CA2046741C - Whey protein concentrate and its use in ice cream - Google Patents

Whey protein concentrate and its use in ice cream

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Publication number
CA2046741C
CA2046741C CA002046741A CA2046741A CA2046741C CA 2046741 C CA2046741 C CA 2046741C CA 002046741 A CA002046741 A CA 002046741A CA 2046741 A CA2046741 A CA 2046741A CA 2046741 C CA2046741 C CA 2046741C
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Canada
Prior art keywords
whey protein
whey
protein concentrate
ice cream
denatured
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
CA002046741A
Other languages
French (fr)
Other versions
CA2046741A1 (en
Inventor
Yashavantkumar Jayasinh Asher
Martha Ann Mollard
Suzette Thomson
Terry J. Maurice
Karen B. Caldwell
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Lactalis Canada Inc
Original Assignee
Parmalat Food Inc
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Publication date
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Publication of CA2046741A1 publication Critical patent/CA2046741A1/en
Application granted granted Critical
Publication of CA2046741C publication Critical patent/CA2046741C/en
Anticipated expiration legal-status Critical
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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23GCOCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G9/00Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
    • A23G9/32Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
    • A23G9/40Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds characterised by the dairy products used
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING OR TREATMENT THEREOF
    • A23C13/00Cream; Cream preparations; Making thereof
    • A23C13/12Cream preparations
    • A23C13/16Cream preparations containing, or treated with, microorganisms, enzymes, or antibiotics; Sour cream
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING OR TREATMENT THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/12Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/1307Milk products or derivatives; Fruit or vegetable juices; Sugars, sugar alcohols, sweeteners; Oligosaccharides; Organic acids or salts thereof or acidifying agents; Flavours, dyes or pigments; Inert or aerosol gases; Carbonation methods
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/20Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey
    • A23J1/205Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey from whey, e.g. lactalbumine
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00Working-up of proteins for foodstuffs
    • A23J3/04Animal proteins
    • A23J3/08Dairy proteins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L23/00Soups; Sauces; Preparation or treatment thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/60Salad dressings; Mayonnaise; Ketchup
    • A23L27/66Use of milk products or milk derivatives in the preparation of dressings
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17Amino acids, peptides or proteins
    • A23L33/19Dairy proteins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Nutrition Science (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Mycology (AREA)
  • Zoology (AREA)
  • Inorganic Chemistry (AREA)
  • Dairy Products (AREA)
  • Confectionery (AREA)
  • Peptides Or Proteins (AREA)

Abstract

Whey protein concentrate having at least about 50% of its protein denatured is produced and used in the production of non-fat, low fat and high fat ice cream.

Description

1S ~

This invention relates to whey protein concentrate and to ice cream utilizing whey protein concentrate as an ingredient. In this application, the term Uice cream"
covers full fat ice cream, reduced fat ice cream, low fat ice cream and non-fat ice cream.

Whey is a by-product when cheese is produced from milk. After suitable pre-treatment well known to persons skilled in the art, milk is treated with a suitable culture to produce curd which is subsequently separated from the remaining liguid, namely dairy ~hey, and used to make cheese. It is known that whey contains useful proteins, generally known as dairy whey proteins. It is also known that the principal proteins in such whey are B-lactoglobulin and ~ -lactalbumin. Other proteins include serum derived immttnoglobulins. Proteose peptones are also present.

Large quantities of whey are produced as a by-product of cheese production, and various uses for such whey have been developed over the years, mainly as a food ingredient. Such whey usually contains about 1~% protein by weight on a total solids basis. It has become conventional to further treat the whey to provide a product containing at least about 30~ protein by weight on a total solids basis which is known as whey protein concentrate. It is usually whey protein concentrate rather than the oriyinal whey which is used as a food ingredient.

Whey protein concentrate has been used as an ingredient in ice craam production, namely in the production of full fat ice cream or reduced fat ice cream and has been proposed as an ingredient in low and non-fat ice cream (sometimes called low and non-fat frozen dairy dessert), see for e~ample U.S. Patent 4,840,81~ (Greenberg et al.).

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However, a major obstacle to such use, particularly in low and non-fat ice cream, has been the fact that the whey protein concentrate tends to cause coagulation of the ice cream mi2 while it is being pasteurized, with the result that ice cream production has to be shut down to enable the coagulated material to be removed. This is because, in the past, the whey protein concentrate used has been whey protein concentrate of a conventional kind, namely with at least most of its protein in the natural state, i e.
undenatured.

It has now been discovered that the problem of coagulation in ice cream production using whey protein concentrate can be substantially overcome if the denaturation of the whey protein in the whey protein concentrate is controlled during its production so as to be at least about 50% relative to untreated cow's milk (i.e.
raw milk), preferably in the range of from about 50 to about 90%, and more preferably from about 60 to about 80%, when measured by the method described at the end of this speci~ication.

