WO2015086027A1 - Turbidité stable pour boissons - Google Patents

Turbidité stable pour boissons Download PDF

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Publication number
WO2015086027A1
WO2015086027A1 PCT/DK2014/050420 DK2014050420W WO2015086027A1 WO 2015086027 A1 WO2015086027 A1 WO 2015086027A1 DK 2014050420 W DK2014050420 W DK 2014050420W WO 2015086027 A1 WO2015086027 A1 WO 2015086027A1
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WIPO (PCT)
Prior art keywords
starch
range
haze
μηι
fragment particles
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PCT/DK2014/050420
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English (en)
Inventor
Iain Donaldson
Pia Vaag
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Carlsberg A/S
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Publication of WO2015086027A1 publication Critical patent/WO2015086027A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C11/00—Fermentation processes for beer
    • C12C11/11—Post fermentation treatments, e.g. carbonation, or concentration
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52—Adding ingredients
    • A23L2/62—Clouding agents; Agents to improve the cloud-stability
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • A23L29/35—Degradation products of starch, e.g. hydrolysates, dextrins; Enzymatically modified starches
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/18—Dextrin, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C08J3/14—Powdering or granulating by precipitation from solutions
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C12/00—Processes specially adapted for making special kinds of beer
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C5/00—Other raw materials for the preparation of beer
    • C12C5/02—Additives for beer
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08J2303/02—Starch; Degradation products thereof, e.g. dextrin

Definitions

  • the present invention relates to the field of haze ingredients useful for production of hazy beverages.
  • clouding agents are emulsions of oils with as neutral a flavor as possible. Citrus oils are the most widely used, however due to the flavor, these have a limited use. Vegetable oil is also used, but less common due to poor resistance to oxidation. Vegetable gums have also been used as clouding agents, but quality has not always been reliable.
  • beta-limit dextrins manufactured from dull waxy starch can be used in the manufacture of beverage clouding agents.
  • US5,482,560 describes beta-limit dextrin produced by the action of a beta amylase on an aqueous slurry of dull waxy starch. It is described that these beta-limit dextrins can produce a solution having a solids content as high as 40% by weight at room temperature and thus the beta-limit dextrins are not useful as beverage clouding agents per se.
  • the document further describes that emulsions of solutions of beta-limit dextrins with flavor oils can be used as clouding agents.
  • the document describes the stability of aqueous emulsions and shows that absorbence decreases already after 35 days. Waxy starch is characterized by low levels of amylose, which are typically less than 10%, and frequently close to 0%. Summary of invention
  • a haze ingredient which is prepared from few ingredients and which is capable of providing a stable haze even upon long term storage.
  • a haze ingredient which does not comprise oil, such as flavour oil.
  • a haze ingredient with a neutral taste There is also a need for a haze ingredient with a neutral taste.
  • the present invention provides a haze ingredient that is prepared solely from starch and which provides a stable haze to a range of different beverages even upon long term storage.
  • the haze ingredient has a neutral taste and is therefore widely applicable.
  • the haze ingredient is prepared from starch and is thus particularly useful in beverages prepared from starch containing material, but can also be used in other kinds of beverages.
  • aqueous composition comprising starch, wherein said starch comprises amylose and amylopectin;
  • composition ii) contacting said composition with an a-amylase capable of hydrolysing
  • aqueous composition comprising starch, wherein said starch comprises amylose and amylopectin;
  • separating the starch fragments according to size iii) separating the starch fragments according to size; iv) recovering starch fragment particles, wherein at least 40% of the recovered starch fragment particles have a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , for example from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ ,
  • Figure 1 shows haze intensity over time of haze ingredient in a regular lager beer of 5% ABV stored for 55 days at 22 ° (Panel A) or at 37 ⁇ ⁇ (Panel B). Haze intensity was measured at 90° angle using light at 650 nm.
  • Figure 2 shows the size distribution of hydrodynamic diameters of starch fragment particles. Results were obtained by dynamic light scattering on a Malvern Mastersizer 3000. Scattering model: Mie. Result transformation type: volume. A) Size distribution of starch fragment particles of haze ingredient prepared from barley starch using ethanol precipitation for size separation. B) Size distribution of starch fragment particles of haze ingredient prepared from barley starch using centrifugation for size separation. C) Size distribution of starch fragment particles of haze ingredient prepared from maize starch using ethanol precipitation for size separation. D) Size distribution of starch fragment particles in haze ingredient prepared from potato starch using ethanol precipitation for size separation.
  • Figure 3 shows haze intensity over time of haze ingredient in a regular lager beer of 5% ABV stored for 1 month at the indicated temperatures. Haze intensity was measured at 90 ° angle using light at 650 nm.
  • Panel A shows the haze intensity of haze ingredient prepared from barley starch.
  • Panel B shows the haze intensity of haze ingredient prepared from wheat starch.
  • Panel C shows the haze intensity of haze ingredient prepared from maize starch.
  • Panel D) shows the haze intensity of haze ingredient prepared from potato starch.
  • Panel E) shows the haze intensity of haze ingredient prepared from pea starch.
  • Figure 4 shows haze intensity of haze ingredient in lager beer stored at 22 °C for 100 days. The haze ingredient was prepared from starch of barley, wheat, maize, and pea using centrifugation for the size separation. Haze intensity was measured at 90 ° angle using light at 650 nm.
  • Figure 5 shows haze intensity over time of haze ingredient prepared from barley starch in apple juice and in a non-alcoholic malt based beverage stored for almost 60 days at the indicated temperatures. Haze intensity was measured at 90° angle using light at 650 nm.
  • Figure 6 shows the absolute molecular weight as a function of eluted volume (left hand axis and dotted line), as well as the relative amount as a function of eluted volume (right hand axis and normal line).
  • A) shows the result for haze ingredient prepared from barley starch and B) the result for haze ingredient prepared from maize starch.
  • Figure 7 shows a proton spectrum obtained by NMR for a haze ingredient prepared from barley starch.
  • haze ingredient refers to composition consisting of small particles, that when added to a transparent liquid, results in reduced transparency of said liquid.
  • haze refers to reduced transparency of a liquid.
  • a beverage with a haze according to the invention is a beverage, which is not completely transparent.
  • internal glucosidic bond refers to any glycosidic bond covalently linking two glucose residues of a starch molecule, wherein said glucose residues are positioned so that there are at least 3 glucose residues separating the internal glucosidic bond from an end of a chain of glucose residues of said starch.
  • glycosidic linkage refers to a covalent linkage between two glucose residues, and may be used interchangeably herein with the term “covalent glycosidic bond”.
