WO2005122785A1 - Concentration of beta-glucans - Google Patents

Concentration of beta-glucans Download PDF

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Publication number
WO2005122785A1
WO2005122785A1 PCT/SE2005/000883 SE2005000883W WO2005122785A1 WO 2005122785 A1 WO2005122785 A1 WO 2005122785A1 SE 2005000883 W SE2005000883 W SE 2005000883W WO 2005122785 A1 WO2005122785 A1 WO 2005122785A1
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WIPO (PCT)
Prior art keywords
beta glucan
process according
containing product
water
molecular weight
Prior art date
Application number
PCT/SE2005/000883
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English (en)
French (fr)
Inventor
Sten Kvist
John Mark Lawther
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Biovelop International B.V.
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.)
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Publication date
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Publication of WO2005122785A1 publication Critical patent/WO2005122785A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L7/00Cereal-derived products; Malt products; Preparation or treatment thereof
    • A23L7/10Cereal-derived products
    • A23L7/104Fermentation of farinaceous cereal or cereal material; Addition of enzymes or microorganisms
    • A23L7/107Addition or treatment with enzymes not combined with fermentation with microorganisms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

Definitions

  • the present invention relates to a process which segregates the beta glucan rich soluble dietary fiber from an aqueous syrup layer increasing the low beta glucan content in the liquor prior to drying, thereby providing a concentrated beta-glucan product.
  • beta glucan component of these cereals has been related and directly linked to a number of beneficial effects, for example the demonstrated reduction of serum cholesterol levels, alongside improvements in HDL/LDL ratios in blood, an effect strongly correlated with improved cardiovascular health in humans [Bell et al, Critical Reviews in Food Science and Nutrition, Vol 39, 2, 1999].
  • highly viscous (and usually high molecular weight) non-starch polysaccharides present in whole cereal grains may be implicated in mechanisms regulating blood glucose, with an implied beneficial effect in long term prevention of type 2 diabetes [Foster-Powell and Brand Miller, Am 3. din.
  • soluble dietary fibers present in oat and barley are not digested in the human intestine and therefore pass through to the colon where they are available for microbial fermentation and as such are effective prebiotic materials.
  • the soluble beta glucans from oat and barley are very interesting as functional ingredients in foods as they exhibit gelling behavior, stabilizing properties, water binding and impart good mouth feel to products.
  • High molecular weight beta glucans have potential as viscosity modifiers, colloidal stabilizers, texturisers etc in foodstuffs.
  • Inglett in two patent applications (US 4,996,063 and WO 92/10106) describes methods to produce water-soluble dietary fiber compositions from milled, heat-treated oat flours and milled barley flours, via treatment with alpha amylase enzymes to degrade starch components and subsequent centrifugation to remove insoluble materials from the hydrolysate mixture.
  • the products are relatively low in soluble dietary fiber content, with no reference to the molecular weight of the beta glucan components. Only one enzyme type is utilized in the processes described. There is no description of a method to further enrich the beta glucan content of the material, or the separation of a distinct layer rich in high molecular weight beta glucan.
  • Lennart et al. (US 5,686,123) inform on methods to produce soluble cereal suspensions from oat.
  • the basis of the invention is treatment of previously heat-treated ground oat, with beta amylase class of enzyme, whilst slurried in water.
  • a second alpha amylase stage may be optionally included to further breakdown starch.
  • No separation of a soluble dietary fiber rich component is described in the invention.
  • the product slurry contains most of the protein and oil present in the raw material.
  • Triantafyllon in WO 00/24270 describes a method to produce beta glucan soluble dietary fiber from heat-treated oat flour, using beta amylase enzyme to hydrolyze starch to lower molecular weight fragments, optionally including alpha amylase and/or protease in a second stage hydrolysis, after which solids are centrifuged off, leaving a soluble phase containing around 2% beta glucan.
  • beta amylase enzyme to hydrolyze starch to lower molecular weight fragments, optionally including alpha amylase and/or protease in a second stage hydrolysis, after which solids are centrifuged off, leaving a soluble phase containing around 2% beta glucan.
  • compositions containing high concentrations of soluble dietary fibers from oat and barley grain are based not on enzymatic extraction, but rather on alkaline extraction either from milled whole grain or a sieved fraction (Fisher et al, US 6,323,338), or even hot water extraction, which yields lower molecular weight soluble beta glucans (Roxdale Foods Ltd and Morgan; WO02/02645 A1 ).
