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EP2475707A1 - Polymerisationsverfahren, im besonderen zur polymerisation von önologischen zusätzen und anhand dieses verfahrens hergestellte polymere - Google Patents

Polymerisationsverfahren, im besonderen zur polymerisation von önologischen zusätzen und anhand dieses verfahrens hergestellte polymere

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Publication number
EP2475707A1
EP2475707A1 EP09760159A EP09760159A EP2475707A1 EP 2475707 A1 EP2475707 A1 EP 2475707A1 EP 09760159 A EP09760159 A EP 09760159A EP 09760159 A EP09760159 A EP 09760159A EP 2475707 A1 EP2475707 A1 EP 2475707A1
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EP
European Patent Office
Prior art keywords
process according
polymers
polymerization
nucleus
molecules
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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.)
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EP09760159A
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English (en)
French (fr)
Inventor
Marc Bonneau
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Calone-Bonneau Marguerite
Original Assignee
Calone-Bonneau Marguerite
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Application filed by Calone-Bonneau Marguerite filed Critical Calone-Bonneau Marguerite
Publication of EP2475707A1 publication Critical patent/EP2475707A1/de
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H1/00—Macromolecular products derived from proteins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H1/00—Macromolecular products derived from proteins
    • C08H1/02—Protein-aldehyde condensates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H1/00—Macromolecular products derived from proteins
    • C08H1/02—Protein-aldehyde condensates
    • C08H1/04—Casein-aldehyde condensates
    • 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
    • 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
    • C12H1/0416—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 organic added material
    • C12H1/0424—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 organic added material with the aid of a polymer

Definitions

  • the present invention relates to a method of polymerization, including oenological auxiliaries and polymers obtained by this process, as well as the characteristics and industrial applications of new non-allergenic processing aids.
  • auxiliaries obtained by the stable chemical bond between a central particulate core, organic or mineral, and peripheral biological molecules of animal, plant or microbial origin, constitute new stable and functional polymers and copolymers in an aqueous medium.
  • These polymers and copolymers are characterized by the fact that they are functional in aqueous media and that they do not leave any contaminants residues, toxic or allergenic, in drinks where they are used as processing aids.
  • the present invention more particularly describes a process for obtaining polymerized organic macromolecules which have specific bonding, clarification and preservation activities for beverages of plant origin and their fermented derivatives, with fruit, with grape must. , still and sparkling wines, beers, vinegars, ...) and for natural beverages, flavored and dietary waters.
  • the various technical operations of sticking, clarifying, filtering and stabilizing wine are essential steps in obtaining drinks with satisfactory physical and organoleptic characteristics for the consumer.
  • Bonding is defined as "the incorporation into the wine of substances capable of flocculating by causing the particles in suspension”.
  • the bonding, clarification and preservation products currently used are:
  • albumin casein
  • gelatines fish glues ...
  • tannins Of vegetable origin: tannins, glutens, prolamines, gums ...,
  • PVPP PolyVinylPolyPyrrolidone
  • U.S. Patent No. 4,479,970 A describes a method of treating wine using a technological compound obtained by cross-linking gelatin with glutaraldehyde.
  • the gelatin may be bound to a carrier matrix.
  • GB Patent No. 2,028,340 A discloses a process for treating beer with a technological compound obtained by crosslinking gelatin or fish glue on a carrier matrix consisting of cellulose, diatomite or albumin using a ligand agent such as than glutaraldehyde.
  • a ligand agent such as than glutaraldehyde.
  • the process which is the subject of the present invention comprises several successive steps, including a final purification step intended to eliminate the toxic residues of the ligands and to ensure the perfect innocuity of the polymers obtained.
  • DE Patent No. 25 38 251 A1 describes a process for the treatment of beverages with the aid of a technological compound obtained by crosslinking gelatin or casein.
  • US Patent 4,490,399 A discloses a method of treating wine with a technological compound obtained by crosslinking gelatin on a silica matrix using a ligand agent such as glutaraldehyde, to obtain an insoluble final product.
  • the method, object of the present invention uses neither gelatin nor silica and develops formulations and composite and original techniques for the preparation of support cores and functional peripheral layers.
