WO1995017830A1 - Procede de production d'un concentre de proteines non denaturees de lactoserum - Google Patents

Procede de production d'un concentre de proteines non denaturees de lactoserum Download PDF

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Publication number
WO1995017830A1
WO1995017830A1 PCT/CA1994/000726 CA9400726W WO9517830A1 WO 1995017830 A1 WO1995017830 A1 WO 1995017830A1 CA 9400726 W CA9400726 W CA 9400726W WO 9517830 A1 WO9517830 A1 WO 9517830A1
Authority
WO
WIPO (PCT)
Prior art keywords
whey
temperature
cheese
milk
curd
Prior art date
Application number
PCT/CA1994/000726
Other languages
English (en)
Inventor
Michel Lange
Gustavo Bounous
Original Assignee
Immunotec Research Corporation Ltd.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Immunotec Research Corporation Ltd. filed Critical Immunotec Research Corporation Ltd.
Priority to AU14097/95A priority Critical patent/AU692508B2/en
Priority to CA002176946A priority patent/CA2176946C/fr
Priority to EP95905493A priority patent/EP0739168A1/fr
Priority to NZ278018A priority patent/NZ278018A/en
Priority to JP7517704A priority patent/JPH09507029A/ja
Publication of WO1995017830A1 publication Critical patent/WO1995017830A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/20—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey
    • A23J1/205—Obtaining 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
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C19/00—Cheese; Cheese preparations; Making thereof
    • A23C19/02—Making cheese curd
    • A23C19/05—Treating milk before coagulation; Separating whey from curd
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/14—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • A23C9/142—Milk 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
    • A23C9/1425—Milk 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 whey, e.g. treatment of the UF permeate
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17—Amino acids, peptides or proteins
    • A23L33/19—Dairy proteins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • This invention relates to an improved process for producing a whey protein concentrate having a serum albumin content of about 9% or more.
  • Dietary W.P.C. produced with lower levels of heat treatment improves systemic humoral immune response, increases the resistance of target cells against the effect of carcinogens including chemical carcinogens such as dimethylhydrazine, improves resistance to pneumococcal infection, and provides a sustained increase of tissue (intracellular) glutathione.
  • the object of this invention is to provide an improved process for preparing a whey protein concentrate that has adequately low bacterial levels without excessive levels of protein denaturation. It is a particular object to provide a process that will achieve a whey protein concentrate having a serum albumin of about 9% and adequate bacterial reduction. This approximately 9% level of serum albumin was found in our studies to be important for the achievement of sustained increase of tissue glutathione for the properties such as improved systemic humoral immune response described above (References 2 and 3).
  • the use of process conditions to give a high serum albumin content will also give a high content of such other Glu-Cys containing proteins.
  • Serum albumin is the most easily denatured serum protein since its denaturation is not as reversible as that of alpha-lactalbumin (4). It therefore is a further object of this invention to maintain rigorous control of temperature and other conditions to minimize denaturation of serum albumin.
  • the casein in raw milk occurs in the form of a colloidal dispersion.
  • the particles of this dispersion range from 20 to 200 nm (nanometers) in diameter and are generally referred to as casein micelles.
  • the industrial methods of separation of the casein are based on the destabilization of these proteins either by lowering the pH of milk to the isoelectric point (pH 4.6) at 20°C or by enzymatic (rennet) hydrolysis of the Kappa casein which stabilizes the micelles.
  • the first procedure is not suitable for the recovery of native whey proteins since low pH has been shown to denature Bovine serum albumin, apparently because of repulsion of acidic amino acids (Haurowitz, 1963) (11). Furthermore, if excessively high temperatures are used in this procedure, there would be a considerable increase in the denaturing effect of a low pH.
  • the second procedure is less economically feasible because the caseins recovered are less functional for dairy industry use.