~ elow about 50%, the prior art problem of coagulation during ice cream production arises. Above about 90%, the ice cream product may have a somewhat sticky, gummy mouth feel which may be unacceptable to some consumers.
However, some consumers are used to and like such a mouth feel.

Since persons skilled in the art may interpret the meaning of denaturation and the manner in which denaturation should be measured in different ways, percentage denaturation in this application means the percentage denaturation when calculated in accordance with the methodology described.

20467~

Because of the comple~ nature of the protein content of whey protein concentrate, the reason for the success of the present invention is not clearly understood.
It had previously been believed that the whey protein concentrate used in ice cream production should initially have at least most of its protein in the undenatured state in order to produce acceptable ice cream.

It is possible, although not certain, that the advantages are connected with the relative degree of denaturation of different proteins, such as B-lactoglobulin and ~-lactalbumin, when the denaturation is as specified in the present invention.

Advantageously, to achieve denaturation in accordance with the present invention, whey is ultrafiltered and the ultrafiltered whey is subjected to a high heat treatment step, with this high heat treatment step preferably being carried out prior to concentration of the ultrafiltered whey to form whey protein concentrate.

The whey protein concentrate of the present invention may be used in the production of full fat or reduced fat ice cream or in the production of low or non-fat ice cream.

Preferred embodiments and e~amples of the invention will now be described, by way of e~ample only, with reference to the accompanying drawings, of which:

. 2~7~

Figure 1 is a schematic view of a process for producing cheese and also whey protein concentrate in accordance with the invention, Figure 2 is a schematic view of a process for making 0% fat ice cream in accordance with the invention, Figure 3 is a schematic view of a process for making 1~ (by weight) fat ice cream in accordance with the invention, and Figure 4 is a schematic view of a process for making ice cream with 7%
(by weight) and higher amounts of fat in accordance with the invention.

Referring to Figure 1, which shows the preparation of whey protein concentrate in accordance with a preferred embodiment o~ the in~ention, raw milk at a temperature of ~rom about 3 to about 6~C is preheated in a preheating step 10 to a temperature of from about 43 to about 49~C and then passed to a ~at separation step 12 where some fat is separated, the actual amount depending upon the type o~
cheese to be produced. The preheated fat-reduced mîlk is then pasteurized in a pasteurization step 14 at a temperature of about 73~C ~or~about 20 seconds, with subsequent cooling to a temperature of from about 32 to about 38~C. The pasteurized fat-reduced milk then passes to a curd forming step 16 where lactic culture is injected and rennet is added in known manner and the contents are cooked and cut to produce curd.

2Q~.~7~

The resultant curd/whey slurry is pumped to curd removal step 18 where raw whey is drained off at a temperature of from about 38 to about 41~C. The curd is subsequently processed into cheese in any desired manner.
At this stage, the protein in the whey is from about 5 to about 10% denatured, relative to the raw milk, most of the denaturation having occurred when the milk was pasteurized in the pasteurization step 14.

The whey from curd removal step 18 is pumped to pasteurization step 20 where further pasteurization occurs at a temperature of about 74~C for about 30 seconds, with subsequent cooling to a temperature of from about 50 to about 52~C. This treatment causes further denaturation of the protein such that the protein is then from about lO to about 15% denatured relative to the raw milk. The pasteurized whey is pumped to an ultrafiltration step 22 where the whey is ultrafiltered with a membrane having a nominal molecular weight cut-off of 5,000. The permeate from ultrafiltration step 20 may be used as desired. Most of the lactose in the whey will be in the permeate.

The retentate, namely ultrafiltered whey with about 9% total solids by weight, is pumped to a heat treatment step 24 where it is subjected to high treatment in a plate heat exchanger at a temperature of about 80~C for about 17 seconds. Further denaturation occurs during the stage such that the protein in the whey is from about 60 to about 80%
denatured relative to the raw milk. The pasteuri~ed ultrafiltered whey proceeds to a concentration step 26 where evaporation is carried out at a temperature of about 69~C
under a vacuum of about 23 inches Hg to concentrate the total solids content to from about 30 to about 32% by weight. ~fter concentration step 26, the whey protein concentrate (WPC) is cooled to about 6~C in a cooling step 28.

2Q~7~
The denaturation of the whey protein concentrate produced in accordance with the process described above can be controlled so as to be at a value in accordance with the invention by varying the temperature and/or time in high heat treatment step 24.

It is envisaged that whey protein concentrate in accordance with the invention may have beneficial uses other than in ice cream, for example in yogurt.