  • the carbon atoms of the glucose units linked by a glycosidic linkage may be specified by indicating the number of the carbon atoms.
  • a glycosidic linkage connecting carbon 1 of one glucose unit with carbon 4 of another glucose unit may be referred to as a 1 ,4-glycosidic linkage.
  • essentially all glycosidic linkages are a-glycosidic linkages.
  • starch fragment refers to a fragment of starch created by enzymatic cleavage of one or more internal glucosidic bonds. Starch fragments may have different sizes depending on the starting material, the degree of enzymatic cleavage and whether the starch fragments have been subjected to size separation.
  • the present invention relates to a haze ingredient, methods for producing the haze ingredient and to beverages comprising the haze ingredient.
  • the haze ingredient according to the present invention is preferably prepared from starch by enzymatic cleavage followed by size separation. Accordingly, the haze ingredient comprises or even consists of starch fragments. Such haze ingredient may also be referred to as dry haze ingredient. Upon contact with water, said starch fragments in general will form particles, which herein are designated "starch fragment particles". Said starch fragment particles preferably comprise water and starch fragments, and even more preferably the starch fragment particles consist of water and starch fragments. The haze ingredient may also comprise or consist of starch fragment particles. Such haze ingredient may also be referred to as wet haze ingredient.
  • a dry haze ingredient can be prepared from a wet haze ingredient by drying. Vice versa a wet haze ingredient can be prepared from a dry haze ingredient by mixing with water or another aqueous liquid.
  • Said starch fragments consist of linear or branched chains of glucose residues linked by glycosidic bonds. It is preferred that at least 50%, such as at least 60%, for example at least 70%, such as at least 80%, for example at least 90%, such as at least 95% of the haze ingredient consists of starch fragments consisting of linear or branched chains of glucose residues linked by glycosidic bonds.
  • the haze ingredient preferably comprises or even consists of starch fragments, wherein the starch fragments when in an aqueous environment are contained in starch fragment particles.
  • the haze ingredient may comprise or even consist of starch fragment particles, wherein the starch particle fragments preferably comprises or even consists of water and starch fragments, and it is preferred that at least 50%, such as at least 60%, for example at least 70%, such as at least 80%, for example at least 90%, such as at least 95% of the part of the starch fragment particles, which is not water consists of starch fragments consisting of linear or branched chains of glucose residues linked by glycosidic bonds.
  • At least some of the starch fragment particles to be used with the present invention have a hydrodynamic diameter of in the range from 0.03 ⁇ to 500 ⁇ , preferably in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , even more preferably from 0.04 ⁇ to 30 ⁇ , for example in the range from 0.04 to 1 ⁇ .
  • At least 40% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 ⁇ to 500 ⁇ , preferably in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , even more preferably from 0.04 ⁇ to 30 ⁇ , yet more preferably in the range from 0.04 to 1 ⁇ .
  • At least 50% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 ⁇ to 500 ⁇ , preferably in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , even more preferably from 0.04 ⁇ to 30 ⁇ , yet more preferably in the range from 0.04 to 1 ⁇ .
  • At least 60%, such as at least 70%, for example at least 80% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 ⁇ to 500 ⁇ , preferably in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , even more preferably from 0.04 ⁇ to 30 ⁇ , yet more preferably in the range from 0.04 to 1 ⁇ .
  • At least 80% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 to 500 ⁇ , preferably in the range of 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , yet more preferably in the range from 0.04 ⁇ to 40 ⁇ , even more preferably in the range from 0.04 to 30 ⁇ .
  • At least 90% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 to 500 ⁇ , preferably in the range of 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , yet more preferably in the range from 0.04 ⁇ to 40 ⁇ , even more preferably in the range from 0.04 to 30 ⁇ .
  • At least 95% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter of in the range from 0.03 to 500 ⁇ , preferably in the range of 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ .
  • At least 50% of the starch fragment particles of the haze ingredient have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ , more preferably from 0.04 to 40 ⁇ , even more preferably from 0.04 ⁇ to 30 ⁇ .
  • at least 60% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ , more preferably from 0.04 ⁇ to 30 ⁇ .
  • at least 70% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ , more preferably from 0.04 ⁇ to 30 ⁇ .
  • At least 80% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ , more preferably from 0.04 ⁇ to 30 ⁇ .
  • at least 90% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ , more preferably from 0.04 ⁇ to 30 ⁇ .
  • at least 95% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 100 ⁇ .
  • At least 30% of the particles of the haze ingredient have a hydrodynamic diameter in the range of 0.04 ⁇ to 1 ⁇ .
  • at least 40% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 1 ⁇ .
  • at least 50% of the particles of the haze ingredient may have a hydrodynamic diameter in the range of 0.04 ⁇ to 1 ⁇ .
  • at least some of the particles of the haze ingredient have a hydrodynamic diameter in the range of 1 to 50 ⁇ .
  • at least 1 %, such as at least of the starch fragment particles may have a hydrodynamic diameter in the range of 1 to 50 ⁇ .
  • at least 1 %, such as at least 5% may have a hydrodynamic diameter in the range of 1 to 30 ⁇ .
  • the hydrodynamic diameter is preferably determined by dynamic light scattering using a Mastersizer 3000 instrument from Malvern
  • hydrodynamic diameter is determined by dynamic light scattering using a Mastersizer 3000 instrument from Malvern Instruments Ltd., UK using a Mie scattering model with instrument settings as described in Example 2.
  • starch fragments of the haze ingredient have a useful molecular weight.
  • the invention relates to a method for preparing a haze ingredient, said method comprising the steps of
  • aqueous composition comprising starch, wherein said starch comprises amylose and amylopectin, e.g. any of the starch described herein below;
  • a-amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch, which e,g, may be any of the a-amylases describe herein below in the section "a-Amylase", thereby obtaining starch fragments contained in starch fragment particles,
  • haze ingredient may be mixed with a beverage in order to produce a beverage with a haze.
  • at least 75% of the starch fragments have a molecular weight in the range of 50 to 250000 kDa, preferably in the range of 53 to 220000 kDa. This may in particular be the case in embodiments of the invention, wherein the starch is starch of barley.
  • At least 75% of the starch fragments have a molecular weight in the range of 40 to100000 kDa, preferably in the range of 40 to 60000 kDa. This may in particular be the case in embodiments of the invention, wherein the starch is starch of maize.
  • Said starch fragments may have a molecular weight falling within the above-mentioned range and in addition having weight average molecular weight of in the range of 1000 to 10000 kDa, preferably in the range of 1500 to 5000 kDa, more preferably in the range of 1800 to 4000 kda.
