EP0346426A1 - Procede de separation des elements dissous et non-dissous du lait - Google Patents

Procede de separation des elements dissous et non-dissous du lait

Info

Publication number
EP0346426A1
EP0346426A1 EP89900604A EP89900604A EP0346426A1 EP 0346426 A1 EP0346426 A1 EP 0346426A1 EP 89900604 A EP89900604 A EP 89900604A EP 89900604 A EP89900604 A EP 89900604A EP 0346426 A1 EP0346426 A1 EP 0346426A1
Authority
EP
European Patent Office
Prior art keywords
membrane
milk
filtrate
peptides
ethanol
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.)
Withdrawn
Application number
EP89900604A
Other languages
German (de)
English (en)
Inventor
Kailash Kumar Dr. Prof. Gauri
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Publication of EP0346426A1 publication Critical patent/EP0346426A1/fr
Withdrawn legal-status Critical Current

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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
    • 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
    • A23C9/1422—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 milk, e.g. for separating protein and lactose; Treatment of the UF permeate
    • 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
    • A23C2210/00—Physical treatment of dairy products
    • A23C2210/20—Treatment using membranes, including sterile filtration
    • A23C2210/208—Removal of bacteria by membrane filtration; Sterile filtration of milk products

Definitions

  • the invention relates to a method for separating the dissolved and undissolved components of milk.
  • the composition of mammalian milk has been very well studied.
  • the dry weight of cow's milk is known to be on average about 12.7%, of which about 3.7% are fat components, 3.4% total protein, 4.7% lactose and about 0.7% ash.
  • the protein component consists mainly of caseins and whey proteins.
  • non-protein nitrogen (non-protein ⁇ aceous nitrogen) fraction protease peptones and minor proteins, which are mainly enzymes.
  • a separation into caseins and whey proteins is usually carried out for milk. This separation is carried out using the so-called rennet, ( ⁇ 30 to 35 C) in which one of heated milk rennet added. The fall
  • Casein out while the whey proteins remain in solution The same applies to the so-called acid precipitation of the caseins, which takes place at the isoelectric point (cow's milk pH 4.7). Caseins are heat-stable, while the whey proteins are heat-unstable.
  • the whey proteins obtained by the known processes are generally contaminated with bacteria and contain fat as well as the calcium and phosphate ions released upon separation into caseins and whey proteins.
  • the invention is therefore based on the object of providing an improved method for separating the milk into soluble and insoluble constituents with the aid of membranes.
  • the invention therefore relates to a process for separating the dissolved and undissolved components of milk, which is characterized in that a microporous membrane with a pore size in the range from 0.1 to 2 ⁇ m is pretreated with lipids and / or peptides and the Separates milk on the membrane pretreated in this way.
  • a membrane based on a fluorocarbon polymer is advantageously used.
  • a membrane made of polyvinylidene fluoride e.g. a so-called "Durapore” membrane from Millipore (e.g. the type designation GVLP or HVLP).
  • the pore size of the membrane is preferably in the range from 0.1 to 1 ⁇ m, in particular 0.1 to 0.6 ⁇ m.
  • the membrane can be pretreated with lipids or peptides alone or first with lipids and then with peptides. With the help of this pretreatment, a membrane is obtained which, in contrast to an untreated membrane, enables the milk to be separated into the dissolved and undissolved components.
  • An explanation for the effect achieved by the pretreatment cannot be given. However, it could be a polarization effect.
  • the membrane is pretreated in a simple manner by treating it with a solution, emulsion or dispersion of the lipids and / or peptides in water in the flow. It is generally sufficient to use a 0.1 to 10%, preferably 2 to 5%, lipid emulsion or a 0.01 to 10%, preferably 0.1 to 5%, solution of the peptides.
  • the pretreatment is expediently carried out at a temperature of 8 to 40 ° C., in particular 15 to 35 ° C.
  • the duration of the pretreatment depends on the lipid or peptide used in each case and on the concentration of the emulsion or solution with which the membrane is treated in the flow. In general, a pretreatment of 1 to 8 hours, in particular 2 to 5 hours, is sufficient to obtain a membrane which allows the milk to be separated.
  • Pretreatment with lipids alone leads to the desired effect, especially with membranes with small pore sizes (e.g. 0.1 to 0.4 ⁇ m). If membranes of larger pore size are pretreated with lipids, the milk components cannot be completely separated. In order to achieve complete separation in such a case, it is sufficient to treat the membrane with peptides after the pretreatment with lipids.
  • This stepwise pretreatment has the advantage that the effect achieved is reversible and that the time for the pretreatment (in particular for the treatment with peptides in the second step) is reduced.
  • Unsaturated vegetable oils are preferably used as lipids. Suitable examples are rapeseed oil, sunflower oil, coconut oil, peanut oil, olive oil, corn oil and linseed oil.