  • the objective is to develop a combination of method steps which are compatible with cheese making.
  • the cheese represents roughly 10% (by weight) of milk being treated and the whey represents approximately 90%, of which 0.6 to 0.7% consists of whey proteins.
  • Moisture content was determined in duplicate by AOAC method (7).
  • Total coliforms count was determined following incubation at 37 °C for 18 h in brilliant green using the most probable number method.
  • Total bacteria count (aerobic mesophiles) was determined following incubation at 32 °C for 48 h in PCA medium. Both methods are approved by the International Dairy Federation and American Public Health Association.
  • Lactose was measured by the enzymatic method. Standardization
  • the first step is the standardization of the milk. This involves skimming the milk to a desired fat content. This procedure is used for two reasons. The first is to attain the legal percentage of fat on a dry basis of the final cheese. The second is to achieve the best yield and quality (body and texture) of cheese.
  • the usual practice has been to use a temperature in the range of 50 °C to 65 °C as this is the most efficient range for skimming to a level of 0.05% of fat.
  • the raw milk used in the examples had the following composition:
  • composition % protein 3.2 % fat 3.65 % lactose 4.7
  • the pH of the composition was 6.65.
  • standardization of milk was carried out with a cold separator (Alfa Laval, CMRPX 714-HGV) coupled with an automatic standardizer (Alfa Laval, Alfast Model 110). All standardization steps were carried out at 4°C. (Figure 1) and for all examples the fat content was adjusted to 3.58% of total milk. The fat content of 3.58% was in accordance with standardization according to the following calculation:
  • pasteurization of the milk was achieved on a heat exchanger type HTST (Alfa Laval H-10) being set at 72.6°C with a retention time of 16 sec., followed by flash cooling to 30 °C. Most countries do not allow the production of dairy products without pasteurization. Different types of pasteurization can be used:
  • the introduction of high temperature pasteurization of milk was prompted by two different objectives. The first was to obtain a near sterilization of milk following the cheese related infection diseases reported during 1988 in Europe. The second objective was to improve the yield during cheese making.
  • the preliminary step in cheese production is to reduce the temperature.
  • the temperature is accordingly immediately reduced, such as by flash cooling to a temperature of 30 °C for cheese making.
  • Another way of controlling the rate of metabolism is to reduce the fermentation temperature. A reduction of 2°C will normally be used for this purpose.
  • the fermentation period was 1.5 hour for our examples at a temperature of 30°C.
  • the pH decreased from 6.65 to 6.55.
  • the pH drop was thus 0.1 before rennet was added.
  • Rennet was added at a rate of 20 ml/ 100 liters of milk.
  • the time required for curd formation was 25 minutes.
  • the rennet used was a pure calf rennet single strength from CH. Hansens Laboratory. The quantity was 20 ml./lOO liters of milk. The temperature is maintained at 30° C. The rennet was diluted in 10 times its volume with water before adding to milk. The clotting time was 25 minutes. Cheese production - culturing the curd
  • the curd was then cut using 6 mm. cheese knives at a temperature of 30°C to provide 6 mm cubes and stirred for 15 minutes before it was cooked.
  • Cheese production - cooking In our examples the cooking period lasted 75 min and continuous agitation was used. The peak temperature of 38 °C was reached in 30 minutes (1.3°C per 5 minutes). After this cooking period agitation was maintained for 1 hour.
  • the pH of the whey after cooking was 6.5. It is highly desirable to avoid any cheese making steps that involves a temperature in excess of 40° C. In fact some cheese production such as Emmental requires a temperature of more than 50°C. Raising the temperature to this level before separation of the whey and maintaining such temperature would adversely affect the serum albumin content. Following post stirring the curd is separated from the whey.
  • the curd should be separated from the whey at this level.
  • the whey that has been collected is first pumped at 38° C in a centrifugal separator to take out excess fat (Alfa-Laval MHMRPX-214TGV) that was present during cheese production.
  • the amount of fat is reduced to a level of 0.06% in the resulting whey.
  • the Ph in our examples was at 6.48.
  • the whey is then chilled to 4°C and stored till ultrafiltration (U.F.) is carried out.