  • the haze ingredient comprises starch fragments having a weight average molecular weight in the range of 2000 to 6000 kDa, preferably in the range of 3000 to 5000 kDa, even more preferably in the range of 3500 to 4600 kda. This may in particular be the case in embodiments of the invention, wherein the starch is starch of barley.
  • the haze ingredient comprises starch fragments having a weight average molecular weight in the range of 500 to 4000 kDa, preferably in the range of 1000 to 3000 kDa, even more preferably in the range of 1500 to 2500 kda. This may in particular be the case in embodiments of the invention, wherein the starch is starch of maize.
  • the haze ingredient comprises starch fragments having a number average molecular weight in the range of 200 to 700 kDa, preferably in the range of 300 to 600 kDa, even more preferably in the range of 350 to 550 kda.
  • the haze ingredient may comprise or consist of starch fragment particles having above mentioned hydrodynamic diameter and comprising starch fragments, wherein 75% of all starch fragments in the haze ingredient a have a molecular weight in the range of 40 to 250000 kDa; and/or
  • the starch fragments have a weight average molecular weight in the range of 1000 to 10000 kDa, preferably in the range of 1500 to 5000 kDa, more preferably in the range of 1800 to 4000 kda; and/or
  • the starch fragments have a number average molecular weight in the range of 200 to 700 kDa, preferably in the range of 300 to 600 kDa.
  • Molecular weight may be determined by any useful method, but is preferably determined using a system combining asymmetric flow field-flow fractionation, multi- angle laser light scattering, and refractive index detection set up to measurement of starch.
  • the molecular weight may be determined as described in Example 6 herein below, on an AF4-MALLS instrument available from Wyatt Technology.
  • Average molecular weight may be calculated as outlined in Example 6 herein below.
  • the haze ingredient comprises or even consists of starch fragments or starch fragment particles, wherein the starch fragment particles preferably consists of starch fragments and water.
  • Said starch fragment may be linear or branched. It is preferred that at least some of the starch fragments are branched.
  • the individual glucose units are linked by 1 ,4 - glycosidic linkages, whereas branching in starch is introduced by 1 ,6-glycosidic linkages.
  • the ratio of 1 ,6-glycosidic linkages to 1 ,4-glycosidic linkages is a measure for the degree of branching of starch.
  • Starch fragments having a high ratio of 1 ,6-glycosidic linkages to 1 ,4-glycosidic linkages are highly branched, and vice versa.
  • the ratio of 1 ,6-glycosidic linkages to 1 ,4-glycosidic linkages is typically 1 to in the range of 24 to 30.
  • the haze ingredient of the invention comprises starch fragments, wherein said starch fragments have an intermediate degree of branching, which preferably is lower than in typical amylopectin.
  • the degree of branching may be intermediate between the degree of branching of amylose (essentially no branching) and amylopectin.
  • the haze ingredient of the invention comprises starch fragments, wherein said starch fragments have a ratio of 1 ,6-glycosidic linkages to 1 ,4- glycosidic linkages of 1 to in the range of 10 to 20, preferably 1 to in the range of 10 to 16, more preferably 1 to in the range of 1 1 to 15, yet more preferably 1 to in the range of 12 to 14.
  • the invention relates to a method for preparing a haze ingredient, said method comprising the steps of
  • aqueous composition comprising starch, wherein said starch comprises amylose and amylopectin, e.g. any of the starch described herein below;
  • a-amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch, which e,g, may be any of the a-amylases describe herein below in the section "a-amylse", thereby obtaining starch fragments contained in starch fragment particles,
  • Said haze ingredient may be mixed with a beverage in order to produce a beverage with a haze.
  • starch fragments are not exclusively amylose fragments, but rather that said fragments comprise some degree of branching.
  • the ratio of 1 ,6-glycosidic linkages to 1 ,4-glycosidic linkages may be determined by any useful method, preferably using NMR.
  • the ratio of 1 ,6-glycosidic linkages to 1 ,4-glycosidic linkages may be determined as described herein below in Example 7.
  • the haze ingredient does not comprise any significant amounts of oil, and in particular, the haze ingredient does not comprise any significant amount of citrus oil. Similarly, the haze ingredient also preferably does not comprise any significant amount of terpene oil. Thus, the haze ingredient preferably comprises at the most 1 % oil, for example the haze ingredient comprises at the most 1 % citrus oil, for example the haze ingredient comprises at the most 1 % terpene oil.
  • the hase ingredient does not comprise any significant amount of starch sodium octenyl succinate.
  • the haze ingredient comprises at the most 1 % starch sodium octenyl succinate, and more preferably the haze ingredient comprises no detectable starch sodium octenyl succinate.
  • the invention relates to a haze ingredient, which in particular may be the haze ingredient described herein above in the section "Haze ingredient".
  • the haze ingredient may preferably e prepared by a method comprising the steps of
  • composition ii) contacting said composition with an a-amylase capable of hydrolysing
  • the composition comprising starch may comprise any of the starches described herein below in the section "Starch".
  • the composition may comprise only one kind of starch, for example barley starch or the composition may comprise a mixture of different starches.
  • the composition may consist of starch, however frequently, the composition consists of a plant product comprising starch. Said plant product is typically a fraction of a plant, which is enriched in starch content.
  • composition comprising starch is in general an aqueous solution or suspension comprising said starch.
  • the composition comprising starch may in one embodiment consist of water and starch.
  • the composition may consist of water and fractions of one or more plants, which are enriched in starch.
  • the composition comprising starch may in yet another embodiment consist of water and plant parts. Said plant may be any of the plants, which are useful sources for starch described herein below in the section "Starch".
  • the ⁇ -amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch may be any of the a-amylases described herein below in the section "a-amylase”.
  • the composition comprising starch may in general be contacted with said ⁇ -amylase in any manner allowing for activity of said a-amylase.
  • the composition comprising starch is contacted with said ⁇ -amylase in an aqueous solution or suspension.
  • the composition comprising starch may be an aqueous solution or suspension comprising starch, and in these embodiments the ⁇ -amylase may be added directly to said solution or suspension.
  • the time for incubation may differ depending on the amount of ⁇ -amylase used and the
  • the amount of enzyme, the time of incubation and the temperature of incubation is preferably selected so as to obtain a large number starch fragments with a hydrodynamic diameter in the range of 0.03 to 500 ⁇ , preferably in the range of 0.03 to 150 ⁇ , more preferably in the range of 0.04 ⁇ to 100 ⁇ , yet more preferably in the range from 0.04 ⁇ to 40 ⁇ , even more preferably in the range of 0.04 ⁇ to 30 ⁇ , such as in the range of 0.04 to 1 ⁇ .