Referring now to Figure 2, a process for preparing 0% fat ice cream in accordance with a preferred embodiment of the invention includes blending liquid sweetener, namely high fructose corn syrup, and water in a blending step 30.
The resultant blend from blending step 30 is then blended with a first dry blend in a blending step 34, the first dry blend comprising skim milk solids, sweeteners, namely corn syrup solids and dry sugar, and bulking agents, namely tapioca starch and maltode~trin. The resultant blend from blending step 32 is blended with a second dry blend in blending step 3~, the second dry blend comprising stabilizers! namely guar gum, carrageenan, locust bean gurn, micro-crystalline cellulose gum, carboxy-methyl cellulose gum and ~anthan gum and emulsifiers, namely mono-diglycer~des. The resultant blend o~ dairy ingredients, sweeteners, bulking agents, stabilizers and emulsifiers from blending step 34 is then blended in a blending step 36 with whey protein concentrate from the process described with reference to Figure 1 to form an ice cream mi~.

The ice cream mi~ from blending step 36 is pasteurized in a pasteurization step 38 at about 78~C for about 10 minutes and is then homogenized in a wo-stage homogenization step 40. The first stage is carried out at a pressure of about 2500 p.s.i. and the second stage is carried out at a pressure of about 800 p.s.i. The homogenized blend is then cooled in a cooling step 42 to about 4~C, and the cooled blend is then aged for about 24 hours in an aging step 44.

7 ~ ~

The aged blend is passed to a flavouring step 46 where appropriate flavouring is added, and the flavoured blend is frozen and whipped with an overrun (i.e. increase in volume due to air content) of from about 40 to about 80%
in a freezing step 48 to produce 0% fat ice cream which is then e~truded from the freezing step 48 at about -6~C. The ice cream is then hardened in a hardening step 50 until a core temperature (in a two litre container) of about -18~C
is reached, this being in about 2 hours.

By way of e~ample, preferred ranges of the ingredients for 0% fat ice cream are as follows:

Per Cent Solids By Weight Innredients Of Total Mix Water to make up 100%
High Fructose Corn Syrup 7 to 12 First DrY Blend Skim Milk Solids 1 to 10 Corn Syrup Solids 2 to 6 Dry Sugar 5 to 8 Tapioca Starch 0 to 2.5 Maltodextrin 0 to 4 Second DrY Blend Guar Gum 0.04 to 0.1 Carrageenan O.OI to 0.04 Locust Bean Gum 0 to 0.05 Mîcro crystalline Cellulose Gum 0 to 0.5 Carbo~y-methyl-cellulose Gum ~ 0 to 0.4 Xanthan Gum 0 to 0.1 Mono-diglycerides 0 to 0.1 2~7~ ~

Per Cent Solids By Weight Whey Protein Concentrate Of Total Mix From about 30 to about 40 protein by weight on a total solids basis -60 to 80% Denatured 25 to 40% solids by weight 2 to 7 In a specific example of the invention, the ~ollowing ingredients for 0% fat ice cream were used:

Per Cent Solids By Weight Inqredients Of Total Mix Water to make up 100%
High Fructose Corn Syrup . 10.00 First DrY Blend Skim Milk Solids 3.00 Dry Corn Syrup Solids 4.00 Dry Sugar 4.75 Tapioca Starch 2.00 Maltode~trin 3.00 Second DrY Blend Guar Gum 0,05 Carrageenan 0.03 Locust Bean Gum 0.04 Micro-crystalline CelluIose Gum 0.3 Carboxy-methyl-cellulose Gum0.03 Xanthan Gum 0.06 Mono-diglycerides 0.07 2~ ~7~1 Per Cent Solids By Weight Whey Protein Concentrate Of Total Mi~
35% protein by weight on a total solids basis -71% Denatured 31% solids by weight 7 The liquid blend is blend~d in a Lanco blender for two minutes at a speed of 1300 r.p.m. The first dry blend is then added slowly and blending is carried out for a further 5 minutes at the same speed. The second dry blend is then added and further hIending is carried out for 5 minutes at the same speed. The speed is then reduced to 400 r.p.m., and the whey protein concentrate is added and further blending carried out for 2-3 minutes. The resultant blend is then treated in the manner described above with reference to Figure 2.

Referring now to F;gure 3, a process for preparing 1% fat (by weight) ice cream in accordance with a preferred embodiment of the invention includes blending liquid sweeteners, a dairy fat source such us cream and/or butter fat and water in a blending step 52, the liquid sweeteners comprising liquid sugar, liquid corn syrup solids and high fructose corn syrup. The resultant blend from bl~ending step 52 is blended with a dry blend in a blending step 54, the dry bl nd comprising skim milk solids and~stabili;zers, namely guar gum, carrageenan, locust bean gum~and micro-crystalline cellulose gum. The resultant blend of da~iry ingredients (including fat), sweeteners~and stabilizers from blending step 54 is then blended in a blending step 56 with whey protein concentrate from the process described with reference to Figure 1 to form an ice cream mix.
::

:' ,,-.