  • the present invention relates to an improvement to a known process for preparing a water- soluble dietary composition.
  • the invention relates to a process for preparing a beta glucan containing product, wherein a low concentrated beta glucan containing product is made subject to a concentration process to raise the content of beta glucan from about 10 % beta glucan on a dry matter basis to at least 30 % of beta glucan on a dry matter basis, wherein the concentration process comprises the steps of;
  • the aqueous low concentrated beta glucan containing product subjected to a concentration process has an average molecular weight of at least 800,000 Daltons, more preferably at least 2 million Daltons and most preferably 3 million Daltons.
  • the aqueous low concentrated beta glucan containing product is deep frozen for at least 24 hrs.
  • the aqueous low concentrated beta glucan containing product is thawed to between 1°C and 8°C, more preferably between 1°C and 4°C.
  • the non-beta glucan containing matter is separated by centrifugation or by decantation.
  • non-beta glucan containing matter are low molecular weight dextrins.
  • the enriched beta glucan containing fraction is made subject to a precipitation in a water-soluble/water-miscible solvent.
  • the solvent comprises 1 to 4 carbon atoms.
  • the solvent is a water-soluble/water-miscible alkanol.
  • the alkanol is present in a mixture with water. In one embodiment the alkanol is present in a 50/50 (v/v) mixture with water.
  • the solvent is ethanol.
  • the precipitated enriched beta glucan containing product is collected by centrifugation.
  • the beta glucan containing product is a glucose rich, enzymatically hydrolyzed cereal grain preparation.
  • the beta glucan content in the final product is more than 30 %, more preferably greater than 40 %, most preferably greater than ⁇ O %.
  • the molecular weight of the beta glucan component in the final product is greater than 800 000 Daltons, more preferably greater than 2 million Daltons and most preferably is greater than 3 million Daltons.
  • the invention relates to a process for preparing a beta glucan containing product, wherein a low concentrated beta glucan containing product is made subject to a concentration process to raise the content of high molecular weight (at least 800,000 Daltons) beta glucan from about 10 % beta glucan on a dry matter basis to at least 30 %, preferably more than 40%, most preferably more than 50%, of beta glucan on a dry matter basis.
  • the process of upgrading the aqueous fraction of soluble dietary fiber cannot be performed on syrup which contains only, or a substantial proportion of, low molecular weight beta glucans, as dextrins resulting from the enzyme hydrolysis of the starch as described below.
  • a beta glucan material with an average molecular weight of at least 800,000 Daltons must be present in the fraction water-soluble dietary composition.
  • Water-soluble dietary fiber compositions such as beta glucans can be recovered from milled products of oats such as oat bran and oat flour after enzymatic hydrolysis of these substrates with ⁇ -amylases.
  • the resulting soluble dietary fiber which is colorless and devoid of undesirable flavors, is therefore suitable for use in a variety of foods.
  • the oat and barley aqueous syrup layers containing high molecular weight beta glucans are prepared by treating an aqueous dispersion of gelatinized, milled, oat or barley substrate with an alpha- amylase under conditions which will hydrolyze the substrate and yield a soluble and an insoluble fraction which can be separated by centrifugation giving a water-soluble dietary composition essentially free of water-insoluble substances.
  • the water-soluble dietary composition containing the beta glucan product is subsequently deep frozen for at least 12 hrs, thawed to between 1°C and 8°C, preferably between 1 °C and 4°C, to separate off non-beta glucan containing matter, mainly dextrins, and isolating an enriched beta glucan fraction.
  • the Lower molecular weight dextrins precipitate and are separated by centrifugation.
  • the top layer after centrifugation is hence enriched in high molecular weight beta glucan.
  • This beta glucan enriched fraction is then made subject to a precipitation in a water-soluble/water-miscible solvent.
  • Such water-soluble/water-miscible solvents are alkanols (alcohols) and ketones, such as acetone and butanone.
  • alkanols alcohols
  • ketones such as acetone and butanone.
  • Inglett (US 4,996,063 and WO 92/10106) was followed using, however, a bran prepared from dehulled oat grain that was not heat treated, containing 8% beta glucan, as the raw material.
  • the procedure was as follows: 1) 2 litres of water were heated to 95°C and 500g of bran was added to this with stirring. The mixture was heated to 135°C and then held at this temperature for 5 minutes, after which the temperature was reduced back to 95°C 2) 0.22 ml of amylase enzyme preparation (Termomyl Classic, obtained from Novozymes, Denmark) was then added to the mixture and incubation was performed for 20 minutes, with stirring, at 95°C, pH 6.3.
  • the temperature of the mix was raised to 135°C for 5 minutes to de-activate the enzyme, prior to final cooling to 40°C. 3)