  • the composition comprising starch is contacted with said ⁇ -amylase for in the range of 30 minutes to 10 hours, for example for in the range of 45 minutes to 10 hours, such as for in the range of 45 minutes to 5 hours, such as in the range of 1 to 5 hours, for example for in the range of 1 to 3 hours.
  • the composition comprising starch may be incubated with the ⁇ -amylase for in the range of 1 to 3 hours at a temperature in the range of 20 to 80°, such as in the range of 20 to 70 °C.
  • the temperature is selected in order to allow activity of said a-amylase.
  • at least part of the incubation of the composition comprising starch with ⁇ -amylase is performed at a temperature above the gelatinization temperature of the starch used.
  • Gelatinization temperature is in general a range, and it is preferred that at least part of the incubation of the composition comprising starch with a-amylase is performed at a temperature above the peak gelatinization temperature of the starch used, such as at least 1 °, for example at least 2° above the the peak gelatinization temperature of the starch used.
  • the peak gelatinization temperature for barley starch may be in the range of 64 to 67°, such as in the range of 65 to 66 °C.
  • the starch comprises or consists of barley starch
  • at least part of the incubation with a-amylase is performed at a temperature above 64 °C, such as above 65 °C, for example above 66 °C, such as above 67 °C, for example above 68 °C, such as above 69 °C.
  • the peak gelatinization temperature may be in the range of 58 to 62 °C.
  • the starch comprises or consists of wheat starch
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 60 °C, such as above 61 °C, for example above 62 °C, such as above 63 °C.
  • the gelatinization is performed at a temperature above 60 °C, such as above 61 °C, for example above 62 °C, such as above 63 °C.
  • the temperature may be in the range of 57 to 70 °C.
  • the starch comprises or consists of rye starch
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 65 °C, such as above 66 °C, for example above 67 °C, such as above 68 °C, for example above 69 °C, such as above 70 °C.
  • the gelatinization temperature may be in the range of 53 to 59 °C.
  • the starch comprises or consists of oat starch
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 56 °C, such as above 57 °C, for example above 58 °C, such as above 59 °C.
  • the peak gelatinization temperature may be in the range of 64 to 66 °C.
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 66 °C, such as above 67°C, for example above 68 °C.
  • the peak gelatinization temperature may be in the range of 69 to 72 °C.
  • the starch comprises or consists of maize starch
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 70 °C , such as above 71 °C , for example above 72 °C.
  • the gelatinization temperature may be in the range of 68 to 78 °C.
  • at least part of the incubation with ⁇ -amylase is performed at a temperature above 74 °C, for example above 75 °C, such as above 76 °C, for example above 78 °C.
  • the peak gelatinization temperature may be in the range of 64 to 67°C.
  • the starch comprises or consists of pea starch
  • at least part of the incubation with a-amylase is performed at a temperature above 65 °C, such as above 66 °C, for example above 67 °C, such as above 68 °C, for example above 69 °C.
  • At least part of the incubation of the composition comprising starch with ⁇ -amylase is performed at a temperature at which a-amylase retains activity.
  • at least part of the incubation of the composition comprising starch with ⁇ -amylase is performed at a temperature at which a-amylase retains activity.
  • composition comprising starch with a-amylase, and even more preferably that most of the incubation of the composition comprising starch with ⁇ -amylase is performed at a temperature below 90 °C, preferably below 80 °C.
  • the incubation of the composition comprising starch may thus be performed at a temperature in the range of 20 to 80 °C, such as a temperature in the range of 20 to 70 °C, for example a temperature in the range of 50 to 80 °C, such as a temperature in the range of 50 to 75 °C, for example a temperature in the range of 50 to 70 °C.
  • the temperature is varied so that the composition comprising starch is contacted with said ⁇ -amylase at a relatively low temperature and the temperature may then be increased gradually.
  • the initial temperature may be in the range of 15 to 30°C.
  • the temperature may for example be increased to a temperature in the range of 50 to 75 °C.
  • the temperature may be increased gradually for example by 0.1 to 5°C per minute.
  • the composition comprising starch may be incubated with said ⁇ -amylase for in the range of 30 to 60 minutes at a temperature in the range of 50 to 75°C.
  • composition comprising starch fragments may be further treated as described below.
  • the incubation may be performed in any useful container. It is preferred that the container is container in which the temperature can be controlled.
  • the container may be a mash kettle, however many other kinds of containers may be employed with the methods of the invention.
  • the method of preparing a haze ingredient does not involve use of endo-a-1 ,6-glucanohydrolase. Thus, it is preferred that no endo-a- 1 ,6-glucanohydrolase is added to the aqueous composition comprising starch.
  • Said endo-a-1 ,6-glucanohydrolase may for example be pullulanase or isoamylase or amylo- 1 ,6-glucosidase.
  • the methods of the invention preferably comprise a step of inactivating the a-amylase subsequent to incubation of the composition comprising starch with said a-amylase.
  • the ⁇ -amylase is inactivated at a time when a large proportion of the starch fragment particles have a hydrodynamic diameter in the range from 0.03 ⁇ to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • the a- amylase may for example be inactivated by increasing the temperature.
  • the method comprises a step of heating the composition comprising starch and ⁇ -amylase to a temperature of at least 90°, preferably to at least 95 °C, such as to around ⁇ ⁇ 00 °C for at least 30 min, such as for in the range of 30 to 120 minutes, for example for in the range of 30 to 75 minutes.
  • the method of the invention may comprise the steps of providing an aqueous composition comprising starch, such as any of the starch described herein below in the section "Starch";
  • ⁇ -amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch (e.g. any of the a-amylases described herein below in the section "a-amylase") at a temperature allowing activity of said a-amylase, thereby obtaining starch fragments contained in starch fragment particles,
  • the method comprises a step of phase separation. This step is optional and may be omitted.
  • the phase separation is generally performed after inactivation of the a-amylase at high temperature by cooling the composition containing starch fragments slightly and leaving the mixture without stirring for an extended amount of time.
  • the phase separation may for example be obtained by incubation of the composition containing starch fragments at a temperature in the range of 70 to 90 °C, such as at a temperature in the range of 75 to 85 °C, for example at a temperature in the range of 78 to 82 °C for in the range of 10 to 60 hours, such as in the range of 10 to 48 hours, for example for in the range of 10 to 24 hours, such as in the range of 15 to 48 hours, such as in the range of 15 to 24 hours, for example for in the range of 18 to 22 hours.
  • Said incubation is preferably done in the absence of movement of said composition, i.e. in the absence of stirring or shaking.