The ice cream mi~ from blending step 56 is pasteurized in a pasteurization step 58 at a temperature of about 82~C for about 32 seconds and is then homogenized in a two-stage homogenization step 60. The first stage is carried out at a pressure of about 1800 p.s.i. and the second stage is carried out at a pressure of about 700 p.s.i. The homogenized blend is then cooled in a cooling step 62 to about 4~C. The cooled blend is then aged for about 24 hours in an aging step 64.

The aged blend then passes to a flavouring step 66 where appropriate flavour is added and the flavoured blend is frozen and whipped with an overrun of from about 40 to about 80% in a freezing step 68 to produce 1% fat ice cream which is then extruded from freezing step 68 at about -6~C.
The 1% fat ice cream is hardened in a hardening step 70 until a core temperature (in a two litre container) of about -18~C is reached, this being in about 2 hours.

By way of example, preferred ranges of ingredients for 1% (by weight) fat ice cream are as follows:
Per Cent Solids By Wei~ht In~redients Of Total Mi~

Liquid Blend Liquid Sugar 4 to 8 Liquid Corn Syrup Solids 2 to 6 Water to make up 100%
Cream/Butter Fat 0.5 to 1.5 High Fructose Corn Syrup 7 to 12 DrY Blend Skim Milk Solids 1 to 10 Carrageenan 0.01 to 0.04 Guar Guam 0.01 to 0.1 Locust Bean Gum 0 to 0.05 Micro-crystalline Cellulose Gum0 to 0.5 Per Cent Solids 'By Weight WheY Protein ConcentrateOf Total Mix From about 30 to about 40%
protein by weight on a total solids basis -60 to 80% Denatured 25 to 40% solids by weight 2 to 7 In a specific esample of the invention, the following ingredients for 1% (by weight) fat ice cream were used:

Per Cent Solids By Weight Inaredients Of Total Mix Li~uid Blend Liquid Sugar 4.75 Liquid Corn Syrup Solids 4.00 Water to make up 100%
Cream/Butter Fat 0.65 High Fructose Corn Syrup 10.00 DrY Blend Skim Milk Solids 4.00 Carrageenan 0.04 Guar Gum 0.016 Locust Bean Gum 0.010 Micro-Crystalline Cellulose Gum 0.008 WheY Protein Concentrate 35% protein by weight on a total solids basis -71% Denatured 31% solids by weight 7.0 2 ~

The liquld blend is blended in a Lanco blender for about 5 minutes at a speed of about 1300 r.p.m. The dry blend is then added and further blending carried out for about 5 minutes at the same speed. The speed is then reduced to about 400 r.p.m., the whey protein concentrate is added and ~urther blending carried out for 2-3 minutes. The resultant blend is then processed in the manner described aboYe with reference to Figure 3.

~ eferring now to Figure 4, a process for preparing ice cream with 7% (by weight) and higher amounts of ~at in accordance with a preferred embodiment of the invention includes blendinq liquid ingredients and water in a blending step 72, the liquid ingredients comprising liquid sugar, liquid corn syrup solids, whey solids, milk solids non fat, and a dairy fat source such as cream and/or butter fat. The resultant blend from blending step 72 is blended with a dry blend of stabilizers and emulsifiers in a blending step 74, the stabilizers being carrageenan, locust bean gum, guar gum and micro-crystalline cellulose gum, and the emulsifiers being polysorbate 80 and mono-diglycerides.

The blend of dairy ingredients, sweeteners, stabilizers and emulsi~iers from blending step 74 is then blended in a blending step 75 with whey protein concentrate from the process described with reference to Fig. 1 to form an ice cream mix. The ice cream mix from blending step 76 is pasteurized in a pasteurization step 76 at about 81~C for about 32 seconds and is then homogenized in a two stage homogenization step 78. The first stage is carried out at a pressure of about 1500 p.s.i., and tbe second stage is carried out at a pressure of about 700 to 800 p.s.i. The homogenized blend is then cooled in a cooling step 80 to about 4~C, and the cooled blend is aged for about 24 hours in a aging step 82.

2 ~

The aged blend is passed to a flavouring step 84 where appropriate flavouring is added, and the flavoured blend is frozen and whipped with an overrun of from about 30 to about 110% in a ~reezing step 86 to produce ice cream with 7~ fat or higher ~~or e~ample up to about 20% fat) which is then e2truded from freezing step 86 at about -6~C.
The ice cream is hardened in a hardening step 88 until a core temperature (in a two litre container) of about -18~C
is reached, this being in about 2 hours.