  • WO 01/3781 2 A discloses an insoluble pharmaceutical composition
  • polymers such as proteins, PVPP and alginate, crosslinked with a crosslinking ligand such as glutaraldehyde.
  • US Pat. No. 5,935,442 A describes the preparation of particles intended for analytical chromatography which comprise a macromolecular support nucleus of various natures (agarose, alginate, albumin, starch, cellulose, dextrans, gelatins, gum arabic, silica). , activated by a ligand agent (cyanogen bromide, divinylsulfon, epichlorohydrin, glutaraldehyde, hydrazine, periodate, tosylate).
  • a ligand agent cyanogen bromide, divinylsulfon, epichlorohydrin, glutaraldehyde, hydrazine, periodate, tosylate.
  • EP 0 648 480 A describes a macromolecular compound based on collagen, made insoluble by crosslinking the protein with carbodiimide or glutaraldehyde.
  • WO 01/68798 discloses a composition for the stabilization and clarification of wine comprising cross-linked PVPP.
  • the composite polymers are specifically developed for exclusive oenological applications. To this end, they comprise, on the surface of various carrier nuclei activated or crosslinked by various ligand agents, one or more fixed layers of functional biological molecules, developed according to various and original formulations.
  • the process according to the invention makes it possible to prepare polymers with guaranteed safety.
  • non-allergenic oenological compositions according to the invention constitute a timely technical innovation for winemaking professionals and a satisfactory solution for the current regulations relating to food safety.
  • the invention relates to a process for the preparation, in particular of oenological auxiliaries, consisting of a polymerization of natural molecules and which comprises the following steps:
  • anchoring by covalent bonds oriented on said activated nucleus of one or more peripheral layers of natural molecules, and - neutralization and removal of residues of said ligand reagents.
  • the step of preparing said macromolecular support nucleus is carried out using flocculable particles of a biological or mineral nature
  • the step of chemical activation of said support nucleus is carried out by means of ligand reagents, homo or hetero-bifunctional, comprising at least two opposite reactive groups connected by several constituent atoms,
  • step of anchoring by covalent moieties oriented on said support core activated by said ligand reagents, one or more layer (s) peripheral (s) of natural molecules is carried out so as to obtain functional molecules,
  • the step of neutralizing and eliminating the residues of said residual ligand reagents is carried out by specific washing and inerting.
  • the natural molecules that make up the peripheral layers are:
  • enzymes such as pectinases, glucanases, oxidases, catalases.
  • the nature, the density and the oriented presentation of the natural peripheral molecules condition the functional properties and the specific performances of the various polymerized technological aids according to the invention.
  • the process makes it possible to prepare and obtain, from inorganic and organic compounds authorized by the Oenological Codex, new purified, insoluble and non-allergenic technological polymers that can be used in the manufacture of beverages and their food derivatives: still wines, sparkling wines , ciders, beers, juices, sodas ....
  • a first embodiment of the polymerization process according to the invention is characterized in that the flocculable particles used in the step of preparing the macromolecular macromolecule are aggregated proteins (caseins, albumins, gelatins, gluten, ...), and in that the ligands used in the chemical activation step are selected from the group consisting of aldehydes, pyrrophenyl chloroformate, N-hydroxysuccinimide chloroformate, and the like. chloro-2-3-epoxypropane, aminobenzyloxymethyl, carboxymethyl hydrazide, aminoalkyl, or carbonyl diimidazole.
  • This embodiment of the polymerization process describes the preparation of fixed and activated macromolecular protein nuclei, on the surface of which are anchored, by oriented covalent chemical moieties, various functional protein glues, hitherto used in enology in soil form. ble, such as albumin, casein, or gelatin.
  • This first mode of the process leads to the realization of three types of homopolymers and six types of copolymers:
  • Nucleus aggregated and activated albumins
  • layer functional oriented albumin
  • Core ines album aggregated and activated
  • -layer functional oriented casein
  • Core aggregated and activated caseins
  • layer functional oriented albumin
  • the manufacture of the casein-type polymer casein functional comprises:
  • the casein polymers thus obtained are washed twice with 1 liter of a solution of glycine (C2H 5 NO 2) -NaCl buffer, pH 6.5. After sedimentation and further washing with 400 ml of buffered water - pH7.2, the casein polymers are dried under vacuum at 5 ° C. and stored as a yellow powder in airtight bags under inert atmosphere at 5 ° C.