  • composition comprising starch fragments will generally have separated into a top phase and a bottom phase.
  • both of these phases comprise starch fragments and either the top phase or the bottom phase may be employed for the further procedure.
  • a mixture of the phases may be employed or the phase separation step may also be omitted.
  • the methods of the invention may comprise an additional step of retrograding the starch fragments after incubation with a-amylase.
  • Retrogradation is the process in which starch fragments realign after gelatinization. Retrogradation is in general obtained by extended incubation at a low temperature. It is especially preferred that the methods comprises a step of retrogradation in embodiments of the invention where incubation with ⁇ -amylase is performed at least partly at a temperature above the gelatinization temperature of the starch used.
  • Retrogradation may for example be obtained by incubation of the composition comprising starch fragments at a temperature in the range of 2 to 10 °C, for example in the range of 2 to 8°C, such as in the range of 2 to 7°C, for example in the range of 4 to 6°C.
  • the incubation at said temperature is preferably extended, and thus the incubation is in general for at least 10 hours, such as at least 15 hours, for example at least 18 hours, such as for in the range of 10 to 40 hours, for example for in the range of 15 to 40 hours, such as in the range of 15 to 30 hours, for example for in the range of 15 to 25 hours, such as for in the range of 18 to 22 hours.
  • the methods of the invention comprises the steps of
  • aqueous composition comprising starch, such as any of the starch described herein below in the section "Starch”;
  • a-amylase optionally inactivating said a-amylase, for example by incubation at a high temperature as described above;
  • starch fragment particles wherein at least 40% of the recovered starch fragment particles have a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , for example from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • the invention relates to a haze ingredient comprising starch fragments or starch fragment particles.
  • starch fragments When in an aqueous environment the starch fragments will be contained in starch fragment particles comprising or consisting of water and starch fragments.
  • Said starch fragment particles preferably have a hydrodynamic diameter in the range of 0.03 ⁇ to 500 ⁇ , and it is preferred that at least 40% of the recovered starch fragment particles have a hydrodynamic diameter in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • methods of preparing the haze ingredient frequently comprises a step of separating starch fragments according to size and then recovering the starch with a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , for example from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • the size separation may be performed by any suitable method known to the skilled person to be useful for separating particles with a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , preferably in the range from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ from smaller and larger particles.
  • the size separation is performed with the aid of precipitation.
  • the precipitation may be done using any useful precipitating agent.
  • the method may contain only one precipitation step or it may contain two or more sequentially precipitation steps. It is however important that sufficient precipitations are undertaken to recover starch fragments of the desired size.
  • the method may for example contain the steps of: contacting the aqueous composition comprising starch fragments particles with a precipitating agent in an amount capable of precipitating starch fragments with a hydrodynamic diameter larger than than 500 ⁇ , preferably larger than 150 ⁇ , more preferably larger than 100 ⁇ , such as capable of precipitating at least part of starch fragments particles with a hydrodynamic diameter larger than 30 ⁇ , such as larger than 1 ⁇ ; and recovering the supernatant; and
  • starch fragment particles wherein at least 40%, such as at least 50% of the starch fragment particles have a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , for example from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • the precipitating agent may be any precipitating agent known to the skilled person to be useful for the precipitation of carbohydrates, such as starch.
  • the precipitating agent may be selected from the group alcohols, small ketones and cationic detergents. 2Q
  • Said small ketone may for example be acetone.
  • Said cationic detergent may for example be compounds comprising an alkyl chain containing at least 10 carbons, and a quaternary ammonium ion.
  • Non-limiting examples of cationic detergents useful as precipitating agents includes cetyltnmethylammonium hydroxide or hexadecyltrimethyl ammonium bromide.
  • the precipitating agent is an alcohol.
  • Said alcohol may for example be a Ci-e-alkyl-OH or an C 5 . 6 -aryl-OH.
  • the alcohol may for example be selected from the group consisting of ethanol, isopropanol and phenol.
  • the precipitating agent is ethanol.
  • the size separation comprises at least one ethanol precipitation.
  • the size separation involves at least two ethanol precipitations, and thus the size separation may contain the steps of: i) contacting the composition comprising starch fragments with an amount of Ci-6-alkyl-OH, preferably ethanol capable of precipitating starch fragments with a hydrodynamic diameter larger than 500 ⁇ , preferably larger than 150 ⁇ , more preferably larger than 100 ⁇ , such as capable of precipitating at least part of starch fragments particles with a hydrodynamic diameter larger than 30 ⁇ , such as larger than 1 ⁇ ; and
  • ethanol capable of precipitating starch fragments with a hydrodynamic diameter larger than 0.03 ⁇ , such as larger than 0.04 ⁇ ; and iv) recovering the precipitate, thereby recovering starch fragment particles, wherein at least 40%, such as at least 50% of the starch fragment particles have a hydrodynamic diameter in the range from 0.03 ⁇ to 500 ⁇ , for example from 0.03 to 150 ⁇ , more preferably in the range of 0.04 to 100 ⁇ , such as from 0.04 ⁇ to 30 ⁇ , for example from 0.04 to 1 ⁇ .
  • the amount of precipitating agent to be employed will depend on the temperature at which the precipitation is performed. It is important that a concentration of precipitating agent is selected, which results in precipitation of starch fragments of sizes as described above.
  • the size separation may comprise the steps of a) contacting an aqueous solution containing the starch fragments with a Ci- 6 -alkyl-OH, for example ethanol to a final concentration in the range of 25 to 35%, such as in the range of 27 to 29%
  • Ci-e-alkyl-OH for example ethanol to a final concentration in the range of 40 to 60%, such as in the range of 45 to 55%
  • concentrations are in particular relevant in embodiments of the invention, where the precipitation is performed at room temperature, such as at a temperature in the range of 20 to 30 °C, for example in the range of 20 to 25°.
  • room temperature such as at a temperature in the range of 20 to 30 °C, for example in the range of 20 to 25°.
  • the precipitation is performed at lower temperatures, then in general less Ci-6-alkyl-OH, for example ethanol may be used.
  • Recovering the supernatant or the precipitate may for example be done by
  • the precipitate may be allowed to settle by simple gravitation followed by separation of the supernatant from the precipitate.
  • Recovering the precipitate may also comprise a step of drying the precipitate in order to remove all supernatant.
  • the precipitate may be recovered and then subjected to drying, for example freeze-drying or spray-drying. After drying the haze ingredient will in general be a dry haze ingredient comprising mainly starch fragments.
  • the size separation may also be performed by chromatographic method and in particular using size exclusion chromatography.