By way of e~ample, preferred ranges of the ingredients for ice cream with 7% Sby weight) fat or higher are as follows:
Per Cent Solids By Weight Inqredients Of Total Mix I,iquid Blend Water to make up 100%
Sucrose Solids 6 to 12 Corn Syrup Solids 3 to 7 Total Fat 7 to 15 Whey Solids 0 to 6 Milk Solids Non Fat 1 to lO

DrY Blend Carrageenan 0.01 to 0.04 Locust Bean Gum 0 to 0.05 Guar Gum 0.04 to 0.1 Micro-crystalline Cellulose Gum 0 to 0.4 Polysorbate 80 0 to 0.1 Mono-diglycerides 0 to 0.25 Whey Protein Concentrate 2 to 9 (as in the previous e~amples) In a specific e~ample of the invention, the ~ollowing ingredients were used for 7% (by weight) fat ice cream:

Per Cent Solids By ~eight Inqredients Of Total Mi~
Liquid Blend Water to make up 100%
Sucrose Solids 10.80 Corn Syrup Solids 7.00 : Total Fat 7.20 Whey Solids 3.30 Milk Solids ~on Fat 3.875 DrY Blend Carrageenan 0.015 Locust Bean Gum 0.0375 Guar Gum 0.06 Micro crystalline Cellulose Gum 0.03 Polysorbate 80 0.02 Mono-diglycerides 0.08 WheY Protein Concentrate 4.375 (as in the previous examples) In a specific example o~ the invention, the following ingredient~ were used for 10% (by weight) fat ice cream:
Per Cent Solids By Weight Inqredients Of Total Mix ' :
: Liquid Blend Water : to make up 100%
Sucrose Solids : 10.'80 : Corn Syrup Solids ~ ~ ~7.00 ' ~ Total Fa~ : ~ :10~.20 Whey Solids : 3.30 Milk Solids ~on Fat: ~ ~ 3.87 ::
: - 14 -::

:' :

..
:: :

2~6~

Per Cent Solids By Weight Dry Blend Of Total Mix Carrageenan 0.0145 Locust Bean Gum 0.036 Guar Gum 0.058 Micro-crystalline Cellulose Gum 0.029 Polysorbate 80 0.02 Mono-diglycerides 0.08 WheY Protein Concentrate 3.88 ~as in the previous e~amples) In a specific e~ample of the invention, the following ingredients were used for 15~ (by weight) fat ice cream:

Per Cent Solids By Weight Inqredients Of Total Mix Liquid Blend Water to make up 100%
Sucrose Solids 12.00 Corn Syrup Solids 4.00 Total Fat 15.00 Milk Solids ~on Fat 4.50 : DrY Blend Carrageenan ~ 0.030 Locust Bean Gum : 0.075 Guar Gum ~ ;0.120 Micro-crystalline Cellulose Gum : 0.060 Polyso:rbate 80 ~ 0.040 : Mono-diglycerides ~ ; 0.160 WheY Protein Concentrate : 4.50 (as in the pre~ious e~amples) -~ 15 -~: - , - , ~.
:
:

2 ~ 7 ~ ~

CALCUhATION OF PERCENTAGE DENATURATION

The methodology for calculating the percentage denaturation of the whey protein concentrate will now be described.

In the broadest sense, denaturation of protein refers to any conformational change in the three dimensional structure of a protein away from its native state. For the purpose of this and in fact most methods which characterize denaturation, the conformational changes must result in a loss of solubility of the protein.

This method involves measuring the protein which remains in solution after a mechanical separation of the precipitated (denatured) portion.

This is a comparative method in which a reference sample is used as a point of "zero denaturation". In most cases, this re~erence will in fact be partially denatured to a degree which may or may not be known. What is being measured is the percent denaturation in the sample with respect to the reference.

Usually the denaturation of the sample in question is associated with a processing step such as a high heat treatment. In this case, the reference could simply be the sample prior to high heat treatment.
~:
The reference sample is centrifuged to separate out the precipitated proteins. The protein which remains in soluti~on is quantified by W spectroscopy.

:

2 ~

The reference is then completely heat denatured and precipitated proteins are separated by centrifugation.
Again, the protein which remains in solution is quantified by W spectroscopy-The sample in question is then centrifuged and theprotein in solution is measured by W spectroscopy. By comparing the spectroscopic data for the sample to the data for the undenatured and completely denatured reference, a relative percent denaturation can be calculated.

ULTRAVIOLET SPECTROSCOPY

The amount of W radiation which a sample absorbs is a function of the concentration of the absorbing components within the sample. This relationship is linear and can be e~pressed in terms of the Beer-Lambert law.

A = ~bc Where: A ~ Absorbance ~ = E~tinction Coe~ficient b ~ Path Length c - Concentration The e~tinction coefficient (~) is a constant for a given substance and the path (b) is a constant for a given cuvette.

For this method, the absoxbances of the aromatic amino acids, tyrosine and tryptophan in the region of 280 nm are used to characterize the concentration of protein in solution. B-lactoglobulin and ~-lactalbumin contain these amino acids in different proportions.

2 0 ~ 6 ~

Both tyrosine and tryptophan absorb in the 280 nm range. The broad peak which is seen in this region is therefore a composite of absorption peaks of these two amino acids. The two peaks can be viewed separately by looking at the first deri~ative of the wavelength scan.