  • the insoluble nature of the cashein-casein granular homopolymer obtained according to the invention is characterized in the following way: a sample of 2 mg of polymers is suspended in a volume of 20 ml of alcoholic water (ethanol 10% VA /) and buffered pH6, and incubated, with gentle shaking, for 24 hours at 15 ° C. After decantation, the absence of residual casein is verified on a sample of 0.1 ml of supernatant by an enzyme immunoassay based on bovine anti-casein antibodies, the specific detection threshold of which is 2 ppm. The results obtained during five successive titrations prove to be negative, thus indicating the absence of 2ppb of allergenic caseins in the solution treated with the polymer.
  • the casein-casein polymer is resuspended in cold water with stirring for 10 minutes.
  • the gluing treatment is carried out on the basis of incorporation in the wine at a rate of 50 to 100 g of polymer hydrate per 100 liters of must or white or rosé wines to be treated.
  • the wine is fined in 2 hours with intermittent and moderate stirring.
  • the adsorption of the polyphenols by the polymer thus makes it possible to lighten the colored wines, to reduce the maderised taste and to stabilize the young wines against oxidase breakage.
  • the bottling and the final filtration of the wine eliminates all the precipitates of the collage, and leads to a drink devoid of unstable tannins.
  • the copolymer is formed of a macromolecular nucleus of aggregated ovalbumin and of an anchored peripheral layer of lysozyme.
  • Lysozyme (E1 105) is an enzyme protein It has a mucamidal activity, extracted from egg yolk and used for its antibacterial activity in food production.
  • Residual traces in treated beverages are known to be lysozyme for allergic consumers of egg proteins.
  • the granular nucleus of ovalbumin is obtained by driping from the micro-pipette 100 ml of ovalbumin in 10% solution (Weight / Volume) in PBS buffer - pH 6.5 at 30 ° C. in a beaker containing 500 ml of water at 90 ° C. with stirring. In contact with water at 90 ° C, the ovalbumin micro-droplets flocculate rapidly as fine granules. After lowering the temperature to 30 ° C., the ovalbumin granules are collected by sieving.
  • the activity and the insoluble nature of the ovalbumin-lysozyme copolymer obtained is controlled as follows: a sample of 10 mg of copolymer is suspended in a volume of 100 ml of white wine containing 5 ⁇ 10 3 malolactic bacteria and is incubated with moderate shaking for 4 hours at 15 ° C. After decantation of the copolymer, the number of viable malolactic bacteria remaining on a 0.5 ml aliquot of supernatant is evaluated by culture on nutrient agar and the presence of residual lysozyme is investigated by immunoenzymatic technique with anti-lysozyme antibody. (detection threshold of 2ppb).
  • a second indicative but non-exclusive embodiment of the polymerization process is characterized in that the flocculable particles used in the preparation step of the macromolecular support core are chosen from the group comprising bentonite, kaolin, bentonite, zeolite , active charcoal, latex, or polyvinylpolypyrrolidone, and characterized in that the ligands used in the chemical activation step are chosen from the group comprising aldehydes (acetaldehyde, formaldehyde, lutaraldehyde, etc.
  • amino-alkyl aminobenzyloxymethyl, bis-sulfosuccinimidyl suberate, dimethyladipimate, carboxymethyl hydrazide, carbonyl di-imidazole, N-hydroxysuccinimide chloroformate, p-nitrophenyl chloroformate.
  • a first indicative but non-exclusive embodiment of the method according to this method describes the preparation of a multilayer copolymer of the bentonite-albumin-enzyme type.
  • the enzymes useful in wine fermentation are pectinases, beta-glucanases, glucose oxidases and fungal catalases, sold in the form of powders or soluble granules.
  • Accidental inhalation or skin contact with enzymes may cause sensitization that generates allergic reactions in operators.
