WO2001041580A1 - Method of obtaining glyco-macro-peptide deplete product from whey - Google Patents

Method of obtaining glyco-macro-peptide deplete product from whey Download PDF

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Publication number
WO2001041580A1
WO2001041580A1 PCT/NZ2000/000246 NZ0000246W WO0141580A1 WO 2001041580 A1 WO2001041580 A1 WO 2001041580A1 NZ 0000246 W NZ0000246 W NZ 0000246W WO 0141580 A1 WO0141580 A1 WO 0141580A1
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WO
WIPO (PCT)
Prior art keywords
whey
stream
protein product
protein
gmp
Prior art date
Application number
PCT/NZ2000/000246
Other languages
English (en)
French (fr)
Inventor
Paul Desmond Signal
Timothy Alan Winter
Michelle Yvette Jenkins
Original Assignee
Fonterra Co-Operative Group Limited
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 Fonterra Co-Operative Group Limited filed Critical Fonterra Co-Operative Group Limited
Priority to AU19036/01A priority Critical patent/AU1903601A/en
Publication of WO2001041580A1 publication Critical patent/WO2001041580A1/en

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Classifications

    • 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
    • A23C9/146Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by ion-exchange
    • 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
    • A23C9/1425Milk 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
    • 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
    • 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

Definitions

  • This invention relates to a method of obtaining a whey product deplete of Glyco-Macro-Peptide (GMP) which is heat stable at low pH from a sweet whey, through the use of anion exchange, and products obtained from the method.
  • GMP Glyco-Macro-Peptide
  • GMP describes a set of long-chain amino acids which occur during the manufacture of cheese and of rennet casein.
  • GMP is the product of the hydrolysis of Kappa-casein by a suitable rennet enzyme. GMP therefore occurs in all cheese whey and rennet casein whey.
  • GMP contributes to acid heat stability, and that, therefore, GMP-deplete products would not be useful in low pH conditions where heat stability was required.
  • the term acid heat stable refers to a product in which the turbidity is quantified by measuring the absorbance at 61 0nm and is found to be less than 0.1 00 AU cm "1 after it has been heated at 60-80°C, pH 3.6-3.8, for 20 minutes.
  • the protein concentration in the solution for the purposes of this test is 4.8-5% .
  • the protein concentration may be equal to, or greater than that found in whey (0.8%) in which case an absorbance at 61 0nm of less than 0.030 AU cm "1 after 20 minutes at 80°C, proves acid heat stability.
  • GMP-deplete whey product refers to a sweet whey stream that has had a degree of GMP removal performed on it via anion exchange.
  • a whey protein product derived from sweet whey by ion exchange using anion medium exchange which is acid heat stable.
  • the whey protein is GMP-deplete.
  • the product may include no more than 1 5 % GMP as a proportion of the total protein.
  • the acid heat stability will be such that at pH 3.6 the application of heat will not result in any observable lack of clarity.
  • the acid heat stability may be such that the absorbance at 61 0nm at a pH of substantially 3.6 and heating to a temperature of substantially 80 °C for substantially 20 minutes, of a solution containing substantially 5 % protein, is ⁇ 0.030 AU/cm.
  • the absorbance under those conditions may be ⁇ 0.01 AU/cm.
  • a method of producing a whey protein product which is acid heat stable, from sweet whey including the steps of:
  • the method may further include ultrafiltration of the non-bound protein stream.
  • the breakthrough stream may be ultrafiltered and diafiltered with water to produce a retentate having a total solids content of 1 8-28 % total solids with a protein content of 90% or greater on a dry basis.
  • a retentate having a total solids content of 1 8-28 % total solids with a protein content of 90% or greater on a dry basis.
  • Figure 1 Chromatogram of product produced by Example 2.
  • the method of the invention begins by taking a whey or whey retentate, acidification of the whey stream to a pH in the range 4 to 6, and then subjecting the acidified whey stream to anion exchange to produce a stream deplete in GMP.
  • the feed whey material may be a cheese whey, rennet whey, cheese whey protein concentrate, rennet whey protein concentrate, cheese whey protein isolate or rennet whey protein isolate.
  • the whey stream may be subject to a process such as microfiltration to remove particulate material which may be present and may cause blocking of a packed ion exchange bed.
  • the acidified whey stream may then be applied to a packed bed column including an anion exchange resin such as SepraPrep Q, which has been previously regenerated.
  • the regeneration may be with mineral or organic acids, salt or a mixture of salts (such as sodium chloride, potassium chloride, or calcium chloride) or a mixture of acid(s) and salt(s) .
  • the breakthrough stream from the anion exchange process may be ultrafiltered and diafiitered with water to produce a retentate, which may then be spray dried.
