GB2035330A - Recovering proteins from milk by ultrafiltration - Google Patents

Recovering proteins from milk by ultrafiltration Download PDF

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Publication number
GB2035330A
GB2035330A GB7933915A GB7933915A GB2035330A GB 2035330 A GB2035330 A GB 2035330A GB 7933915 A GB7933915 A GB 7933915A GB 7933915 A GB7933915 A GB 7933915A GB 2035330 A GB2035330 A GB 2035330A
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United Kingdom
Prior art keywords
milk
proteins
filtration
ultra
heat treatment
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Granted
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GB7933915A
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GB2035330B (en
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Societe des Produits Nestle SA
Nestle SA
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Societe des Produits Nestle SA
Nestle SA
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    • 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 THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/14Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • A23C9/142Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by dialysis, reverse osmosis or ultrafiltration
    • A23C9/1422Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by dialysis, reverse osmosis or ultrafiltration by ultrafiltration, microfiltration or diafiltration of milk, e.g. for separating protein and lactose; Treatment of the UF permeate
    • 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
    • A23J1/207Co-precipitates of casein and lactalbumine

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Water Supply & Treatment (AREA)
  • Biochemistry (AREA)
  • Dairy Products (AREA)

Abstract

A process is disclosed for separating one or more proteins from milk, which comprises subjecting the milk to a heat treatment in order to partially denature the proteins present therein, separating the proteins from the other non-fat constituents of the milk by ultrafiltration, the proteins ending up in the retentate fraction, and subsequently subjecting retentate fraction to a complementary heat treatment in order to denature the proteins. The milk proteins obtained may be used for preparing infant and/or dietetic products, and for making cheese.