  • the polymerization process is carried out as follows:
  • bentonite is a powder of alumina, with an average particle size of 100, which swells
  • the hydrated bentonite is prepared by pouring with stirring 100 g of powder in 1 liter of buffered water at pH 6.5 and at a temperature of 50 ° C. and incubated for 2 hours. The gel obtained is filtered through a 45 micron porosity clarifying plate filter. The wet gel retentate is collected and gradually incorporated in suspension, with gentle stirring, in 2 liters of a 5% (W / V) solution of ovalbumin in pH 4.5 buffer. The adsorption phase of the proteins on the granular support is carried out for two hours at 5 ° C., by intermittent stirring every 10 minutes.
  • the oval binder adsorbed on the bentonite is crosslinked by the aldehyde, with gentle stirring, for 60 minutes.
  • the crosslinked bentonite-ovalbumin compound is then filtered on a 45 ⁇ porosity plate filter. If it is washed twice to remove excess residues of aldehyde then filtered again on 45 ⁇ porosity disk.
  • anchoring the activated and washed retentate is taken up in 500 ml of a buffered solution co m po rta ntun enzymatic mixture, equal parts, pectinases (EC3.2.1 .1 5) and beta- (1 - 3; 1-6) -giucanases) at 5g / l.
  • the oriented covalent bonding of the enzymatic molecules to the activated ovalbumin molecules continues for 60 minutes with gentle agitation.
  • the bentonite-albumin-enzyme copolymer thus obtained is centrifuged (7500 rpm for 20 minutes) then resuspended and washed twice in 1 liter of glycine buffer (C2H5NO2) -NaCl-pH 6.5 to neutralize residual reactive groups of the aldehyde.
  • the copolymer is centrifuged again (7500 rpm for 20 minutes) and then dried under vacuum at -25 ° C. and it is preserved in the form of a pale yellow granular powder in hermetic bags under an inert atmosphere at 5 ° C.
  • the insoluble nature of the bentonite-ovalbumin-pectinase copolymer thus obtained is characterized in the following manner: a sample of 10 mg of copolymer is suspended in a volume of 100 ml of wine and is then incubated, with moderate stirring, for 2 hours at 1 5 ° C. After decantation, the presence of ovalbumin residues and allergenic pectinases is characterized on a sample of 10 ml of wine supernatant treated with an enzyme immunoassay technique using anti-ovalbumin and anti-pectinase antibodies, the specific detection thresholds of which are 2 ppb. The results of five successive titrations are negative and confirm the absence of 2ppb.
  • the SDS-Page-immunoblot assays demonstrate that musts and red and white wines clarified by the bentonite-ovalbumin-pectinase copolymer are devoid of ovalbumin residues and pectinases and are not allergenic to the consumer.
  • a second non-limiting example of embodiment of the method according to this second mode concerns the preparation of a multilayer bentonite-albumin-plant lectin copolymer.
  • Lectins are naturally occurring proteins or glycoproteins with one or more specific binding sites with a carbohydrate. They bind so Specific to oligosaccharides, by hydrophobic interactions and by hydrogen bridges between carbohydrate hydroxyls and amino acid NH 2, OH and carbonyl functions of the protein.
  • Concanavalin A ConA a lectin extracted from the bean genus Canavalia ensiformis, binds in particular D-mannose and D-glucose.
  • the preparation of a bentonite-albumin-Con.A copolymer, supplied as a non-limiting indication, is carried out following the steps of the method already described:
  • the copolymer obtained is resuspended in water (1 M / 10 V) and used at a dose of 100 g per 100 L of white or red grape juice.
  • the copolymer incubated for 2 hours at 10 ° C. with slow stirring, fixed sugars present in the r isin and d im in ue the final concentration after fiitration.
  • the insoluble copolymer characterized by its capacity to bind sugars, constitutes a new oenological compound according to the invention which makes it possible, according to the doses used, to reduce the sugar content of musts and fruit juices and consequently to reduce ui re the final re q ual d alcohol beverages from the alcoholic fermentation of musts previously treated with this copolymer.
  • the steps of the process according to the invention are similar and applicable to the manufacture of various copolymers with one or more peripheral layers, formed either of bentonite-proteins or of bentonite-proteins. plants of either bentonite-microbial proteins, and all objects of the invention.
  • a third nonlimiting embodiment of the method according to this second embodiment relates to the preparation and characteristics of a copolymer formed between alginates and glues of plant origin.