  • packed bed ion exchange such as expanded bed systems, fluidised bed systems or stirred tank systems, may be used.
  • Radial flow columns may be employed as opposed to conventional axial flow columns.
  • salts such as sodium chloride, potassium chloride, or calcium chloride may be used instead of acid to regenerate the ion exchange bed.
  • the product may be processed and dried at pH 3.4-5.0, or it may be neutralised and dried.
  • the end product has a GMP level, less than that of the original whey stream.
  • the GMP content is less than 1 5% of the total protein content, and it may be below 2% of the total protein content.
  • the product is acid heat stable.
  • rennet whey protein concentrate retentate 1 7% total solids, 9.5% protein
  • the diluted retentate was microfiltered.
  • the microfiltered permeate was adjusted to pH 4.7 with 98% sulphuric acid.
  • Example I The process of Example I was repeated to produce the retentate of 1 8 % total solids from the breakthrough stream.
  • the retentate was pH adjusted to near pH 6.8 with a mixture of 2.5 % sodium hydroxide and 2.5 % potassium hydroxide, before being spray dried.
  • This powder was tested for its functional characteristics of solubility, and acid stability, as shown in Tables II, and III. 20g of powder were reconstituted in distilled water, made up to 400g. Whilst the solution was stirred, NaOH or HCI was added to increase or decrease the pH. Samples were withdrawn at specified pH values ( ⁇ 0.01 ), centrifuged and the volume of sediment measured. The results are shown in Table II.
  • the powder was reconstituted at 3% protein concentration, adjusted to pH 3.8 with phosphoric acid (or sodium hydroxide), heated to 80°C for 20 minutes, cooled and allowed to stand for 6 hours.
  • phosphoric acid or sodium hydroxide
  • GMP content was measured by reverse-phase HPLC (column - Pharmacia Resource RPC 1 ml flow rate 1 ml/min; injection volume 20 ⁇ ; start buffer 0.1 % trifluoroacetic acid in water; end buffer: 90% acetonitrile, 0.1 % trifluoroacetic acid in water; UV detection at 214 nm) .
  • the results are shown in Figure 1 , which identifies the individual peaks.
  • the level of GMP was 4.8% of protein.
  • Rennet whey protein concentrate retentate was diluted to 1 .9% protein and microfiltered.
  • a 50 ml bed ( 10cm bed depth) of Pharmacia Q Sepharose Big Beads was regenerated with 1 M HCI then washed with demineralised water.
  • the microfiltered whey stream was adjusted to pH 4.43 with sulphuric acid and passed through the anion exchange resin at 3m/hr. Samples of the non bound protein fraction were collected during the run and tested for GMP content and acid stability.
  • Whey material was prepared for ion exchange by microfiltering rennet whey protein concentrate diluted to 1 .9 % protein.
  • the microfiltered feed material was split into 4 batches and the batches were adjusted to pHs 5.25, 5.00, 4.75, and 4.55 using sulphuric acid.
  • the batches were then passed through the anion exchange resin at 3m/hr, with 1 M HCI followed by a water flush being used to regenerate the column between batches. Samples of the non bound protein fraction were collected during the run and tested for GMP content and acid stability. The lower than expected absorbance measurement for the column feed material is explained by the formation of discrete aggregates in this sample which gives fluctuating absorbance measurements.
  • Rennet whey protein concentrate was diluted to 1 .9% protein and microfiltered to prepare it for ion exchange.
  • a 50L ion exchange column ( 1 0cm bed height) was packed with Sepraprep Q anion exchange resin and regenerated with 1 M HCI then washed with demineralised water.
  • the microfiltered whey was adjusted to pH 5.25 with sulphuric acid and 800L was passed through the resin.
  • the resin was then regenerated again with 1 M HCI and the process repeated.
  • the non bound protein stream from both cycles was then ultrafiltered and diafiitered at pH 3.6 using 5kD ultrafiltration membranes (Koch HFK328s). A retentate of 1 6.5 % total solids ( 90% protein on a dry basis) was produced.
  • the acid heat stability of the GMP-deplete product of the invention may be compared to that of a whey protein product produced by cation exchange, having a GMP level in the range 5 % of total protein, which failed to have the functional characteristic of clarity and stability in acid and heat-acid conditions. It may also be compared with an acid whey product produced by microfiltration, including 1 5-20% GMP, which was also not acid heat stable.
  • the acid heat stable whey protein product of the invention produced by anion exchange has functional properties and characteristics which distinguish it from other whey proteins produced from sweet whey, such as by cation exchange methods, particularly with regard to acid heat stability.
  • the whey protein product of the invention has excellent acid heat stability and is ideally suited for protein fortification of low pH beverages (such as substantially pH 3.2-4.0) such as those marketed for sports nutrition and refreshment.
  • the acid heat stable product may also have application for other liquid, solid or semi-solid nutritional or dietary products, such as yoghurts.