Description

SPECIFICATION A process for recovering proteins from milk This invention relates to a process for recovering proteins from milk.
The traditional processes for recovering or separating proteins from milk use technologies based on the coagulation of casein, for example with animal or microbial rennet, or by biologicai or chemical acidification.
These processes have the following disadvantages: - non-retention of the serum proteins and, normally, losses thereof; presence of acid residues; - heavily polluting by-products (wheys); - difficult utilization of these by-products (acid wheys for example); - often unpleasant taste of the casein after drying; - difficulties of handling the casein after coagulation.
In other processes, the proteins are separated from the other constituents of the milk by ultra-filtration and are thus recovered in the state in which they are present in the milk, i.e. in the non-denatured state. This particular characteristic introduces significant limitations in regard to the ultra-filtration operation which is confined to low throughputs and narrow temperature ranges and involves dangers of blockage, in short it is characterised by relatively modest yields. In addition; the ultra-filtration membranes have to washed at very frequent intervals.
The process according to the present invention seeks to overcome these difficulties whilst, at the same time, affording considerable and unexpected advantages. In the process according to the present invention, the milk is subjected to a heat treatment enabling the proteins present therein to be partially denatured, the proteins are separated from the other nonfat contituents of the milk by ultra-filtration, said proteins ending up in the retentate fraction, after which the retentate is subjected to a complementary heat treatment for denaturing the proteins.
The present invention therefore relates to a process for separating one or more proteins from milk, which comprises subjecting the milk to a heat treatment in order to partially denature the proteins present therein, separating the proteins from the other non-fat constituents of the milk by ultra-filtration, the proteins ending up in the retentate fraction, and subsequently subjecting the retentate fraction to a complementary heat treatment in order to denature the proteins.
In other words, the process according to the present invention is characterised by a sequence of three operations, namely: - a heat treatment of the skimmed or whole milk, if desired thermally preconcentrated by ultrafiltration or by hyper-filtration, the milk used optionally being a reconstituted milk, - ultra-filtration ofthe milkthustreated, - a heat treatment of the retentate obtained.
In order to simplify the rest of the description and with regard to the thermal effect on the proteins, these three operations will be respectively termed "pre-denaturing", "ultra-filtration" and "post-denaturing".
All the percentages quoted herein are used on a weight basis unlss otherwise indicated.
The milk which is treated may be, for example, a skimmed milk, or a whole milk, and it may be concentrated thermally or by ultra-filtration or by hyper-filtration.
In one embodiment of the process according to the present invention, the proteins are separated from the other non-fat constituents of the milk by ultra-filtration with dilution, for example with water, acidified water or whey, the volume of the retentate fraction preferably being kept constant.
The pre-denaturing of the proteins by the effect of heat may be obtained in various ways, for example over a period of from 5 seconds to 2 minutes at an elevated temperature, i.e. at a temperature of from 100 to 180"C, or over a period of from 10 seconds to 50 minutes at a lower temperature in the range of from 85 to 100"C, the denaturing levels varying from 20 to 60%.
It has been found that the effect of pre-denaturing is to precipitate the heat-sensitive proteins and to fix them to the micelles of casein, which considerably reduces their sensitivity to the subsequent technological treatments, for example drying, and safeguards their nutritional quality (inhibition of the Maillard reaction).
As already known, the ultra-filtration operation may be carried out in a closed circuit, with a buffer tank in which the retentate is recycled. It may also be carried out by means of several ultra-filtration membranes or modules arranged in series. The protein content of the milk gradually increases to a content of, for example, from 10 to 13% and, if desired, to a content of 25% which may be reached without major difficulties. The content of the other constituents of the milk remains unchanged, which means that the relative proportion of proteins has been greatly increased. If is is desired to recover proteins whose residual lactose and mineral salts content is reduced in terms of absolute value, the retentate is diluted during ultra-filtration.
This technique of ultra-filtration with simultaneous dilution is sometimes referred to as "diafiltration". The diluent, generally water, acidified water or whey, is added in the buffer tank or between two successive ultra-filtration modules.
The temperature at which ultra-filtration is carried out may be freely selected and, since the proteins of the milk have already been heat-treated, they are in no danger of being harmed by the effects of heat. In order to obtain high ultra-filtration rates (high permeation levels) and for reasons of bacteriological safety, ultra-filtration is advantageously carried out at a temperature in the range of from 50 to 90"C.
The post-denaturing of the proteins by heat applied to the retentate may be carried out in the same way as pre-denaturing, for example over a period of from 5 seconds to 20 minutes at a high temperature in the range of from 100 to 1 800C or over a period of from 10 seconds to 50 minutes at a lower temperature in the range of from 85 to 100 C.
The conditions under which the thermal pre- and post- denaturing treatments are carried out may be crossed, for example pre-denaturing at 100/180"C for 5s/2 mins. and post-denaturing at 85/100 C for 10s/50 mins. or even pre-denaturing at 851100,0 for 10 s/2 mins. and post-denaturing at 100/180"C for 5s/20 mins.
Also, it has been found that the degree of denaturation obtained by post-denaturing is higher for the same conditions because of the lower lactose content of the treated product, lactose having an anit-denaturing protective function with respect to the proteins. In additon, a low lactose content minimises the risk of the Maillard reaction.
The total degree of denaturation resulting from the combination of pre-denaturing and post-denaturing after ultra-filtration may be very high and close to the possible theoretical maximum (of the order of 95%).
The advantages of the process according to the present invention are as follows: - ease of treating whole milks which are always very difficult to ultra-filter on a industrial scale, it being possible to carry out ultra-filtration at a higher temperature and with a higher throughput; - direct recovery of all the proteins present in the milk; - better reduction of the microbial population of the proteins collected by virtue of the double pre-denaturing and post-denaturing heat treatment; - better protection of the lysine which is an essential factor of the nutritional value; - milder global treatment in comparison with a single-stage treatment, post-denaturing being more effective for the same conditions or requiring milder conditions for the same effectiveness;; - higher permeation levels (i.e. yieids) of from 80 to 400% in comparison with the permeation levels obtained when the proteins of the milk are not pre-denatured.
