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WO1998000519A1 - Compositions colloidales et leur utilisation dans la clarification de liquides aqueux - Google Patents

Compositions colloidales et leur utilisation dans la clarification de liquides aqueux Download PDF

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Publication number
WO1998000519A1
WO1998000519A1 PCT/GB1997/001546 GB9701546W WO9800519A1 WO 1998000519 A1 WO1998000519 A1 WO 1998000519A1 GB 9701546 W GB9701546 W GB 9701546W WO 9800519 A1 WO9800519 A1 WO 9800519A1
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WO
WIPO (PCT)
Prior art keywords
pectin
fining
composition
apple
citrus
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.)
Ceased
Application number
PCT/GB1997/001546
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English (en)
Inventor
Barry Morson
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.)
LAPORTE BSD Ltd
Original Assignee
LAPORTE BSD 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 LAPORTE BSD Ltd filed Critical LAPORTE BSD Ltd
Priority to AU30406/97A priority Critical patent/AU3040697A/en
Publication of WO1998000519A1 publication Critical patent/WO1998000519A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0408—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of inorganic added material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof

Definitions

  • Colloidal compositions and their use in the clarification of aqueous liquids Colloidal compositions and their use in the clarification of aqueous liquids.
  • This invention relates to colloidal compositions and to the use of the compositions in the clarification of aqueous liquids.
  • the use of the compositions for the fining of beverages produced by fermentation, such as ales, beers, lagers or wines or low alcohol or alcohol-freed derivatives of these is within the ambit of the present invention although the invention is not limited to this.
  • the term "fining" is used to indicate the removal of haze from a liquid such as, for example, the beverages mentioned above, by the addition of a suitable treatment agent to produce a product of acceptable clarity for consumption.
  • fermented beverages In the production of fermented beverages, after the separation of the main body of yeast, it is necessary to achieve the clarification of the remaining beverage to a high standard. While in the case of some wines acceptable clarification may occur over an extended period of t me, in the case of ales and lagers it may be necessary to achieve rapid clarification so as to achieve a short storage time and rapid delivery of the product to the consumer.
  • the clarification of fermented beverages may be conducted in clarification tanks, where the product is to be bottled or canned, or in the cask in the case of some ales which are dispensed directly.
  • the haze in fermented beverages is due to the presence of protein and tannin molecules as well as residual yeast cells and without the addition of a fining agent this haze may be slow to clear.
  • Isinglass has traditionally been used as a fining agent, possibly in conjunction with auxiliary fining agents.
  • Isinglass is derived from the swim bladders of certain species of fish and contains collagen.
  • the collagen has a positively charged structure and sediments slowly entrapping negatively charged yeast cells and proteins as it does so. This may reduce the number of yeast cells in suspension in the main body of the liquid from up to about 2xl0 ⁇ /ml to less than about lxlO-Vml.
  • the auxiliary fining agents may be silicates or polysaccharides . These materials have a negatively charged structures and help to increase the electrostatic attraction between protein molecules and the isinglass thereby encouraging the sedimentation of these molecules.
  • fining agents are preferably capable of causing repeated re-sedimentation without the need to use such a quantity of fining agent that an unduly large volume of "bottoms" forms in the cask.
  • the present invention more particularly relates to a composition of matter comprising pectin and to its use as a new or improved clarification or fining agent.
  • Pectins are polysaccharide materials having gelation properties which are found in variable amounts in the primary cell walls and intercellular tissues of land plants. They are most abundant in fruit and vegetables, especially in the rinds of citrus fruitsand apples and in beets, carrots and potatoes and in sunflower heads.
  • British Patent No 555089 describes the production of pectinic acid salts by the hydrolysis of pectin using, for example, a solution of N/15 or N/30 NaOH at 15.55°C (60°F) for 12 or 15 minutes. Further hydrolysis is inhibited by back-titration to pH 7.5 or thereabouts.
  • the effect of this hydrolysis is to de-esterify at least a proportion of the ethoxyl side groups on the pectin molecule without causing appreciable depolymerisation.
  • a solution of the pectinic acid salts so produced having a 0.5k pectin content was used as a fining agent for beer the quantity which was sufficient to achieve fining was 1.04k vol. (3 pints/barrel) for low gravity beers but 2.08% vol. (6 pts. /barrel) for all gravity beers.
  • the Applicant is unaware of any current commercialisation of such a product as a fining agent.