  • a further 600 mis of water was added to the resulting slurry and the mixture was allowed to settle and decanted into a heavier fraction containing insoluble bran fibers and much of the protein and oil present in the starting material, and a lighter fraction containing starch breakdown products such as dextrins, maltodextrins alongside beta glucan and some further more soluble protein.
  • the lighter fraction was then further centrifugally separated into a protein rich fraction and an aqueous fraction rich in starch derived dextrins and maltodextrins and beta glucan.
  • the yields before drying of the fractions were: 601 g of the fiber /protein-oil mix, 1700 mis of the decanted liquid phase. This was then centrifugally split into 1000 mis of the beta glucan containing syrup, the remainder being the protein rich material.
  • the beta glucan rich fraction was found to contain 12.1 % beta glucan, on a dry matter basis.
  • the beta glucan component in this sample had a mean molecular weight of over 3 million Daltons as determined using a gel permeation chromatography, GPC, method.
  • the beta glucan content of the separated fraction was then increased in a two step procedure treating the liquor prior to drying: A. Freezing the separated liquor for for 24 hours and then allowing it to thaw. This facilitates the separation of dextrin rich heavy phase containing precipitated dextrins, from a layer rich in beta glucan.
  • the beta glucan rich layer is separated by decantation and a representative portion was freeze dried and found to have a beta glucan content of 20.2 %.
  • the molecular weight of the beta glucan component was found to be unaltered at greater than 3 million Daltons, as determined by GPC analysis. B.
  • the liquor produced after stage A was split into two equal parts and precipitated into an equal volume of ethanol, or into an equal volume of a mixture of 50% ethanol, 50% water.
  • the precipitates were isolated by centrifugation, freeze dried and were found to be enriched in high molecular weight beta glucan.
  • the material precipitated in ethanol had a beta glucan content of 37.6 % on a dry matter basis.
  • the material precipitated into 50% ethanol/50% water was found to have a beta glucan content of 58.5 % on a dry matter basis. In both cases, the molecular weight of the beta glucan component remained greater than 3 million Daltons, as determined by GPC analysis.
  • a second trial was performed using prepared oat bran supplied by Skane M ⁇ llorna (SMC45) as the raw material.
  • This sample is also prepared by milling de-hulled oat grain, except that the grain was heat treated prior to milling.
  • the method was as follows: 1) 2 liters of water were heated to 95°C and 475 g of bran was added to this with stirring. The mixture was heated to 135°C and then held at this temperature for 5 minutes, after which the temperature was reduced back to 95°C 2) 0.22 ml of amylase enzyme preparation (Termomyl Classic, obtained from Novozymes, Denmark) was then added to the mixture and incubation was performed for 20 minutes, with stirring, at 95°C, pH 6.3.
  • SMC45 Skane M ⁇ llorna
  • the temperature of the mix was raised to 135°C for 5 minutes to de-activate the enzyme, prior to final cooling to 40°C. 3)
  • a further 600 mis of water was added to the resulting slurry and the mixture was allowed to settle and decanted into a heavier fraction containing insoluble bran fibers and much of the protein and oil present in the starting material, and a lighter fraction containing starch breakdown products such as dextrins, maltodextrins alongside beta glucan and some further more soluble protein.
  • the yields before drying of the fractions were: 734 g of the fiber /protein-oil mix, 1200 mis of the decanted liquid phase.
  • the beta glucan rich fraction was found to contain 13.2 % beta glucan, on a dry matter basis.
  • the beta glucan component in this sample had a mean molecular weight of over 3 million Daltons as determined using a GPC method.
  • the beta glucan content of the separated fraction was then increased in a two step procedure treating the liquor prior to drying: A. Freezing the separated liquor for for 24 hours and then allowing it to thaw. This facilitates the separation of dextrin rich heavy phase containing precipitated dextrins, from a layer rich in beta glucan.
  • the beta glucan rich layer is separated by decantation and a representative portion was freeze dried and found to have a beta glucan content of 18.8 %.
  • the molecular weight of the beta glucan component was found to be unaltered at greater than 3 million Daltons, as determined by GPC analysis. B.
  • the liquor produced after stage A was split into two equal parts and precipitated into an equal volume of ethanol, or into an equal volume of a mixture of 50% ethanol, 50% water.
  • the precipitates were isolated by centrifugation, freeze dried and were found to be enriched in high molecular weight beta glucan.
  • the material precipitated in ethanol had a beta glucan content of 39.8 % on a dry matter basis.
  • the material precipitated into 50% ethanol/50% water was found to have a beta glucan content of 56.2 % on a dry matter basis.
  • the molecular weight of the beta glucan component was maintained at the high level of greater than 3 million Daltons.