  • the size separation may also be performed using Asymmetric Flow-Field-Flow-Fractionation (AF4).
  • AF4 Asymmetric Flow-Field-Flow-Fractionation
  • the size separation may also be accomplished by centrifugation.
  • the size separation may comprise one or more centrifugation steps followed by recovery of supernatant.
  • the composition comprising the starch fragments may be stored at a low temperature for an extended period of time.
  • the method for preparing the haze ingredient may comprise the steps of providing an aqueous composition comprising starch, such as any of the starch described herein below in the section "Starch";
  • a-amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch (e.g. any of the a-amylases described herein below in the section "a-amylase") at a temperature above the gelatinization temperature of said starch, wherein said temperature allows activity of said a-amylase, thereby obtaining starch fragments contained in starch fragment particles,
  • a-amylase optionally inactivating said a-amylase, for example by incubation at a high temperature as described above;
  • steps v) and vi) are performed more than once, such as twice, for example 3 times, such as 4 times, for example 5 times, such as in the range of 2 to 10 times, for example in the range of 3 to 7 times, such as in the range of 4 to 6 times.
  • the centrifugation may be performed for any suitable amount of time, such as for in the range of 5 to 60 minutes, such as in the range of 5 to 40 minutes, such as in the range of 10 to 30 minutes, for example for in the range of 10 to 20 minutes.
  • the time for each centrifugation may be the same or different and thus each centrifugation may individually be for in the range of 5 to 60 minutes, such as in the range of 5 to 40 minutes, such as in the range of 10 to 30 minutes, for example for in the range of 10 to 20 minutes.
  • the centrifugation may be performed at any speed, which is sufficiently high to settle particles larger than 500 ⁇ , preferably larger than 150 ⁇ , more preferably larger than 100 ⁇ , such as capable of settle at least part of starch fragments particles with a hydrodynamic diameter larger than 30 ⁇ , such as larger than 1 ⁇ in the pellet.
  • centrifugation may be performed for at in the range of 2000 to 10.000 xG, preferably in the range of 2500 to 7000 xG, more preferably in the range of 2800 to 5000 xG, such as in the range of 3000 to 4500 xG.
  • the speed for each centrifugation may be the same or different and thus each centrifugation may individually be for in the range of 2000 to 10.000 xG, preferably in the range of 2500 to 7000 xG, more preferably in the range of 2800 to 5000 xG, such as in the range of 3000 to 4500 xG.
  • the speed of centrifugation may vary during the centrifugation.
  • the speed of centrifugation may increase during the centrifugation. This may be done step-wise or gradually.
  • the invention also relates to methods for producing beverages, and in particular to methods of producing beverages with a haze.
  • the invention also relates to beverages producedby the method.
  • the method for producing a beverage in general comprises the steps of
  • the haze ingredient may be any of the haze ingredients described herein above, and said haze ingredient may be prepared by any of the methods for preparing a haze ingredient described herein above.
  • the haze ingredient may be provided as a dry haze ingredient or as a wet haze ingredient.
  • the beverage may be any beverages, for example any of the beverages described herein below in the section "Bevarage".
  • the method of preparing a beverage with a haze thus comprises the steps of providing an aqueous composition comprising starch, wherein said starch may be any of the starch described herein above in the section "Starch”, and wherein said starch comprises amylose and amylopectin;
  • a-amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages of starch (e.g. any of the a-amylases described herein below in the section "a-amylase") thereby obtaining starch fragments contained in starch fragment particles;
  • a beverage which for example may be any of the beverages described herein below in the section "Beverage";
  • the starch fragments are recovered as a precipitate. This is in particular the case, when the seize separation is performed using precipitation with an alcohol.
  • the haze ingredient When the haze ingredient is in the form of a precipitate, then it may be desirable to include a step of dispersing the haze ingredient between steps iv) and v) of the method.
  • Said additional step may comprise dispersing the haze ingredient in an aqueous solution.
  • This may for example be obtained by incubating the haze ingredient in an aqueous solution (e.g. in water) at an elevated temperature, such as a temperature in the range of 90 to 100°C for in the range of 5 to 120 min., such as in the range of 10 to 60 min. e.g. for in the range of 15 to 30 min.
  • the haze ingredient may be boiled in an aqueous solution (e.g. in water).
  • the aqueous solution may then be mixed with said beverage.
  • the beverage according to the present invention may be any beverage in which a haze is desirable. For many kinds of beverage a haze is desirable for aesthetic reasons.
  • the beverage is a plant derived beverage.
  • a plant derived beverage may be any beverage prepared using plants, for example a plant derived beverage may be a beverage prepared by extraction of a plant or plant part in water or by squeezing a plant or plant part.
  • the beverage may comprise or even consist of an extract or a juice of a plant or a plant part.
  • the beverage may also be an extract or a juice of a plant or a plant part to which one or more additional ingredients have been added, for example flavouring compounds or preservatives.
  • the beverage is a fruit juice, such as a juice of a citrus fruit or a pomaceous fruit.
  • the citrus fruit may for example be selected from the group consisting of orange, lime, pomelo, lemon, mandarin, satsuma, grape fruit and kumquats.
  • the pomaceous fruit may for example be selected from the group consisting of apple and pear.
  • the beverage is a fermented fruit juice.
  • the beverage may be selected from the group consisting of fermented apple juice and fermented pear juice.
  • the beverage is an extract of a fruit, for example an extract of dried fruits or berries
  • the beverage may be an extract of a fruit selected from the group consisting of rosehip, sloe and crowberry.
  • the beverage may also be or comprise an extract of a plant for example a herbal extract.
  • herbal extracts includes an extract of green tea, black tea, rooibos, peppermint or hops.
  • the extract of a plant may also be a flower extract.
  • Non limiting examples of flower extracts includes hibiscus camomile, elderflower, lavender or linden flower.
  • the extract of a plant may also be a fruit extract.
  • the flavour compound may be any useful flavour compound.
  • the flavour compound may for example be selected from the group consisting of aromas, plant extracts, plant concentrates, plant parts and herbal infusions.
  • the flavour compound may for example be an aroma.
  • Aromas are typically organic compounds, for example they may be plant secondary metabolites.
  • the aroma may be any aroma, for example a fruit aroma or vanilla aroma.
  • Non-limiting examples of fruits useful for fruit aroma, fruit extract or fruit concentrates include orange, apple, banana, lemon, passion fruit, mango, pineapple, pears, kumquats or pomelo.
  • the beverage may also be any carbonated beverage, such as a carbonated soft drink.