  • the present invention provides a composition of matter, suitable for use as a fining agent, and also a process for fining using the composition, the composition being characterised in that it comprises pectin having a molecular size range indicated by a limiting viscosity number (hereafter LVN) of less than 0.5.
  • LVN is measured according to Atkins (Physical Chemistry, 2nd. Ed., pages 825 to 827 using a U-tube viscometer.
  • the pectin has a LVN of less than 0.4, particularly preferably less than 0.3, for example no more than 0.2.
  • the pectin has a LVN of at least 0.005, for example at least 0.01.
  • Such a composition when in the form of an aqueous solution of a concentration suitable for use as a fining agent, has been found to be effective in comparison with commercially available pectins, such as apple or citrus pectins, which can have a natural LVN about 0.6 and have little or no fining activity either in their normal state or when de-esterified.
  • the present invention also provides a process for the production of a fining agent according to the invention comprising modifying pectin by depolymerising it into the LVN range stated above.
  • a fining agent comprising modifying pectin by depolymerising it into the LVN range stated above.
  • pectins for example fruit pectins such as apple or citrus pectins, or root or tuber pectins such as beet, carrot or potato pectins, or sunflower pectin, after suitable modification according to the invention, as effective fining agents.
  • the pectin may be modified according to the invention by exposure to the action of the enzyme pectinase.
  • the pectin is preferably treated with the pectinase in the form of an aqueous solution of about 1% to 10% by weight concentration of pectin.
  • the pectinase is preferably present in about 0.01% to 1* by weight.
  • the solution is preferably held at above-ambient temperature, for example at from 30°C to 60°C, for from 1 to 4 days.
  • the precise conditions, concentrations etc. are selected to achieve the required LVN, for example, very suitably, an LVN of from 0.01 to 0.2.
  • the modified pectin according to the invention is also de-esterified to a degree of esterification of less than 50%, particularly preferably less than 30%, for example, very suitably, less than 25%. There may be residual esterification of, for example, up to 10% or more.
  • De-esterification is preferably achieved by treatment with dilute alkali, for example as disclosed in British Patent No 555089 referred to above.
  • the de-esterification is conducted on the already modified pectin.
  • the susceptibility of different liquids requiring fining to the action of the fining agent according to the invention may vary.
  • effective fining action may be obtained using the fining agent, added at a concentration of from about 0.5% to 2% and/or in a quantity of from about 0.17% to 1.04% vol. (0.5 to 3 pints/barrel), or at a concentration or quantity outside those ranges, the concentration or quantity being selected to be appropriate for the particular beer or lager, or other beverage or liquid.
  • a small quantity of isinglass may additionally be used.
  • Auxiliary fining agents may also be used but are not usually necessary.
  • Tests 2 to 5, 7 to 10, 13, 14, 16 to 18 and 20 to 51 are examples according to the invention and the remaining tests are comparative tests outside the invention.
  • pectinase The effect of pectinase on the molecular size of samples of pectin was examined by adding a selected quantity of pectinase in the range 0.001% to 0.5% by weight, as the product Pectinol (Pectinol is a Trademark) , to a colloidal dispersion of pectin in water at a concentration selected in the range 0.5% to 5% by weight and maintaining the dispersion at a temperature of 20°C or 40°C for a given time.
  • % proportions of these materials are weight % unless otherwise stated.
  • the resulting dispersion of modified pectin was de-esterified by the addition of 0.5% by weight of NaOH, added as a 1 molar solution and the maintainance of the dispersion at a temperature of 20°C for 30 minutes. Unless otherwise stated the pectin used in the following tests had been de-esterified after the pectinol treatment.
  • the pectin dispersion was then examined as to its LVN, by the method referred to above, or as to its fining effect on one of a variety of beers and lagers. The fining effect was judged by the following tests.
  • the height of the sediment was expressed as a % of the total height of the liquid.
  • C Visual tests. i Visual observation of the formation of floes and their sedimentation to leave a clear supernatant liquid (yes/no) ii Visual assessment according to Institute of brewing method (A,B etc. )
  • Tests were carried out to compare the fining activity of a pectin which had depolymerised to an LVN of 0.105 with isinglass and auxiliary fining agents.
  • the tests for fining activity were visual clarity (Cii) and sediment weight (B) .
  • the quantities of fining agent are stated in % vol. as conversions from pints/barrel.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Genetics & Genomics (AREA)
  • General Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Food Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Molecular Biology (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Non-Alcoholic Beverages (AREA)