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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)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Peptides Or Proteins (AREA)
PCT/NZ2000/000246 1999-12-08 2000-12-08 Method of obtaining glyco-macro-peptide deplete product from whey WO2001041580A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU19036/01A AU1903601A (en) 1999-12-08 2000-12-08 Method of obtaining glyco-macro-peptide deplete product from whey

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NZ50165599 1999-12-08
NZ501655 1999-12-08

Publications (1)

Publication Number Publication Date
WO2001041580A1 true WO2001041580A1 (en) 2001-06-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/NZ2000/000246 WO2001041580A1 (en) 1999-12-08 2000-12-08 Method of obtaining glyco-macro-peptide deplete product from whey

Country Status (4)

Country Link
AR (1) AR026771A1 (es)
AU (1) AU1903601A (es)
UY (1) UY26478A1 (es)
WO (1) WO2001041580A1 (es)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002028194A1 (en) * 2000-10-05 2002-04-11 New Zealand Dairy Board Process for recovering proteins from whey protein containing feedstocks
EP1204328A1 (en) * 1999-07-29 2002-05-15 New Zealand Co-Operative Dairy Company Limited Reduced fat whey protein concentrate and method of manufacture
US9055752B2 (en) 2008-11-06 2015-06-16 Intercontinental Great Brands Llc Shelf-stable concentrated dairy liquids and methods of forming thereof
US20150250222A1 (en) * 2003-06-23 2015-09-10 Nestec S.A. Infant or follow-on formula
WO2016128254A1 (en) * 2015-02-09 2016-08-18 Nestec S.A. Process for treating a sweet whey material containing cgmp and related method for producing a protein material having a targeted tryptophan/threonine ratio
WO2016128251A1 (en) * 2015-02-09 2016-08-18 Nestec S.A. Process for treating sweet whey such as to obtain a protein material suitable for hypoallergenic infant formulae
AU2014363470B2 (en) * 2013-12-13 2018-09-06 Société des Produits Nestlé S.A. Use of a modified sweet whey and a modified sweet whey containing infant formula for promoting the postnatal development of the infant central nervous system and related cognitive functions
US11490629B2 (en) 2010-09-08 2022-11-08 Koninklijke Douwe Egberts B.V. High solids concentrated dairy liquids

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995019714A1 (en) * 1994-01-21 1995-07-27 Valio Oy Process for fractionating whey proteins and the components so obtained
WO1997026797A1 (en) * 1996-01-26 1997-07-31 John Stephen Ayers Method of separating and recovering proteins from a protein solution
WO1999018808A1 (en) * 1997-10-09 1999-04-22 Wisconsin Alumni Research Foundation Production of kappa-casein macropeptide
US5968586A (en) * 1997-10-09 1999-10-19 Wisconsin Alumni Research Foundation Production of κ-casein macropeptide for nutraceutical uses