  • Some vegetable proteins extracted from legumes or cereals, the different tannins (gallic tannins, ellagic tannins, and condensed tannins,) prepared from various plants and mannoproteins from yeasts are authorized as glues for musts and wines ( Regulations EC 2165/2005 and EC 1493/1999).
  • a first indicative and nonlimiting variant of the preparation of an alginate-gluten copolymer is described below: an aliquot of 5 g of sodium alginate (E 401) is removed and dispersed with strong stirring in a mixer in 1 1 liter of an aqueous 5% (W / V) gluten solution at pH 7.2 and 20 ° C. A solution of 1 liter of calcium chloride at 10 g / liter is prepared in a beaker. Then, by dropwise distribution, the 5% gluten solution is added to the calcium chloride bath.
  • each drop of the alginate -gluten mixture immediately forms a gelled and coagulated minibill.
  • the beads thus formed are washed twice in succession in one liter of distilled water.
  • the beads are then immersed for 60 minutes in a 5% solution of glutaraldehyde (C5H8O2) at pH 8.5.
  • the beads are then drained on sieves and then immersed in 1 liter of a new aqueous solution of gluten at 5% (W / V) pH 7.2 for 60 minutes at 25 ° C.
  • the beads are again drained on sieves and then washed in 1 liter of glycine buffer (C2H5NO2) -NaCl pH7.
  • the beads thus treated constitute an alginate-gluten copolymer with a functional surface which is then dried under vacuum at 5 ° C. and then kept in sealed bags under an inert atmosphere at 5 ° C.
  • the safety test of the alginate-gluten copolymer obtained according to the invention is carried out using anti-gluten antibodies and according to the immunoenzymatic technique already described.
  • This copolymer is used alone or in combination with filtration aids and is an effective and non-allergenic alternative for the refining of wines.
  • a variant of the above process also applies to the preparation of an alginate-tannin copolymer: a sample of 5 g is taken. of sodium alginate (E 401) which is dispersed with strong stirring in a mixer in 1 liter of an aqueous solution of 5% (W / V) gallic tannin at pH 7.2 and 20 ° C. A solution of 1 liter of calcium chloride at 10 g / liter is prepared in a beaker.
  • each drop of the alginate - tannin mixture immediately forms a gelled and coagulated minibilla.
  • the beads thus formed are washed twice in succession in one liter of distilled water.
  • the beads are then immersed for 60 minutes in a 5% solution of formaldehyde (CH 2 O) at pH 8.5.
  • the beads are then drained on sieves and then washed in 1 liter of glycine buffer (C2H5NO2) - NaCl-pH7.
  • the beads thus treated constitute a functional surface alginate-tannin copolymer which is then dried under vacuum at 5 ° C. then kept in airtight bags under inert atmosphere at 5 ° C. This copolymer is used at a rate of 300 to 500 gr of beads per hectolitre of wine to be glued.
  • the alginate-protein and alginate-tannin copolymers obtained according to the process which is the subject of the invention can be prepared with various biological molecules of animal, plant, fungal (mannoprotein) or bacterial origin used as oenological auxiliaries and they are new non-allergenic oenological compounds.
  • a fourth non-limiting example of realizing the process according to this second mode concerns the preparation and characteristics of a stable copolymer formed between an organic polyvinylpolypyrrolidone (PVPP) core and an anchored tanned peripheral layer.
  • PVPP organic polyvinylpolypyrrolidone
  • PVPP PolyvinylPolyPyrrolidone
  • the adsorption phase of the tannins on the PVPP is then carried out for 2 hours at 10 ° C., with intermittent stirring.
  • the preparation is then centrifuged (5000 rpm / 20 min) and the PVPP-tannin pellet is resuspended, by successive incorporation of 10 g aliquots, into one liter of a solution of tresyl chlorate 2-trifluoroethane sulfonyl - (C2H2CIF3O2S ) at 5% in phosphate buffer pH 8.5.
  • the anchoring of the tannins on the surface of the PVPP is continued for 60 minutes under gentle agitation, followed by centrifugation (5000 rpm / 20 min) and 2 washes of the PVPP-tannin pellet in 1 liter of water.
  • the compound is then dried under vacuum at 5 ° C. It is stored in powder form in a sealed bag under an inert atmosphere at 5 ° C.