Abstract

L'invention concerne une composition appropriée pour être utilisée comme agent de clarification et comprenant de la pectine dont la plage de dimensions moléculaires indiqué par un indice de viscosité limite est inférieur à 0,5 et compris de préférence entre 0,005 et 0,2. Cette pectine peut être dérivée de la pomme, des citrus, de la betterave, de la carotte, de la pomme de terre ou du tournesol et transformée sous la forme requise, par modification à l'aide d'une pectase, dans des conditions appropriées pour que l'indice de viscosité limite requis soit atteint. Cette composition est notamment appropriée pour clarifier les bières hautes ou les bières basses.
PCT/GB1997/001546 1996-06-29 1997-06-06 Compositions colloidales et leur utilisation dans la clarification de liquides aqueux Ceased WO1998000519A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU30406/97A AU3040697A (en) 1996-06-29 1997-06-06 Colloidal compositions and their use in the clarification of aqueous liquids

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9613698.1 1996-06-29
GB9613698A GB2314564B (en) 1996-06-29 1996-06-29 Colloidal compositions and their use in the clarification of aqueous liquids

Publications (1)

Publication Number Publication Date
WO1998000519A1 true WO1998000519A1 (fr) 1998-01-08

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PCT/GB1997/001546 Ceased WO1998000519A1 (fr) 1996-06-29 1997-06-06 Compositions colloidales et leur utilisation dans la clarification de liquides aqueux

Country Status (4)

Country Link
AU (1) AU3040697A (fr)
GB (1) GB2314564B (fr)
WO (1) WO1998000519A1 (fr)
ZA (1) ZA975392B (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006032088A3 (fr) * 2004-09-20 2006-10-19 Carlton And United Beverages L Procedes et compositions permettant de clarifier des boissons
EP1955750A1 (fr) 2007-02-01 2008-08-13 Lallemand UK Limited Agent de clarification
AU2005287868B2 (en) * 2004-09-20 2010-10-21 Danstar Ferment Ag Methods and compositions for fining beverages
WO2014048558A3 (fr) * 2012-09-25 2014-05-30 Technische Universität Berlin Procédé de clarification
JP2020074707A (ja) * 2018-11-07 2020-05-21 三栄源エフ・エフ・アイ株式会社 濁りが抑制された発泡性飲料とその製造方法、発泡性飲料の濁り抑制方法、及び酸性飲料の濁り抑制剤
CN112831533A (zh) * 2019-11-22 2021-05-25 中国科学院大连化学物理研究所 一种具有高抗氧化能力的小分子果胶及制备方法
US11015158B2 (en) 2007-06-04 2021-05-25 Danstar Ferment Ag Methods and compositions for fining fermentable beverages

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3351343B2 (ja) * 1998-05-22 2002-11-25 不二製油株式会社 酸性蛋白食品及びその製造法
IT1303918B1 (it) * 1998-06-05 2001-03-01 Esseco S P A Metodo di chiarificazione delle bevande
GB0319503D0 (en) 2003-08-19 2003-09-17 Danisco Process
US9833006B2 (en) 2012-04-03 2017-12-05 Cp Kelco Aps Stable fermented milk products and methods
FR3049287B1 (fr) * 2016-03-25 2019-09-06 Biolaffort Procede de clarification, d'amelioration de la filtrabilite et de stabilisation d'un milieu liquide alimentaire