  • the carbonated soft drinks may be prepared from fruit extracts, fruit juices or fruit concentrates, however, the soft drinks may also be based on other flavours, such as ginger or tonic.
  • the carbonated beverage may also be an alcoholic drink.
  • the beverage is a cereal based beverage.
  • the beverage may be a malt based beverage.
  • the malt based beverage may be any beverage prepared from malt.
  • the malt will in general be barley malt, but in some embodiments of the invention the malt may also be malt of other cereal, for example wheat.
  • preparation of malt based beverages comprises a step of milling malt followed by an aqueous extraction, for example by mashing.
  • the milled malt may be subjected to several rounds of aqueous extraction, for example to mashing and sparging.
  • the aqueous malt extract is wort, such as first wort, second wort, further worts or a mixture of one or more of the aforementioned.
  • the malt is mixed with one or more adjuncts before or during the aqueous extraction.
  • the adjuncts may be any carbohydrate source other than malt, such as, but not limited to unmalted cereals e.g. barley, cereal syrups, cereal starch or grits.
  • the cereal may be any cereal, for example any member of the Graminae plant family, cultivated primarily for their starch-containing seeds or kernels. Cereals include, but are not limited to barley (Hordeum), wheat (Triticum), rice (Oryza), maize (Zea), rye (Secale), oat (Avena), sorghum (Sorghum), and Triticale, a rye-wheat hybrid.
  • the wort may be further treated by a number of methods to arrive at the final beverage.
  • the wort may for example be treated with one or more enzymes, such lipases, starch degrading enzymes (e.g. amylases, such as oc-amylase, ⁇ -amylase and/or maltogenic oc-amylase), glucanases [such as (1 -4)- and/or (1 -3,1 -4) ⁇ -glucanase], and/or xylanases (such as arabinoxylanase), and/or proteases, or enzyme mixtures comprising one or more of the aforementioned enzymes, e.g. Cereflo, Ultraflo, or Ondea Pro (Novozymes).
  • the beverage has not been treated with protease, such as with proline-specific endo-proteases at any time during production of said beverage.
  • the cereal based beverage may also be added to the wort, e.g. hops.
  • the wort may be heated or even boiled.
  • the wort such as the heated or boiled wort may also be subjected to fermentation, for example to fermentation by yeast.
  • the cereal based beverage or the malt based beverage may also be carbonated.
  • the beverage is beer, for example the beer may be a lager beer or an ale.
  • the beer may for example be selected from the group consisting of altbier, Amber ale, Barley wine, Ralph weisse, Whye de Garde, Bitter, Blonde Ale, Bock, Brown ale, California Common, Cream Ale, Dortmunder Export, Doppelbock, Bis, Bisweizen, Eisbock, Fruit Iambic, Golden Ale, Gose, Gueuze, Hefeweizen, Helles, India pale ale, Kolsch, Lambic, Light ale, Maibock, Malt liquor,
  • the cereal based beverage may also be a non-alcoholic beverage.
  • the malt based beverage may for example be a non-alcoholic beer or other kinds of nonalcoholic malt based beverages.
  • Said non-alcoholic malt based beverages may also contain flavor compounds, such as fruit flavor compounds.
  • Non-limiting examples of non-alcoholic malt based beverages includes Maltina,Moussy, or Holsten.
  • the beverage may also be any of the above-mentioned beverages to which one or more additional ingredients have been added, although in other embodiments the beverage is any of the aforementioned to which no further ingredients have been added except for the haze ingredient.
  • Said additional ingredient may in one
  • an embodiment be an extract of a cereal and/or a malt extract, such as an extract made from non-malted cereals and malted barley.
  • a malt extract such as an extract made from non-malted cereals and malted barley.
  • examples of such an extract include an extract of oat, an extract of barley, a multigrain extract, an extract of wheat, an extract of non-malted oat and malted barley, an extract of non-malted barley and malted barley, a non-malted multigrain extract and malted barley, an extract of non-malted wheat and malted barley.
  • Such extracts are for example Otex or Whetex available from Senson, Finland.
  • Said additional ingredient may also be a polysaccharide, such as maltodextrin.
  • the beverages of the invention may be any of the aforementioned beverages containing the haze ingredient according to the invention.
  • the beverage may contain 0.5 to 10 g/L, such as 1 to 5 g/L, for example 1 to 3 g/L of dry haze ingredient.
  • the beverage may be any of the aforementioned beverages containing 5 to 10 g/L, preferably 1 to 5 g/L, such as 1 to 4 g/L, for example 1 to 3 g/L of dry haze ingredient according to the invention.
  • the beverage contains sufficient haze ingredient for the beverage to appear hazy to the human eye.
  • the haze intensity of the beverage is at least 4 EBC units, preferably at least 5 EBC units, for example at least 6 EBC units, when determined at 650 nm at 90° angle.
  • the haze ingredient according to the present invention can provide a stable haze, i.e. that a beverage containing the haze ingredient of the invention continues to be hazy even upon storage.
  • beverages containing in the range of 1 to 5 g/L, preferably in the range of 1 to 4 g/L of dry haze ingredient continues to be hazy even upon storage.
  • the haze intensity of the beverage determined as EBC units at 650 nm at 90° angle decreases at the most 20%, preferably at the most 10%, even more preferably at the most 5% upon storage at 22 °C for 50 days compared to the haze intensity after storage for 1 day.
  • the haze intensity of the beverage determined as EBC units at 650 nm at 90° angle decreases at the most 20%, preferably at the most 10%, even more preferably at the most 5% upon storage at 37 °C for 50 days compared to the haze intensity after storage for 1 day.
  • the haze intensity determined as EBC units at 650 nm at 90° angle decreases at the most 20%, preferably at the most 10%, even more preferably at the most 5% upon storage at 22 °C for 50 days compared to the haze intensity after storage for 1 day compared to the haze intensity after storage for 1 day.
  • the haze intensity determined as EBC units at 650 nm at 90° angle decreases at the most 20%, preferably at the most 10%, even more preferably at the most 5% upon storage at 37 °C for 50 days compared to the haze intensity after storage for 1 day.
  • the haze intensity of the beverage determined as EBC units at 650 nm at 90° angle is not altered by more than 20%, preferably not by more than 10% upon storage at 22 °C for 30 days compared to the starting haze intensity.
  • the invention relates to a haze ingredient and methods of preparing it from a composition comprising starch.
  • the composition comprising starch preferably comprises a high level of starch.
  • the composition is an aqueous composition comprising starch dissolved or suspended in water. It is preferred that the composition apart from water comprises at least 80%, preferably at least 90%, more preferably at least 95%, even more preferably at least 99% starch.