  • the PVPP-tannin complex thus formed applies directly to white and rosé wines at a dose of 40 g per hectolitre. After incubation for 3 hours at 10 ° C., the PVPP-tan-ins complex binds the wine proteins in excess, and in particular natural oxidation enzymes such as laccase (EC 1 .10.3.2) and tyrosinase. (EC 1 .14.18.1) present in weathered grape juice. The PVPP-tannin-enzyme complex thus obtained is completely removed by clarifying filtration of the treated wines. This complex has the characteristics of insolubility and non-allergenicity of oenological products according to the invention.
  • An alternative embodiment of a PVPP-based compound according to the invention relates to the preparation and properties of a PVPP-tannin-protein multilayer copolymer.
  • the adsorption phase of the ovalbumin on the tannins is carried out for 2 hours at 10 ° C., by intermittent stirring every 10 minutes.
  • the PVPP-tannin-ovalbumin complex is filtered on fried glass or is resuspended. by successive additions of 5 g aliquots in 1 liter of a 1% solution of glutaraldehyde (C5H8O2) in pH 8.5 phosphate buffer with slow stirring for 60 minutes.
  • the PVPP-tannin-ovalbumin copolymer thus obtained is filtered and washed twice in 1 liter of glycine-NaCl buffer - pH 6.5 and then drained and dried under vacuum. It is stored in a bag under an inert atmosphere at 5 ° C. It is used for the bonding and clarification of wines and it has the immunological safety properties of the compounds according to the invention.
  • the manufacturing process according to the invention makes it possible to obtain a range of various oenological polymers which are within the scope of the present invention as functional and non-allergenic polymers.
  • various oenological polymers which are within the scope of the present invention as functional and non-allergenic polymers.
  • agarose-albumin copolymers agarose-casein copolymers, and agarose-gelatin copolymers, whose manufacturing uses, for the preparation of the support nucleus and for the anchoring of the functional molecules, to cyanogen bromide reagent ligands, or aldehyde type, or epichlorohydrin type, or dimethyladipimate type, or bis-sulfosuccinimidyl suberate type.
  • the agarose-lectin and agarose-enzyme copolymers whose production uses, for the preparation of the support nucleus and for the anchoring of the functional molecules, to ligand reagents of p-nitrophenyl chloroformate type or N-hydroxysuccinimide chloroformate type or type epichlorohydrin, or periodate type.
  • the activated carbon-protein copolymers, the zeolite-protein copolymers and the alumina-protein copolymers whose production uses, for the preparation of the support nucleus and for the anchoring of the functional proteins, to ligands reagents type aldehydes.
  • the present invention describes, according to various possible variants, a process for obtaining technological polymers with specific functional activities and without allergenic toxicity in an aqueous medium.
  • the present invention also relates to the industrial use of the technological polymers obtained according to the process and their implementation, alone or in various combinations, in the gluing, clarification and preservation of beverages of vegetable origin, in particular grape must, still and sparkling wines, juices, beers, ciders and vinegars.

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  • Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Wood Science & Technology (AREA)
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  • Inorganic Chemistry (AREA)
  • Peptides Or Proteins (AREA)
EP09760159A 2009-09-10 2009-09-10 Polymerisationsverfahren, im besonderen zur polymerisation von önologischen zusätzen und anhand dieses verfahrens hergestellte polymere Withdrawn EP2475707A1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/FR2009/051708 WO2011030007A1 (fr) 2009-09-10 2009-09-10 Procédé de polymérisation, notamment d'auxiliaires oneologiques et polymères obtenus par ce procédé

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EP2475707A1 true EP2475707A1 (de) 2012-07-18

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US4479970A (en) * 1983-04-15 1984-10-30 Corning Glass Works Process for removing natural colorants from wine
US4554088A (en) * 1983-05-12 1985-11-19 Advanced Magnetics Inc. Magnetic particles for use in separations
US5141611A (en) * 1985-05-16 1992-08-25 Memtec Limited Removing and recovering plant polyphenols
DE60017017T2 (de) * 1999-01-27 2006-04-13 Bayer Corp. Immuntest unter verwendung von partikeln mit kaseinumhüllungen

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