  • the peptides or peptide mixtures used according to the invention are generally short-chain peptides with a molecular weight of up to about 10,000, preferably up to about 5,000 and particularly preferably up to about 2,000.
  • the following peptides are preferred according to the invention:
  • Whey proteins Whey proteins, plant proteins (in particular banana proteins), animal proteins (from fish, eggs, meat) or bacterial proteins (in particular yeast proteins) are included, including enzymatically treated (for example with liposes such as pancreatin and proteases such as p-peptide protease) ) Raw milk per se,
  • Peptide fractions which can be isolated from raw milk and the particularly preferred peptide fractions with the arbitrary names A, B and C are obtainable, for example, by:
  • Untreated raw milk is subjected to membrane filtration on a 0.1 to 0.6 ⁇ membrane;
  • the filtrate obtained is subjected to a third membrane filtration on a membrane with a separation limit of 1000 MG; - The filtrate obtained is subjected to reverse osmosis on an open or closed membrane;
  • the filtrate obtained is concentrated to about 20% of the volume used in the reverse osmosis, left to stand in the cold and filtered off from the solid matter which has precipitated out;
  • the filtrate obtained is further concentrated, adjusted to an ethanol content of about 80% with absolute ethanol and filtered;
  • Substance 3 is characterized by:
  • FIG. 1 schematically reproduces the production process.
  • Said raw milk is subjected to a first membrane filtration on a microporous membrane with a pore size in the range from 0.1 to 0.6 ⁇ m, preferably 0.2 ⁇ m. It is advantageous to use a membrane filter arrangement that enables filtration in the tangential flow.
  • ⁇ such as for example, has proven to be a polyvinylidene fluoride membrane, a GVLP or HVLP Durapore membrane from Millipore.
  • the permeate contains all salts, milk sugar, amino acids, oligopeptides and low molecular weight polypeptides in a genuinely undenatured form. In the retained all the casein and fat ⁇ are virtually ingredients of milk included.
  • the dry matter of the filtrate (permeate) is about 6% and the nitrogen content of the dry matter is about 1.2%.
  • the filtrate from the first membrane filtration is subjected to a second membrane filtration on a membrane with a separation limit of 8-10,000 MG.
  • the so-called whey proteins essentially remain in the retentate.
  • the filtrate which essentially contains NPN compounds, lactose, short fatty acids and some salts, is fed to a third membrane filtration on a membrane with a separation limit of 1,000 MW.
  • the resulting retentate is described below.
  • the filtrate is fed to a reverse osmosis. You can either work with a so-called closed membrane or with a so-called open membrane.
  • a Millipore type Mr-3-NF-40 HF membrane can be used as the open membrane, for example. When using an open membrane, the desired product A is mainly in the filtrate. 10
  • Product A is ninhydrin-positive and has good solubility in chloroform, isopropanol and ethanol. and water and shows chemical and chromatographic behaviors of short chain peptides.
  • product A is obtained from the retentate, while the permeate (filtrate) consists practically only of water, a few salts and a small amount of NPN compounds.
  • Said retentate is worked up in the same way as described above for the filtrate of reverse osmosis on an open membrane.
  • somewhat larger amounts of the above-mentioned organic solvents are required, since the retentate contains larger amounts of lactose and salts than the filtrate of the reverse osmosis on an open membrane.
  • product A is also obtained from the retentate of the reverse osmosis on a closed membrane.
  • 100 milligrams of product A are obtained from one liter of milk.
  • the product B / C is obtained from the retentate III of the third membrane filtration.
  • Retentate is extracted with about 10 times the volume of 80% ethanol.
  • the ethanolic extract solution is suctioned off or filtered off and the residue is washed again with a little 80% ethanol. Subsequently, it is extracted with approximately 10 times the amount of 25% aqueous ethanol and also briefly washed again when the extract solution is suctioned off.
  • the extract solutions obtained are each evaporated to dryness in vacuo. In both cases, a colorless solid substance is obtained, referred to here as product / C.
  • the two fractions can be combined or used separately.
  • the substance obtained from the 25% ethanol extract is * B "; the substance obtained from the 80% ethanol extract is.”
  • C * also referred to below as Rt-103-25.
  • whey or the NPN fraction of a non-heat-denatured milk can also be used.
  • whey or the NPN fraction of a non-heat-denatured milk can also be used.
  • FIG. 1 a photographic illustration of the filtrates obtained according to the example
  • FIG. 2 a chromatogram (HPLC) of a filtrate obtained according to the invention
  • Figure 3 the image of a membrane pretreated according to the invention after spraying with ninhydrin compared to the untreated membrane.