Pure solutions of ~LA and B~G are used to determine the e~tinction coefficients of each of these proteins.
Accurately prepared mi~tures containing different ratios of the two proteins are used to determine composite extinction coefficients for blends.

PERCENT DENATURATION

Once protein concentration in the sample ~Csample)~
the undenatured re~erence (CZerO)~ and the completely denatured reference (C100%) have been determined, the percent denaturation is determined by the following equation.

% DenaturatiOn = ~(Czero Csample)/~ zero 100%)] ~ 100 SAFET~ CONSIDERATIONS

This method does not involve any hazardous chemicals. Proper care should be exercised when using the superspeed centrifuge~

2~ ~7~1 APPARATUS

1. Double Beam Scanning W Spectrophotometer and Quartz Cuvettes (Shimadzu W 160U) 2. Superspeed Centrifuge and Tub~s (approx. 25000 G) 3. Boiling Water-Bath 4. 250 ml volumetric flasks 5. Ice-Bath 6. Computer and Spectra-Calc, and RS-l Software Packages REAGENTS

1. Distilled Water 2. Purified ~-lactalbumin (Sigma L-7269) 3. Purified ~-lactoglobulin (Sigma L-0130) PROCEDURE

1. Determination Of Extinction Coefficient For d-lactalbumin a) Accurately prepare a minimum of 5 solutions (10 ml each) of pure ~LA ranging from 0.02 to 0.12% (w/w).

: b) :Set up the parameters of the W
spectrophotometer~as follows: :

Mode: Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow 2 !~

c) Run a baseline correction on the instrument using distilled water in the reference and sample holders.

d) Scan each solution of ~LA using distilled water as the reference.

; e) Accurately record the peak absorbance in the 280 nm region for each sample. (Use Spectra-Calc to determine peak A) ~See "CALCULATIO~S" section for determination of ~) 2. Determination Of E~tinction Coefficient For B-lactoqlobulin a) Accurately prepare a minimum of 5 solutions (10 ml each) o~ pure ~LG ranging from 0.04 to 0.20~ (w/w).

b) Set up the parameters of the W
spectrophotometer as follows:

Mode: ~Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow c) Run a baseline correction on the instrument using distilled~water ln the reference and sample~holders.

d) Scan each solution of BLG using distilled ; water as the reference.

2~$~

e) Accurately record the peak absorbance in the 280 nm region for each sample. (Use Spectra-Calc to determine Peak A) (See "CALCULATIONS" section for determination o~ ~ ) 3. Determination Of Composite Extinction Coefficients a) Accurately prepare 0.1% (w/w) solutions (25 ml of each) of pure ~LA and BLG.

b) Using these solutions, accurately prepare a minimum of 6 composite samples of varying protein ratios.

c) Set up the parameters of the W
spectrophotometer as follows:

Mode: Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow d) Run a baseline correction on the instrument using distilled water in the reference and sample holders.

e) Scan each composite sample with distilled water as the reference~.~;Using Spectra-Calc, determine the~m~im~lm~peak intensities of the two main first derivative peaks.~ These peaks will~be at app~ro~imately 293 and 286 nmO
(See "CALCULATIONS" section for the determination of~compos~1te ~) ~

, ::

' 4a. Analysis of Reference Sample (Zero Point) a) Accurately dilute a portion of the reference sample to a solids level of 0.4%.

b) Centrifuge at room temperature for 20 minutes at approximately 25000 G.

c) Set up the parameters of the W spectrophotometer as follows:

Mode: Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow d) Run a baseline correction on the instrument using distilled water in the reference and sample holders.

e) Scan the supernatant using distilled water in the reference cuvette.

f) Record the peak absorbance (280 nm) as well as the peak intensity of the two main first derivative peaks. (Use Spectra-Calc software) 4b. Analysis of Reference Sample (100% Denaturation Point) a) Fill about 5 250 ml volumetrics with the reference sample.

b) Place the flasks into a boiling water bath and remove 1 every twenty minutes.

For Each Sample:

c) Cool in an ice-bath and use distilled water to bring the volume back to 250 ml.

d) Accurately dilute to 0.4~ solids and centrifuge for 20 minutes at approximately 25000 G.

e) Set up the parameters for the W spectrophotometer as follows:
Mode: Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow f) Run a baseline correction on the instrument using distilled water in the reference and sample holders.

g) Scan the supernatant using distilled water in the reference cuvette.

h) Record the absorbance at 280 nm and the intensities of the two main first derivative peaks.

i) Continue testing samples until there is no further decrease in the absorbance at 280 nm, i.e. after about 60 minutes.