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  • Polysaccharides And Polysaccharide Derivatives (AREA)
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PCT/SE2005/000883 2004-06-17 2005-06-13 Concentration of beta-glucans WO2005122785A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE0401567-3 2004-06-17
SE0401567A SE0401567D0 (sv) 2004-06-17 2004-06-17 Concentration of beta-glucans

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008096044A1 (en) 2007-02-08 2008-08-14 Valtion Teknillinen Tutkimuskeskus Method for fractionating oat, products thus obtained, and use thereof
WO2011061144A2 (en) 2009-11-20 2011-05-26 Basf Se The present invention relates to the use of beta-(1, 3)- beta-(1, 4) glucan with an average molecular weight of from 5.000 to 150.000 da for the increase of synthesis of collagen
US9572490B2 (en) 2011-04-28 2017-02-21 Universidad De Murcia Method and system for measuring intraocular scattering

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4960697A (en) * 1989-01-06 1990-10-02 The Standard Oil Company Recovery of polysaccharides by employing a divalent cation with a water miscible organic solvent
US5518710A (en) * 1994-01-11 1996-05-21 University Of Saskatchewan Methods for extracting cereal β-glucans
US5846590A (en) * 1993-06-04 1998-12-08 Exavena Oy Method for enriching soluble dietary fibre
US6113908A (en) * 1999-03-22 2000-09-05 Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Agriculture Methods for processing oat groats and products thereof
US6426201B1 (en) * 1996-09-25 2002-07-30 Gracelinc Limited β-glucan products and extraction processes from cereals
US20030154974A1 (en) * 2000-02-07 2003-08-21 Morgan Keith Raymond Process for extraction of beta-glucan from cereals and products obtained therefrom
US20040023923A1 (en) * 2000-07-03 2004-02-05 Morgan Keith Raymond Cold water soluble beta-glucan product and process for preparing the same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4960697A (en) * 1989-01-06 1990-10-02 The Standard Oil Company Recovery of polysaccharides by employing a divalent cation with a water miscible organic solvent
US5846590A (en) * 1993-06-04 1998-12-08 Exavena Oy Method for enriching soluble dietary fibre
US5518710A (en) * 1994-01-11 1996-05-21 University Of Saskatchewan Methods for extracting cereal β-glucans
US6426201B1 (en) * 1996-09-25 2002-07-30 Gracelinc Limited β-glucan products and extraction processes from cereals
US6113908A (en) * 1999-03-22 2000-09-05 Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Agriculture Methods for processing oat groats and products thereof
US20030154974A1 (en) * 2000-02-07 2003-08-21 Morgan Keith Raymond Process for extraction of beta-glucan from cereals and products obtained therefrom
US20040023923A1 (en) * 2000-07-03 2004-02-05 Morgan Keith Raymond Cold water soluble beta-glucan product and process for preparing the same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008096044A1 (en) 2007-02-08 2008-08-14 Valtion Teknillinen Tutkimuskeskus Method for fractionating oat, products thus obtained, and use thereof
US9433236B2 (en) 2007-02-08 2016-09-06 Valtion Teknillinen Tutkimuskeskus Method for fractionating oat, products thus obtained, and use thereof
WO2011061144A2 (en) 2009-11-20 2011-05-26 Basf Se The present invention relates to the use of beta-(1, 3)- beta-(1, 4) glucan with an average molecular weight of from 5.000 to 150.000 da for the increase of synthesis of collagen
US9572490B2 (en) 2011-04-28 2017-02-21 Universidad De Murcia Method and system for measuring intraocular scattering

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