In one preferred embodiment of the process according to the present invention, the proteins of a whole or skimmed milk are denatured by a heat treatment for from 10 to 30 minutes at from 95 to 1000C either in a heat exchanger or by the injection of steam and storage in a tank, or for from 10 seconds to 2 minutes at from 120 to 160"C either in a heat exchanger or by the direct injection of steam with holding in a tube.
The milk thus treated is then ultra-filtered at a temperature of from 55 to 75"C. If necessary, the retentate is diluted with water during ultra-filtration or even with acidified water or whey. The retentate is then subjected to a thermal post-denaturing treatment identical with, or different from the heat treatment applied to the starting milk before ultra-filtration.
In one embodiment, the proteins are recovered in the dry state by drying the retentate fraction after heat treatment.
The proteins obtained, which may be dried, are distinguished by their high quality and by a composition cabable of varying within wide limits according to the method of denaturing and the type of ultra-filtration used. In particular, it is possible to obtain proteins whose residual lactose and salt contents are remarkably low. These proteins are thus most suitable for use in dietetics, particularly infant dietetics. Information on this subject will be given in the following Examples which illustrate the present invention and in which the percentages are expressed in terms of weight based on dry matter.
Example I A skimmed milk which has been subjected to a thermal pre-denaturing treatment for 10 s at 95 C, followed by cooling to 55"C is passed through an ABCOR ultra-filtration module equipped with HFM 180 SG membranes. Ultra-filtration is continued until a 3-fold increase in concentration is obtained. Under these conditions, the ultra-filtration throughput (treated product expressed in l/m2/h) is 50 l/m2/h with a ratio of proteins to lactose of the order of 2.
A thermal post-denaturing treatment is then applied for 60 s at 140"C. A retentate having the following composition is obtained: dry matter 14.14% total nitrogen 1.26% non-casein nitrogen 0.24% lactose 4.26% ash 1.10% calcium 0.21% It is also found that, after pre-denaturing the percentage of denatured proteins in the total protein is 25%.
The post-denaturing treatment increases this percentage to 90%.
Comparison example A skimmed milk is passed without pre-denaturing through an ABCOR module equipped with HFM 180 SG membranes at a temperature of 55 C. After 3 hours, the ultra-filtration throughput is less than 30 l/m2/h.
Example 2 A whole milk which has been subjected to a thermal pre-denaturing treatment for lOs at 11500 and cooled :o 75"C is passed through an ABCOR UF module equipped with HFM 180 SG membranes.
Ultra-filtration is continued until a 2.5-fold increase in concentration is obtained. Under these conditions, he ultra-filtration throughput is 60 l/m2/h with a ratio of proteins to lactose of 1.4 to 1.
A thermal post-denaturing treatment is then applied for 30 minutes at 95"C.
After pre-denaturing, the percentage of denatured proteins, based on the total protein, is 22%. The post-denaturing treatment increases this percentage of denatured proteins to 92%.
Comparison example Awhole milk is passed without pre-denaturing through an ABCOR module equipped with HFM 180 SG membranes at a temperature of 75"C. After 2 hours, the ultra-filtration throughput is less than 15 l/m2/h.
Example 3 A skimmed milk which has been subjected to a thermal pre-denaturing treatment for 10 s at 120"C and then cooled to 550C is passed through an ABCOR ultra-filtration module equipped with HFM 180 SG membranes.
The volume is reduced by 3fold, after which the retentate is diluted with water by introducing water in a quantity equal to the permeate eliminated.
The ultra-filtration/diafiltration throughput is 33 l/m2/h and the retentate obtained after diafiltration has a proteins/lactose ratio of 6.45 to 1.
Post-denaturing is then carried out for 10 s at 110"C which gives a denaturing level of 91%, the composition being as follows: dry matter 10.50% total nitrogen 1.27% non-casein nitrogen 0.20% lactose 1.26% ash 0.78% calcium 0.81% Comparison example The procedure is as described in Example 3, but without the pre-denaturing treatment. An ultra-filtration/ diafiltration throughput of only 19 l/m2/h is obtained.
Example 4 The procedure is as described in Example 3, except that the retentate is diluted (diafiltered) with water acidified with lactic acid, its pH value being kept constant at 6.00. The retentate obtained is then heat-treated for 10 s at 95"C.
The product obtained, which has the following composition: dry matter 10.60% total nitrogen 1.29% non-casein nitrogen 0.21% lactose 1.17% ash 0.65% calcium 0.12% is partially decalcified. It has a proteins/lactose ratio of 7.05 to 1 for a degree of denaturation of 90%.
Example5 The procedure is as described in Example 3, except that the retentate is diluted (diafiltered) with a mildly denatured lactoserum having a dry matter content of 6%. 2000 1 of starting milk are diafiltered with 2300 1 of lactoserum, the increase in concentration being 3-fold. After post-denaturing as described in Example 3, a retentate having a casein/lactalbumin ratio of 2 to 1 is obtained.
The proteins/lactose ratio is 1.93 to 1.
Example 6 A milk having a dry matter content of 10% is reconstituted from skimmed milk powder and water. It is denatured for 10 s at 950C. After cooling to 55"C, it is passed through an ABCOR ultra-filtration module equipped with HFM 180 SG membranes. Concentration is continued to a 3-fold reduction in volume. Under these conditions, the ultra-filtration throughput is 61 l/m2/h with a proteins/lactose ratio of 2 to 1 in the retentate.
The retentate is then post-denatured for 60 s at 1 400C, and a degree of denaturation of 93% is obtained.
Example 7 A milk is reconstituted from water and a powdered milk which has been subjected during its preparation to a denaturing treatment corresponding to the thermal pre-denaturing treatment. Ultra-filtration and post-denaturing are then continued as described in Example 6 and an end product very similar to the product obtained in that Example is obtained.
Example 8 A skimmed milk is concentrated by hyper-filtration to a dry matter content of 20%. The concentrate obtained (1000 1) is then heat-treated for 10 s at 95"C and directly diafiltered at 55with 1500 1 of water, the level being kept constant.
The proteins/lactose ratio obtained is 1.2 to 1 the ultra-filtration throughput amounting to 26 l/m2/h.
A post-denaturing treatment is then applied for 60 seconds at 140"C, giving a degree of denaturation of 91%.
Example 9 The product obtained in accordance with Example 4 is spray-dried after adjustment of its pH to 5.2 and standardisation of its fat content. The powder obtained has interesting characteristics. In particular, after reconstitution with heating, it has a stringy and fibrous texture and may advantageously replace cheese of the Mozzarella type.
Example 10 An infant dietetic product is prepared by mixing wheat flour, sucrose, vegetable oil and the product obtained in Example 1.
The pasty mixture is then dried on rolls, giving a product which has a remarkable nutritional value and which constitutes an excellent weaning cereal.
The available lysine content is high, the value determined being 4.2%, expressed as the lysine to total protein ratio.
Example 11 A whole milk which has been heat-treated for 10 s at 1150C and then cooled to 65This passed through an ultra-filtration module until a 2.5-fold reduction in volume is obtained. Another heat treatment is then applied for 10 s at 95"C.
The product obtained may be used as such in the production of cheese, particularly cheese of the soft curd type (Brie, Camembert, etc). It may also be spray-dried and the powder obtained may be added to milk during periods of low yields in order to standardise and regularise (cheese) manufacture.
The cheese yield is markedly increased through effective retention of the serum proteins.