5. Analysis of Unknown Sample a) Accurately dilute the sample to 0.4% solids.

b) Centrifuge for 20 minutes at 25000 G.

c) Set up the parameters of the W spectrophotometer as follows:
Mode: Wavelength Scan Wavelengths: 400 to 230 nm Scanning Speed: Slow d) Run a baseline correction on the instrument using distilled water in the reference and sample holders.

e) Scan the supernatant using distilled water in the reference cuvette.

f) Record the absorbance at 280 nm and the intensities of the two main first derivative peaks.

CALCULATIONS

1. Extinction Coefficient For ~-lactalbumin a) Plot a graph of peak absorbance as a function of concentration for the solutions of pure ~LA.

2~7~

b) Using RS-l, fit a linear function to the data using the following format:
Absorbance = e x Concentration c) ~dLA = e 2. Extinction Co~efficient For:~B-lactoqlobulin a) Plot a graph of peak abssrbance as a function of concentration for the solutions for pure ~LG.
::
b) Using RS-l, fit a linear function to the data using the following forrnat:
Absorbance = e x Concentration c) ~BLG = e 3. ComPosite E~tinction Coef~icient a) Plot a graph of the Ratio ~LA/BLG as a function of the ratio o~ the first derivative peaks (A293nm/A286nm) for each of the composite protein samples.

b3 Using RS-l, fit a function to the data using the following format~
LA/~LG = a~+ [b x ~A293nm/A286nmj]
: determine: a, b,~:and n :

: : ' : ;
: -~25 -:: :: :::
:

2 ~

4. Concentration Of Reference SamPle (Zero Point) a) Calculate the ratio of the two main first derivative peaks.
A2 9 3nrn~A2 8 6nm b) Use this value in the equation derived in step 3 above to determine R, the:ratio dLA~BLG.

c) Calculate the soluble protein concentration, c(zero)~ in the undenatured reference sample as follows:

(zero) = A/C{~l/(R+~ BLG} + ~[l-~l/R~l)] ~ ~lLA}]
5. Concentratlon Of Reference SamPle ~100%) For the sample subjected to the longest heat treatment:

a) Calculate the ratio of the two main first derivative peaks.
A293nm/A286nm b) Insert this value into the equation derived in step 3 above to determine R, the ratio ~LA/~LG.

c) Calculate the soluble protein concentration, c(10O~), in the undenatured reference sample as follows: ~

~ C(100%) a A/[{~l/(R+l)]~ ~ ~BLG) ~ {~l-(l/R+l)] ~ ~LA~]
:

:~- 26 -:.
' , , 6. Concentration Of Unknown SamPle a) Calculate the ratio of the two main first derivative peaks.
A293nm/A286nm b~ Use this value in the equation derived in step 3 above to determine R, the ratio dLA/BLG.

c) Calculate the soluble protein concentration, c(sample)~ in the undenatured reference sample as follows: :
C(sample) = AJ L{[1~(R+1)] ~ ~LG} ~ {~1 (l/R+ )] ~ LA~
7. Determination Of De~ree Of Denaturation a) Calculate the percent denaturation relative to the re~erence sample as ~ollows:
Denaturation = C(C(zero) C(sample)/( (zero) (100~))] ~ 100 As previously mentioned, the percentage denaturation specified in the present invention is the percentage denaturation relative to raw milk.

Other embodiments and examples of the invention will be readily apparent to a person skilled in~the art f~om~the foregoing description o~ preferred embodlments and examples, the : scope of the invention being defined in the~~ollowing claims.
::

: ~- 27 -:
WPP1029 ~ : :

:
:

Claims (23)