  • the filtrate contains the dissolved components, namely all salts, lactose, amino acids and other NPN components as well as oligopeptides and low molecular weight polypeptides (whey proteins). It is bacteria-free, casein-free and fat-free and also contains no calcium and phosphate ions, because in the process according to the invention the casein which binds the calcium and phosphate ions is not denatured.
  • raw milk and fresh milk means that fresh untreated raw milk and fresh milk from a pet, preferably cow's milk, are used which do not have any of the heating treatments (pasteurization, ultra-high temperature or sterilization) that are customary in dairies. has been subjected. However, it can be carried out in the usual way, e.g. by centrifugation.
  • the filtrate about 16 liters, is fed to a third membrane filtration, using a membrane with a separation limit of 1000 MG.
  • a membrane with a separation limit of 1000 MG is fed to a third membrane filtration, using a membrane with a separation limit of 1000 MG.
  • ProductBy'C is obtained from this retentate in the manner described below.
  • the filtrate is now fed to reverse osmosis.
  • Ver ⁇ application of an open membrane the filtrate is concentrated to "about 3 liters and allowed to stand in the refrigerator a few hours. It crystallize some products insbeson particular lactose aus..
  • Man filtered off from the solids the filtrate is concentrated to such an extent that an ethanol content of about 80% is formed by adding about 10 times the volume of absolute ethanol in the total mixture, the mixture is mixed vigorously, then the undissolved constituents are filtered off with suction or filtered off, the filtrate is evaporated to dryness, and the residue obtained is extracted with 90-95% ethanol (about 10 times the volume), the extract solution is filtered off or suction filtered and concentrated, the resulting residue is treated with about 10 times the amount of chloroform or about 10 times the amount of isopropanol is evaporated to give the desired product A.
  • the substance sought is in the retentate and the retentate must be worked up in the manner described above for the filtrate.
  • the retentate III of the third membrane filtration is mixed with about 5 times the amount of absolute ethanol, so that a mixture is obtained which is about 80% pure in ethanol. The whole is stirred vigorously, left to stand for a few hours, then the undissolved constituents are filtered off, and the filtrate is evaporated to dryness.
  • the residue of the extractive treatment is then subjected to an extractive aftertreatment with 25% strength aqueous ethanol (approximately 10 times the volume).
  • the precipitate is filtered or filtered from the un ⁇ dissolved constituents, the filtrate is concentrated to dryness, and receives a second fraction of product B / C
  • the two products may be combined.
  • a polyvinylidene fluoride membrane with a pore size of 0.2 ⁇ m was cleaned and rinsed with water for one hour. The membrane is not . able to filter milk clearly.
  • the membrane is then treated with a 0.1% solution of fraction A (obtained according to Example 1) for eight or fourteen hours in a flow at room temperature.
  • the membrane is then suitable for separating the dissolved and undissolved components of the milk. A clear filtrate is obtained.
  • the properties of the membrane do not change even after treatment with 0.3 N NaOH.
  • a Durapore membrane 0.2 ⁇ m is cleaned and rinsed as described in Example 2.
  • the membrane is then treated for 3.5 hours at room temperature with a 0.3% solution of Rt-103-25 (obtained according to Example 1) in the flow. After this pretreatment, the membrane is suitable for separating the dissolved and undissolved components of the milk, and a clear filtrate is obtained. Treatment of the pretreated membrane with 0.6% NaOH for one hour does not change the properties of the membrane.
  • Membrane 2 The cleaned membrane was treated for 2 hours at room temperature with a 4% emulsion of rapeseed oil in water in the flow;
  • Diaphragm 3 The purified membrane was treated for 8 hours at room temperature • with a 4% aqueous canola oil emulsion in the effluent;
  • Membrane 4 It was first treated like membrane 3 and then for 2 hours with an 8% total hydrolyzate from raw milk. These membranes were used to try to separate the dissolved and undissolved components from milk. The filtrates obtained are shown in FIG. 1. It can be seen that the membrane 1 does not allow separation, only a slight separation is possible with membrane 2, an almost complete separation is possible with membrane 3 and the membrane 4 gives a clear separation of the dissolved and undissolved components Q.
  • a 0.1 ⁇ m polyvinylidene fluoride membrane (Durapore) was treated and cleaned as described in Example 2.
  • the membrane was then treated for 8 hours with a 4% emulsion of sunflower oil in water in the flow at room temperature.
  • the membrane was then suitable for filtering milk clearly.
  • a 0.6 ⁇ m polyvinylidene fluoride membrane (Durapore) was treated with an 8% raw milk hydrolyzate at room temperature in the flow. After 8 hours the milk could be filtered clearly.
  • the filtrate obtained according to the invention contains the dissolved components of the milk, in particular the whey proteins.
  • FIG. 2 representatively shows the composition of the filtrate obtained according to the invention. The chromatogram was obtained under the following conditions:

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Biochemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Peptides Or Proteins (AREA)
  • Dairy Products (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Selon un procédé de séparation des éléments dissous et non-dissous du lait, on traite au préalable une membrane microporeuse dont les pores ont une grandeur comprise entre 0,1 et 2 mum avec une solution aqueuse, dispersion ou émulsion de lipides ou de peptides, puis on utilise cette membrane traitée au préalable pour séparer le lait.
EP89900604A 1987-12-21 1988-12-21 Procede de separation des elements dissous et non-dissous du lait Withdrawn EP0346426A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3743440 1987-12-21
DE19873743440 DE3743440A1 (de) 1987-12-21 1987-12-21 Verfahren zum trennen der geloesten und ungeloesten bestandteile von milch

Publications (1)

Publication Number Publication Date
EP0346426A1 true EP0346426A1 (fr) 1989-12-20

Family

ID=6343207

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89900604A Withdrawn EP0346426A1 (fr) 1987-12-21 1988-12-21 Procede de separation des elements dissous et non-dissous du lait

Country Status (7)

Country Link
US (1) US5028436A (fr)
EP (1) EP0346426A1 (fr)
JP (1) JPH02502517A (fr)
AU (1) AU2826189A (fr)
DE (1) DE3743440A1 (fr)
DK (1) DK407889A (fr)
WO (1) WO1989005586A1 (fr)

Families Citing this family (17)

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Publication number Priority date Publication date Assignee Title
DE3829552A1 (de) * 1988-08-31 1990-03-01 Gauri Kailash Kumar Milchbestandteile, verfahren zu ihrer herstellung und mittel, die diese bestandteile enthalten
DE3942028A1 (de) * 1989-12-20 1991-06-27 Kali Chemie Ag Verfahren zur fraktionierung von milch oder milcherzeugnissen
DE4026365A1 (de) * 1990-08-21 1992-02-27 Biotest Pharma Gmbh Sterilfiltrierte kolostralmilch
NZ240725A (en) * 1990-11-30 1994-05-26 Snow Brand Milk Products Co Ltd Preparation of milk having a high alpha-lactalbumin content by ultrafiltration or cross-flow filtration treatment of heat treated milk
WO1993012807A1 (fr) * 1991-12-26 1993-07-08 Snow Brand Milk Products Co., Ltd. Agent de consolidation des os, et aliment et boisson contenant ledit agent
DK170035B1 (da) * 1992-05-04 1995-05-08 Md Foods Amba Fremgangsmåde til regulering af mælketørstofbestanddele i koncentrerede mælkeprodukter i forbindelse med ultrafiltrering
US5256437A (en) * 1992-06-19 1993-10-26 Pall Corporation Product and process of making sterile milk through dynamic microfiltration
CA2095057C (fr) * 1992-06-19 1998-06-16 Peter John Degen Production de lait sterile par microfiltration dynamique
WO1994009888A1 (fr) * 1992-10-30 1994-05-11 The Dow Chemical Company Procede de microfiltration a ecoulement transversal
US5356651A (en) * 1992-12-30 1994-10-18 Pall Corporation Manufacturing method for producing sterile milk using dynamic microfiltration
US5431941A (en) * 1994-06-02 1995-07-11 Pall Corporation Method of reducing the butterfat content of a milk product
US6268487B1 (en) * 1996-05-13 2001-07-31 Genzyme Transgenics Corporation Purification of biologically active peptides from milk
US6326044B1 (en) * 1997-06-19 2001-12-04 Tetra Laval Holdings & Finance S.A. Filter apparatus and method for the production of sterile skimmed milk
FR2776208B1 (fr) 1998-03-20 2000-06-16 Agronomique Inst Nat Rech Produits, en particulier laitiers, comprenant des fractions selectionnees de globules gras, obtention et applications
FI110752B (fi) 1999-05-25 2003-03-31 Novatreat Oy Menetelmä ternimaidon käsittelemiseksi
US8133524B1 (en) * 2010-12-10 2012-03-13 Tokitae Llc Food composition for hemophagous insects
MY179671A (en) * 2014-07-21 2020-11-11 Xyleco Inc Processing biomass

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Also Published As

Publication number Publication date
US5028436A (en) 1991-07-02
DK407889D0 (da) 1989-08-18
WO1989005586A1 (fr) 1989-06-29
DK407889A (da) 1989-08-18
DE3743440A1 (de) 1989-06-29
JPH02502517A (ja) 1990-08-16
AU2826189A (en) 1989-07-19

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