  • the temperature is then raised at 40°C for the Ultrafiltration (using Romicon cartridge with a cut off of 50,000 Dalton). If necessary it can be given a second pasteurization as shown in Figure 1 under conditions similar to the pasteurization previously described. Whev - pasteurization
  • whey was pasteurized. This heat treatment was mainly applied to control the activity of lactic acid bacteria that was previously added to milk. It also serve to control post pasteurization contamination that could occur during cheese making. Ultrafiltration
  • the retentate is submitted to diafiltration by adding water so as to reduce the lactose level (4.6%) so that the retentate from ultrafiltration contains less than 1 % of lactose.
  • the retentate following completion of ultrafiltration has a total solids of 19-20%.
  • the conditions of ultrafiltration are set forth below in Table 1.
  • TMP Transmembrane pressure
  • the temperature utilized in most other commercial methods during this procedure is 50° C. This level of temperature facilitates a higher flux through the membranes hence more retentate production per unit of time and per unit of membrane. In our method, the draw-back of less production per unit of membrane is compensated by increasing the membrane surface.
  • the objective of not exceeding 40 °C is obtained throughout the system by fine tuning the points of input and output in the system so as to avoid a heat producing unbalance between the two.
  • the temperature of the retentate is then lowered to 4°C and kept at that temperature till freeze drying is started.
  • the composition of the retentate is about 19-20% total solids.
  • a typical composition is:
  • Vitamins and flavours may, if desired, be added to the retentate after ultrafiltration.
  • the retentate may be regarded as a final product and sold in liquid form.
  • the retentate can be concentrated to provide a dry product as described below. Whey - Freeze drying
  • Concentration to produce a dry product by lyophilization is performed at temperatures under O°C for 15 to 18 hours. This does not denature the themnolabile proteins.
  • the retentate was subjected to a blast freeze at -25 °C before entering in the freeze dryer.
  • the temperature of the condenser were maintained at -50 °C during the 17 hours of the freeze drying period.
  • the microbial counts of the retentate compare favourably with standards applicable to conventional pasteurization. These standards differ in each jurisdiction. As an example, the province of Quebec, Canada, requires that total bacteria count (aerobic mesophiles (32 °C) be maintained below 50,000 (log 4.69), both in the factory and in the final product in the case of powdered milk products. Coliforms are to be below 10.
  • the province of Quebec, Canada requires that total bacteria count (aerobic mesophiles (32 °C) be maintained below 50,000 (log 4.69), both in the factory and in the final product in the case of powdered milk products. Coliforms are to be below 10.
  • the province of Quebec, Canada requires that total bacteria count (aerobic mesophiles (32 °C) be
  • Quebec has a standard of a bacteria count of 25,000 (log 4.39) and a coliform count of 5 in the factory for milk products that have not been pasteurized or fermented.
  • Table 2 illustrates the composition of whey protein concentrate powder obtained using the principles described above.
  • thermolabile proteins such as serum albumin and to avoid substantial loss of the glutamylcysteine groups in the whey proteins.
  • PROTEIN (%) 77.5 77.04 78.08 a Lactalbumin (%) 23.68 23.85 22.20 ⁇ Lactoglobulin (%) 59.90 60.37 61.40
  • the process of this invention therefore provides a practical procedure for making undenatured whey protein concentrate. Furthermore it has the advantage of using a by-product of cheese production which is otherwise considered to be a troublesome waste product, and a potential pollutant. It should solve what was until now a continuing financial problem for the dairy industry responsible for the disposal of this major water pollutant. In conclusion, it is the objective of this invention to preserve intact the conformation of the labile whey proteins in the W.P.C. This objective of leniency is obtained through several inter-dependent steps involving temperature, ions content, ultrafiltration flux and drying techniques.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Water Supply & Treatment (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Mycology (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Biochemistry (AREA)
  • Dairy Products (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)