Claims (17)

1. A process for separation of one or more proteins from milk, which comprises subjecting the milk to a heat treatment in order to partially denature the proteins present therein, separating the proteins from the other non-fat constituents of the milk by ultra-filtration, the proteins ending up in the retentate fraction, and subsequently subjecting the retentate fraction to a complementary heat treatment in order to denature the proteins.
2. A process as claimed in Claim 1, wherein the milk is a skimmed milk.
3. A process as claimed in Claim 1, wherein the milk is a whole milk.
4. A process as claimed in Claim 1, wherein the milk is a milk thermally concentrated by ultra-filtration or by hyper-filtration.
5. A process as claimed in any of claims 1 to 4, wherein the proteins are separated from the other non-fat constituents of the milk by ultra-filtration with dilution.
6. A process as claimed in Claim 5, wherein the volume of the retentate fraction is kept constant.
7. A process as claimed in Claim 5 or 6, wherein the proteins are separated from the other non-fat constituents of the milk by ultra-filtration with dilution with water, acidified water or whey.
8. A process as claimed in any of claims 1 to 7, wherein the heat treatment before ultrafiltration is carried out for from 5 seconds to 2 minutes at from 100 to 1 80 C.
9. A process as claimed in any of claims 1 to 7, wherein the heat treatment before ultra-filtration is carried out for from 10 seconds to 50 minutes at from 85 to 1 00 C.
10. A process as claimed in any of Claims 1 to 9, wherein the heat treatment after ultra-filtration is carried out for from 5 seconds to 20 minutes at from 100 to 1 80 C.
11. A process as claimed in any of Claims 1 to 9, wherein the heat treatment after ultrafiltration is carried out for from 10 seconds to 50 minutes at from 85 to 1 00 C.
12. A process as claimed in any of Claims 1 to 11, wherein ultrafiltration is carried out at a temperature of from 50 to 90 C.
13. A process as claimed in any of Claims 1 to 12, wherein the proteins are recovered in the dry state by drying the retentate fraction after heat treatment.
14. A process for separating one or more proteins from milk substantially as described with particular reference to the Examples, excluding the comparative material.
15. A milk protein when recovered by a process as claimed in any one of Claims 1 to 14.
16. An infant and/or dietectic product which comprises one or more milk proteins as claimed in Claim 15.
17. A cheese product which comprises one or more milk proteins as claimed in Claim 15.
GB7933915A 1978-10-06 1979-10-01 Recovering proteins from milk by ultra-filtration Expired GB2035330B (en)