1. A process for preparing whey protein concentrate comprising pasteurizing raw milk with resultant denaturation of some whey protein, forming curds in said milk, removing the curds from the remaining whey, subjecting the whey to an ultrafiltration step to remove lactose as permeate, subjecting the ultrafiltered whey retentate to heat treatment to denature further whey protein to cause a total of at least about 50% of the whey protein to be denatured relative to the raw milk, and concentrating the heat treated whey to produce whey protein concentrate.
2. A process according to claim 1 wherein from about 5 to about 10% of the whey protein is denatured when the raw milk has been pasteurized.
3. A process according to claim 1 wherein the whey is pasteurized after curd removal and before ultrafiltration.
4. A process according to claim 3 wherein from about 10 to about 15% of the whey protein relative to the raw milk has been denatured when the whey has been pasteurized.
5. A process according to claim 1 wherein the ultrafiltered whey retentate is heat-treated to denature further whey protein to cause a total of from about 50 to about 90% of the whey protein relative to the raw milk to be denatured.
6. A process according to claim 5 wherein the ultrafiltered whey retentate is heat treated to denature further whey protein to cause a total of from about 60 to about 80% of the whey protein relative to the raw milk to be denatured.
7. Whey protein concentrate prepared by the process of claim 1.
8. Whey protein concentrate prepared by the process of claim 2.
9. Whey protein concentrate prepared by the process of claim 3.
10. Whey protein concentrate prepared by the process of claim 4.
11. Whey protein concentrate prepared by the process of claim 5.
12. Whey protein concentrate prepared by the process of claim 6.
13. Whey protein concentrate containing from about 25 to about 40% by weight total solids, from about 30 to about 40% by weight of said solids being whey protein and at least about 50% of the whey protein being denatured relative to raw milk.
14. Whey protein concentrate according to claim 13 wherein from about 50 to about 90% of the whey protein is denatured.
15. Whey protein concentrate according to claim 14 wherein from about 60 to about 80% of the whey protein is denatured.
16. A process for preparing ice cream including forming an ice cream mix as an aqueous blend of solids comprising whey protein concentrate whose solids are in an amount from about 2 to about 9% by weight of the solids in the blend, said whey protein concentrate solids containing from about 30 to about 40% by weight whey protein and having at least about 50% of its whey protein content denatured relative to raw milk, and processing said mix to form ice cream.
17. A process according to claim 16 wherein the whey protein concentrate has from about 50 to about 90% of its whey protein content denatured.
18. A process according to claim 17 wherein the whey protein concentrate has from about 60 to about 80% of its whey protein content denatured.
19. A process according to claim 16 wherein said aqueous blend is prepared by first blending ingredients other than said whey protein concentrate, and then blending in said whey protein concentrate.
20. Ice cream prepared by a process according to any one of claims 16-19.
21. Ice cream prepared by a process according to any one of claims 16-19 and containing less than about 5% by weight fat.
22. Ice cream prepared by a process according to any one of claims 16-19 and containing about 1% by weight fat.
23. Ice cream prepared by a process according to any one of claims 16-19 and containing substantially no fat.
CA002046741A 1991-05-16 1991-07-10 Whey protein concentrate and its use in ice cream Expired - Lifetime CA2046741C (en)

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WO1993002567A2 (en) * 1991-08-01 1993-02-18 Ault Foods Limited Whey and ice cream products and processes
DE4313014A1 (en) * 1992-06-10 1993-12-16 Danmark Protein A S Videbaek Partly denatured whey protein product
EP0779035B1 (en) * 1995-07-04 2002-09-11 Snow Brand Milk Products Co., Ltd. Modified whey protein
US5858441A (en) * 1995-08-31 1999-01-12 Van Den Bergh Foods Company, Division Of Conopco, Inc. Low fat spread
US6635302B1 (en) 1998-11-20 2003-10-21 The Pillsbury Company Milk protein dispersions
DE19964370B4 (en) * 1999-02-16 2006-05-11 Huss, Manfred Preparation of a foamed whey protein product
EA200200582A1 (en) * 1999-12-23 2002-12-26 Нираньян Чхоталал Мехта METHOD OF OBTAINING FROZEN MILK DESSERT
US20060159804A1 (en) * 2002-12-24 2006-07-20 Bhaskar Ganugapati V Dairy protein process and applications thereof
DE102012216990A1 (en) 2011-09-21 2013-03-21 Hochschule Anhalt (Fh) Microparticulation of whey protein by thermal precipitation, comprises heating whey proteins below their isoelectric points for protein unfolding, and carrying out whey protein precipitation, when pH is increased in isoelectric region
EA029154B1 (en) * 2012-02-06 2018-02-28 Арла Фудс Амба Low-protein frozen confectionery product
CN103859025B (en) * 2014-03-22 2016-07-06 吉林大学 Ginsenoside's microcapsule Yoghourt and preparation method thereof
JP6518248B2 (en) 2014-06-30 2019-05-22 株式会社日清製粉グループ本社 Method of concentrating specific components in powder
PH12016501526B1 (en) * 2015-01-23 2024-05-17 Goodman Fielder Pte Ltd Milk based compositions comprising milk derived, denatured retentate

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FR2069930A7 (en) * 1969-12-09 1971-09-10 Bel La Vache Qui Rit Fromage Reincorporation of soluble whey proteins - into curd
US4120989A (en) * 1976-11-01 1978-10-17 Stauffer Chemical Company High protein pasta formulation
CH630243A5 (en) * 1978-05-11 1982-06-15 Nestle Sa PROCESS FOR RECOVERY OF WHEY PROTEINS.
GB2055846B (en) * 1979-07-03 1983-02-23 Express Dairy Foods Process for lowering the gelling temperature of whey proteins obtained from milk
US4675201A (en) * 1979-11-19 1987-06-23 Ciba Corning Diagnostics Corp. Protein composition characterized by lower thermogelation temperature and improved acid solubility
US4840813A (en) * 1987-08-24 1989-06-20 General Mills, Inc. Low and non-fat frozen dairy desserts and method of preparation
DE68914724T2 (en) * 1988-06-16 1994-08-11 Unilever Nv Edible plastic composition.

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CA2046741A1 (en) 1992-11-17
AU1750892A (en) 1992-12-30

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