Abstract

L'invention concerne un procédé de production d'un concentré de protéines non dénaturées de lactosérum sous la forme d'un produit dérivé de la fabrication du fromage, ayant une teneur en sérumalbumine d'environ 9 % ou plus. Ce procédé repose sur la régulation de la température, ainsi que sur d'autres paramètres.
PCT/CA1994/000726 1993-12-30 1994-12-23 Procede de production d'un concentre de proteines non denaturees de lactoserum WO1995017830A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
AU14097/95A AU692508B2 (en) 1993-12-30 1994-12-23 Process for making undenatured whey protein concentrate
CA002176946A CA2176946C (fr) 1993-12-30 1994-12-23 Procede de production d'un concentre de proteines non denaturees de lactoserum
EP95905493A EP0739168A1 (fr) 1993-12-30 1994-12-23 Procede de production d'un concentre de proteines non denaturees de lactoserum
NZ278018A NZ278018A (en) 1993-12-30 1994-12-23 Producing undenatured whey protein concentrate
JP7517704A JPH09507029A (ja) 1993-12-30 1994-12-23 未変性ホエータンパク質濃縮物の製造法

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US17563793A 1993-12-30 1993-12-30
US31590494A 1994-09-30 1994-09-30
US08/175,637 1994-09-30
US08/315,904 1994-09-30

Publications (1)

Publication Number Publication Date
WO1995017830A1 true WO1995017830A1 (fr) 1995-07-06

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Application Number Title Priority Date Filing Date
PCT/CA1994/000726 WO1995017830A1 (fr) 1993-12-30 1994-12-23 Procede de production d'un concentre de proteines non denaturees de lactoserum

Country Status (9)

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EP (1) EP0739168A1 (fr)
JP (1) JPH09507029A (fr)
AU (1) AU692508B2 (fr)
CA (1) CA2176946C (fr)
NZ (1) NZ278018A (fr)
PL (1) PL315195A1 (fr)
TW (1) TW267095B (fr)
WO (1) WO1995017830A1 (fr)
ZA (1) ZA949789B (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996035336A1 (fr) * 1995-05-09 1996-11-14 Immunotec Research Corporation Ltd. Procede permettant de produire un concentre de proteines de lactoserum non denaturees
EP1611795A1 (fr) * 2004-07-02 2006-01-04 Landfrisch Molkerei registrierte Genossenschaft mit beschränkter Haftung Méthode de fabrication de concentre de protéines de petit-lait acide et leur utilisation
ITRM20120412A1 (it) * 2012-08-13 2014-02-14 Biontologia S R L Lab Metodo per la preparazione di un concentrato di proteine sieriche.
US8815797B2 (en) 2008-03-12 2014-08-26 N.V. Nutricia High protein liquid enteral nutritional composition
US8999423B2 (en) 2007-12-05 2015-04-07 N. V. Nutricia High energy liquid enteral nutritional composition
CN111620937A (zh) * 2020-03-09 2020-09-04 烟台双塔食品股份有限公司 一种高纯度白蛋白的提取方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4701472B2 (ja) 2000-04-21 2011-06-15 雪印乳業株式会社 乳カルシウム組成物の製造方法
JP6749774B2 (ja) * 2016-03-24 2020-09-02 森永乳業株式会社 液状発酵乳の製造方法

Citations (4)

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Publication number Priority date Publication date Assignee Title
US4112123A (en) * 1976-07-21 1978-09-05 Beatrice Foods Co. Nutritionally balanced single food composition and method of production
FR2387039A1 (fr) * 1977-04-15 1978-11-10 Nestle Sa Procede de fabrication d'un concentre proteique contenant des facteurs immunologiques d'origine lactique
EP0022696A1 (fr) * 1979-06-26 1981-01-21 Institut National De La Recherche Agronomique (Inra) Produit enrichi en alpha-lactalbumine, obtention à partir de lactosérum et applications dudit produit
EP0375852A1 (fr) * 1988-12-23 1990-07-04 Immunotec Research Corporation Ltd. Composition de protéines de petit lait biologiquement active, méthode de production et utilisation de la composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4112123A (en) * 1976-07-21 1978-09-05 Beatrice Foods Co. Nutritionally balanced single food composition and method of production
FR2387039A1 (fr) * 1977-04-15 1978-11-10 Nestle Sa Procede de fabrication d'un concentre proteique contenant des facteurs immunologiques d'origine lactique
EP0022696A1 (fr) * 1979-06-26 1981-01-21 Institut National De La Recherche Agronomique (Inra) Produit enrichi en alpha-lactalbumine, obtention à partir de lactosérum et applications dudit produit
EP0375852A1 (fr) * 1988-12-23 1990-07-04 Immunotec Research Corporation Ltd. Composition de protéines de petit lait biologiquement active, méthode de production et utilisation de la composition

