (No.l spindle, 60 R.P.M.).
The quantities of each such gum are chosen so as to
achieve effective stabilization of the particular juice-
containing product (i.e., prevention or reduction of solidsseparation) while minimizing undesired changes in organoleptic
properties such as fla~orand mouthfeel. As such, the quantities
chosen will depend, for example, upon the type gum employed
(e.g., low or high viscosity), the relative ratios of the
gums, and the type product being treated. Utilization of too
little of the gum system will result in ineffective stabiliza-
tion whereas an excess amount of the gum system may undesirably
thicken the product or, indeed, result in the counter-productive
separation of gum solids in the product. Typically, additive
~5 levels will fall within the range of from about 0.015 to about
0.20% for the propylene glycol alginate and from about 0.01
to about 0.10~ for the sodium carboxymethylcellulose, percents
by weight of the total weight of single-strength product.
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li~717~8
Hence, additive levels to dry mixes or aqueous-based
concentrates will be chosen so as to result in the presence
of the gums within the mentioned levels when the mix or con-
centrate is reconstituted to a single-strength product.
Fruits which may be used as the basis for the fruit
juice-containing products to which the present invention is
applicable include lemon, grapefruit, lime, orange, tomato,
pineapple and the like as well, of course, as mixtures of
juices from one or more such products. Additionally, the
gum system of the present invention may be employed to reduce
or prevent solids separation in products wherein fruit juices
are combined with vegetable-derived juices and in products
solely containing such vegetable juices.
In a number of controlled experiments, the efficacy
of a number of known hydrophilic colloids to effectively
reduce or prevent separation of solids in fruit juice-
containing products was tested. Among the gums tested were
locust bean gum, furcelleran, pectin, gum acacia, gum traga-
canth, guar gum, xanthan gum, sodium carboxymethylcellulose,
propylene glycol alginate, differing varieties of these gums
and mixtures thereof. In all cases, no single gum or
combinations displayed the effectiveness found for the pro-
pylene glycol alginate and sodium carboxymethylcellulose com-
bination with respect to reducing or preventing solids
separation. Additionally, the gum combination of the present
invention possesses the advantages of ease of incorporation
into the manufacturing process, compatability with conventional
ingredients of juice-containing products, lack of significant
..~
~ - 15 -
117~ 8
effect on the viscosity of the product and absence of dis-
advantageous organoleptic effects, e.g., gritty or slimy
mouthfeel, off-flavors, and the like.
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