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995019714A1 (en) * 1994-01-21 1995-07-27 Valio Oy Process for fractionating whey proteins and the components so obtained
WO1997026797A1 (en) * 1996-01-26 1997-07-31 John Stephen Ayers Method of separating and recovering proteins from a protein solution
WO1999018808A1 (en) * 1997-10-09 1999-04-22 Wisconsin Alumni Research Foundation Production of kappa-casein macropeptide
US5968586A (en) * 1997-10-09 1999-10-19 Wisconsin Alumni Research Foundation Production of κ-casein macropeptide for nutraceutical uses
US6168823B1 (en) * 1997-10-09 2001-01-02 Wisconsin Alumni Research Foundation Production of substantially pure kappa casein macropeptide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XU ET AL., PROCESS BIOCHEMISTRY, vol. 36, 2000, pages 393 - 399 *

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1204328A1 (en) * 1999-07-29 2002-05-15 New Zealand Co-Operative Dairy Company Limited Reduced fat whey protein concentrate and method of manufacture
EP1204328A4 (en) * 1999-07-29 2003-03-12 New Zealand Co Operative Dairy REDUCED WHEY PROTEIN CONCENTRATE AND METHOD FOR PRODUCTION
WO2002028194A1 (en) * 2000-10-05 2002-04-11 New Zealand Dairy Board Process for recovering proteins from whey protein containing feedstocks
US20150250222A1 (en) * 2003-06-23 2015-09-10 Nestec S.A. Infant or follow-on formula
US9055752B2 (en) 2008-11-06 2015-06-16 Intercontinental Great Brands Llc Shelf-stable concentrated dairy liquids and methods of forming thereof
US11490629B2 (en) 2010-09-08 2022-11-08 Koninklijke Douwe Egberts B.V. High solids concentrated dairy liquids
US10517918B2 (en) 2013-12-13 2019-12-31 Societe Des Produits Nestle S.A. Use of a modified sweet whey and a modified sweet whey containing infant formula for promoting the postnatal development of the infant central nervous system and related cognitive functions
AU2014363470B2 (en) * 2013-12-13 2018-09-06 Société des Produits Nestlé S.A. Use of a modified sweet whey and a modified sweet whey containing infant formula for promoting the postnatal development of the infant central nervous system and related cognitive functions
WO2016128251A1 (en) * 2015-02-09 2016-08-18 Nestec S.A. Process for treating sweet whey such as to obtain a protein material suitable for hypoallergenic infant formulae
US10561159B2 (en) 2015-02-09 2020-02-18 Societe Des Produits Nestle S.A. Process for treating a sweet whey material containing cGMP and related method for producing a protein material having a targeted tryptophan/threonine ratio
US10912311B2 (en) 2015-02-09 2021-02-09 Societe Des Produits Nestle S.A. Process for treating sweet whey such as to obtain a protein material suitable for hypoallergenic infant formulae
WO2016128254A1 (en) * 2015-02-09 2016-08-18 Nestec S.A. Process for treating a sweet whey material containing cgmp and related method for producing a protein material having a targeted tryptophan/threonine ratio
EP3256001B1 (en) * 2015-02-09 2023-08-09 Société des Produits Nestlé S.A. Process for treating sweet whey such as to obtain a protein material suitable for hypoallergenic infant formulae
EP4241578A3 (en) * 2015-02-09 2023-10-25 Société des Produits Nestlé S.A. Process for treating a sweet whey material containing cgmp and related method for producing a protein material having a targeted tryptophan/threonine ratio
EP4245152A3 (en) * 2015-02-09 2023-10-25 Société des Produits Nestlé S.A. Process for treating sweet whey such as to obtain a protein material suitable for hypoallergenic infant formulae

Also Published As

Publication number Publication date
AR026771A1 (es) 2003-02-26
AU1903601A (en) 2001-06-18
UY26478A1 (es) 2001-03-16

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