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
A. PIERRE, J. FAUQUANT: "PRINCIPES POUR UN PROCÉDÉ INDUSTRIEL DE FRACTIONNEMENT DES PROTÉINES DE LACTOSÉRUM", LE LAIT, vol. 66, no. 4, pages 405 - 419 *
ANON.: "MEMBRANE PROCESSING UPGRADES FOOD WASTES", ENVIRONMENTAL SCIENCE & TECHNOLOGY, vol. 5, no. 5, pages 396 - 397 *

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996035336A1 (fr) * 1995-05-09 1996-11-14 Immunotec Research Corporation Ltd. Procede permettant de produire un concentre de proteines de lactoserum non denaturees
EP1611795A1 (fr) * 2004-07-02 2006-01-04 Landfrisch Molkerei registrierte Genossenschaft mit beschränkter Haftung Méthode de fabrication de concentre de protéines de petit-lait acide et leur utilisation
US9345256B2 (en) 2007-12-05 2016-05-24 N.V. Nutricia High energy liquid enteral nutritional composition
US8999423B2 (en) 2007-12-05 2015-04-07 N. V. Nutricia High energy liquid enteral nutritional composition
EP2835059B1 (fr) 2008-03-12 2023-12-06 N.V. Nutricia Composition nutritionnelle entérale liquide riche en protéine
US9420816B2 (en) 2008-03-12 2016-08-23 N.V. Nutricia High protein liquid enteral nutritional composition
US8815797B2 (en) 2008-03-12 2014-08-26 N.V. Nutricia High protein liquid enteral nutritional composition
CN104582508A (zh) * 2012-08-13 2015-04-29 Lb里奥法姆有限公司 制备血清蛋白质浓缩物的方法
WO2014027305A1 (fr) * 2012-08-13 2014-02-20 Laboratorio Biontologia S.R.L. Procédé pour la préparation d'un concentré de protéines sériques
US9534028B2 (en) 2012-08-13 2017-01-03 Lb Lyopharm S.R.L. Method for the preparation of a serum protein concentrate
EA031775B1 (ru) * 2012-08-13 2019-02-28 ЭлБи ЛИОФАРМ Эс.Эр.Эл. Способ получения концентрата сывороточных белков
ITRM20120412A1 (it) * 2012-08-13 2014-02-14 Biontologia S R L Lab Metodo per la preparazione di un concentrato di proteine sieriche.
CN111620937A (zh) * 2020-03-09 2020-09-04 烟台双塔食品股份有限公司 一种高纯度白蛋白的提取方法
CN111748023A (zh) * 2020-03-09 2020-10-09 烟台双塔食品股份有限公司 一种环保节能提取白蛋白的方法
CN111793120A (zh) * 2020-03-09 2020-10-20 烟台双塔食品股份有限公司 一种绿色循环提取白蛋白的方法

Also Published As

Publication number Publication date
CA2176946A1 (fr) 1995-07-06
EP0739168A1 (fr) 1996-10-30
ZA949789B (en) 1995-10-25
NZ278018A (en) 1998-04-27
AU1409795A (en) 1995-07-17
CA2176946C (fr) 2006-02-07
JPH09507029A (ja) 1997-07-15
TW267095B (fr) 1996-01-01
PL315195A1 (en) 1996-10-14
AU692508B2 (en) 1998-06-11

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