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2419930A (en) * 1942-02-16 1947-04-29 Fruit Growers Exchange Ca Process for clarifying liquids
FR2502908A1 (fr) * 1981-03-31 1982-10-08 Asama Kasei Kk Procede de traitement antiseptique d'aliments et de boissons et composition pour sa mise en oeuvre a base d'un produit de decomposition de la pectine
EP0552728A1 (fr) * 1992-01-20 1993-07-28 Japan Tobacco Inc. Pectinase, pectine à bas poids moléculaire, et aliment et boisson contenant la pectine à bas poids moléculaire

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2986133B2 (ja) * 1991-07-29 1999-12-06 ポーラ化成工業株式会社 ミネラル吸収促進剤

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2419930A (en) * 1942-02-16 1947-04-29 Fruit Growers Exchange Ca Process for clarifying liquids
FR2502908A1 (fr) * 1981-03-31 1982-10-08 Asama Kasei Kk Procede de traitement antiseptique d'aliments et de boissons et composition pour sa mise en oeuvre a base d'un produit de decomposition de la pectine
EP0552728A1 (fr) * 1992-01-20 1993-07-28 Japan Tobacco Inc. Pectinase, pectine à bas poids moléculaire, et aliment et boisson contenant la pectine à bas poids moléculaire

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
RÖCKEN, W.: "Studies concerning the destabilization of haze-forming material in orange lemonade by pectinesterase.", BRAUWISSENSCHAFT, vol. 32, no. 1, 1979, DE, pages 7 - 13, XP002043371 *
SHOMER, I.: "Protein self-encapsulation: a mechanism involved with colloidal flocculation in citrus fruit extracts.", JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE., vol. 42, 1988, BARKING GB, pages 55 - 66, XP002043373 *
SULC, D.: "Stability of pulpy nectars.", FLÜSSIGES OBST, vol. 45, no. 12, 1978, DE, pages 450 - 451, 454-456, 461, XP002043372 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006032088A3 (fr) * 2004-09-20 2006-10-19 Carlton And United Beverages L Procedes et compositions permettant de clarifier des boissons
AU2005287868B2 (en) * 2004-09-20 2010-10-21 Danstar Ferment Ag Methods and compositions for fining beverages
US8697169B2 (en) 2004-09-20 2014-04-15 Carlton And United Beverages Limited Methods and compositions for fining beverages
EP1955750A1 (fr) 2007-02-01 2008-08-13 Lallemand UK Limited Agent de clarification
US11015158B2 (en) 2007-06-04 2021-05-25 Danstar Ferment Ag Methods and compositions for fining fermentable beverages
WO2014048558A3 (fr) * 2012-09-25 2014-05-30 Technische Universität Berlin Procédé de clarification
US10287537B2 (en) 2012-09-25 2019-05-14 Technische Universität Berlin Clarification method
JP2020074707A (ja) * 2018-11-07 2020-05-21 三栄源エフ・エフ・アイ株式会社 濁りが抑制された発泡性飲料とその製造方法、発泡性飲料の濁り抑制方法、及び酸性飲料の濁り抑制剤
CN112831533A (zh) * 2019-11-22 2021-05-25 中国科学院大连化学物理研究所 一种具有高抗氧化能力的小分子果胶及制备方法
CN112831533B (zh) * 2019-11-22 2022-08-30 中国科学院大连化学物理研究所 一种具有高抗氧化能力的小分子果胶及制备方法

Also Published As

Publication number Publication date
ZA975392B (en) 1998-01-05
GB9613698D0 (en) 1996-08-28
AU3040697A (en) 1998-01-21
GB2314564A (en) 1998-01-07
GB2314564B (en) 2000-09-27

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