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Application Number Priority Date Filing Date Title
CH1040078A CH634969A5 (en) 1978-10-06 1978-10-06 PROCESS FOR RECOVERING MILK PROTEINS.

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GB2035330A true GB2035330A (en) 1980-06-18
GB2035330B GB2035330B (en) 1982-11-03

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IT (1) IT1162389B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0041346A1 (en) * 1980-06-04 1981-12-09 Stauffer Chemical Company Fabricated shellfish products and production thereof
EP0043962A1 (en) * 1980-07-11 1982-01-20 Societe Des Produits Nestle S.A. Process for preparing a pasteurised powdered cheese
US4462932A (en) * 1983-06-22 1984-07-31 Purdue Research Foundation Isolation of native casein by cryodestabilization
FR2638063A1 (en) * 1988-10-24 1990-04-27 Union Laitieren Normande NEW FOOD PRODUCTS BASED ON MILK ULTRAFILTRATION RETENTATION AND PROCESS FOR THEIR PREPARATION
FR2644983A1 (en) * 1989-03-30 1990-10-05 Pierre Coquin Food products especially long-life beverages and desserts and their production
EP2166866A4 (en) * 2007-06-26 2012-03-21 Valio Ltd Process for producing well-preserving low-lactose or lactose-free milk product
WO2016118021A1 (en) * 2015-01-23 2016-07-28 Goodman Fielder New Zealand Limited Milk based compositions comprising milk derived, denatured retentate

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0041346A1 (en) * 1980-06-04 1981-12-09 Stauffer Chemical Company Fabricated shellfish products and production thereof
EP0043962A1 (en) * 1980-07-11 1982-01-20 Societe Des Produits Nestle S.A. Process for preparing a pasteurised powdered cheese
US4462932A (en) * 1983-06-22 1984-07-31 Purdue Research Foundation Isolation of native casein by cryodestabilization
FR2638063A1 (en) * 1988-10-24 1990-04-27 Union Laitieren Normande NEW FOOD PRODUCTS BASED ON MILK ULTRAFILTRATION RETENTATION AND PROCESS FOR THEIR PREPARATION
US5114729A (en) * 1988-10-24 1992-05-19 Union Laitiere Normande Method of making a new dairy-based food product from a milk ultrafiltration retentate
FR2644983A1 (en) * 1989-03-30 1990-10-05 Pierre Coquin Food products especially long-life beverages and desserts and their production
EP2166866A4 (en) * 2007-06-26 2012-03-21 Valio Ltd Process for producing well-preserving low-lactose or lactose-free milk product
US10085462B2 (en) 2007-06-26 2018-10-02 Valio Ltd. Process for preserving low-lactose or lactose-free milk product
WO2016118021A1 (en) * 2015-01-23 2016-07-28 Goodman Fielder New Zealand Limited Milk based compositions comprising milk derived, denatured retentate
GB2537314A (en) * 2015-01-23 2016-10-12 Goodman Fielder New Zealand Milk based compositions comprising milk derived, denatured retentate
CN107205412A (en) * 2015-01-23 2017-09-26 古德曼菲尔德新西兰有限公司 The milk-based composition of denaturation retentate comprising newborn source
US10750757B2 (en) 2015-01-23 2020-08-25 Goodman Fielder Pte. Ltd Milk based compositions comprising milk derived, denatured retentate
GB2537314B (en) * 2015-01-23 2021-04-21 Goodman Fielder Pte Ltd Milk based compositions comprising milk derived, denatured retentate

Also Published As

Publication number Publication date
IT7950197A0 (en) 1979-09-07
IT1162389B (en) 1987-03-25
CH634969A5 (en) 1983-03-15
GB2035330B (en) 1982-11-03

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Effective date: 19951001