  • the composition comprising starch may consist of water and a non-water component and said non-water component preferably comprises at least 80%, preferably at least 90%, more preferably at least 95%, even more preferably at least 99% starch.
  • the composition comprising starch consists of water and starch.
  • the starch is preferably homopolysaccharide composed only of glucoside units.
  • the starch may comprise amylose and/or amylopectin. More preferably, the starch consists of amylose and/or amylopectin.
  • Amylose is a homopolysaccharide composed only of glucoside units, wherein almost all are connected through a-D-1 ,4- glucosidic bonds.
  • Amylopectin is a homopolysaccharide composed only of glucoside units, wherein in the range of 2 to 10% are connected through a-D-1 ,6-glucosidic bonds and the rest are connected through a-D-1 ,4-glucosidic bonds.
  • the starch may have a different content of amylopectin and amylose.
  • the starch comprises at least 10%, such as at least 15%, such as at least 20% amylose.
  • the starch may in one embodiment comprise in the range of 15 to 35%, preferably in the range of 20 to 35% amylose, for example in the range of 15 to 30%, more preferably in the range of 20 to 30% amylose.
  • Aforementioned content of amylose may be advantageous to obtain a good yield of haze ingredient.
  • the starch may comprise in the range of 20 to 30% amylose and in the range of 70 to 80% amylopectin.
  • starch with a different composition of amylose and amylopectin can also be used with the present invention.
  • the starch may be starch of any useful source, in general the source will be a plant.
  • the starch may be starch of a plant selected from the group consisting of barley, maize, wheat, rice, rye, oat, sorghum, pea, potato, cassava, sweet potato, millet, buckwheat, quinoa, amaranth, legumes and seaweed.
  • the starch is starch of a cereal, a tuber or a legume, preferably the starch is starch of a cereal or a tuber, more preferably of a cereal.
  • the starch may also be a mixture of any of the aforementioned starches.
  • the starch is barley starch.
  • Barley starch in general comprises in the range of 20 to 30% amylose and in the range of 70 to 80% amylopectin. a-Amylase
  • the present invention relates to methods for preparing a haze ingredient using an a- amylase as well as to a haze ingredient prepared using these methods.
  • the a-amylase to be used with the invention may be any ⁇ -amylase capable of hydrolysing internal (1 ⁇ 4)-a- glucosidic linkages.
  • the ⁇ -amylase to be used with the present invention is an enzyme capable of hydrolysing internal (1 ⁇ 4)-a-D- glucosidic linkages.
  • ⁇ -amylase capable of catalysing hydrolysis.
  • the ⁇ -amylase to be used with the present invention is an enzyme capable of catalysing hydrolysis of (1 ⁇ 4)-a-D-glucosidic linkages, which are located more than two glucose-units away from the non-reducing ends of polysaccharides.
  • the ⁇ -amylase may be an ⁇ -amylase capable of hydrolizing (1 ⁇ 4)-a-D- glucosidic linkages of cyclodextrins.
  • the ⁇ -amylase may also contain one or more additional activities, although this is not required.
  • the ⁇ -amylase may also be a maltogenic amylase, and thus the ⁇ -amylase may also be capable of hydrolyzing (1 ⁇ 4)-a-D-glucosidic linkages in polysaccharides so as to remove successive a- maltose residues from the non-reducing ends of polysaccharides, in particular from starch.
  • the a-amylase is an anti-staling amylase.
  • useful antistaling amylases include Novamyl available from Novozymes, Denmark or G4 or G+ enzymes from Dupont, Denmark.
  • Novamyl One example of an ⁇ -amylase which is particularly useful with the present invention is Novamyl.
  • the activity of Novamyl is for example described by Christophersen et al. (1998): "enzymatic characterization of Novamyl, a thermostable alpha-amylase".
  • the ⁇ -amylase may be an ⁇ -amylase from any useful organism, such as from Bacillus stearothermophilus.
  • the ⁇ -amylase may for example be an enzyme of SEQ ID NO: 1 or a functional homologue thereof sharing at least 70% sequence identity there with, for example at least 75%, such as at least 80%, for example at least 85%, such as at least 90%, for example at least 95%, such as at least 98% sequence identity therewith.
  • Said sequence identity is determined over the entire length of SEQ ID NO:1 .
  • Said functional homologue is an enzyme capable of hydrolyzing both internal (1 ⁇ 4)-a-D-glucosidic linkages in polysaccharides as well as hydrolyzing (1 ⁇ 4)-a-D-glucosidic linkages in polysaccharides so as to remove successive a-maltose residues from the non-reducing ends of polysaccharides.
  • the ⁇ -amylase may also just contain the active part of the enzyme of SEQ ID NO:1 .
  • amino acid 1 to 33 of SEQ ID NO:1 is a signal peptide.
  • the ⁇ -amylase to be used with the invention may also be amino acid 34 to 719 of SEQ ID NO:1 or a functional homologue thereof sharing at least 70%, for example at least 75%, such as at least 80%, for example at least 85%, such as at least 90%, for example at least 95%, such as at least 98% sequence identity with amino acid 34 to 719 of SEQ ID NO:1 over the entire length.
  • Said functional homologue is an enzyme capable of hydrolyzing both internal (1 ⁇ 4)-a-D-glucosidic linkages in polysaccharides as well as hydrolyzing (1 ⁇ 4)-a-D-glucosidic linkages in polysaccharides so as to remove successive ⁇ -maltose residues from the non-reducing ends of polysaccharides.
  • the a-amylase is a glucan 1 ,4-a- maltotetraohydrolase, which also is capable of hydrolysing internal (1 ⁇ 4)-a-D- glucosidic linkages in amylose or amylopectin.
  • Said glucan 1 ,4-a-maltotetraohydrolase may be derived from any useful organism, but in a preferred embodiment of the invention the glucan 1 ,4-a-maltotetraohydrolase is derived from Pseudomonas saccharophila.
  • the exo-amylase is Pseudomonas saccharophila maltotetraohydrolase of SEQ ID NO: 1 of international patent application WO2010/133644 or a variant thereof sharing at least 65% identity therewith.
  • Said variant preferably is capable of catalysing hydrolysis of (1 ⁇ 4)-a-D-glucosidic linkages in amylose or amylopectin to remove successive maltotetraose residues from the non- reducing chain ends and preferably shares at least 65%, more preferably at least 70%, even more preferably at least 75%, yet more preferably at least 80%, even more preferably at least 85%, yet more preferably 90% identity with SEQ ID NO: 1 of international patent application WO2010/133644.
  • Pseudomonas saccharophila maltotetraohydrolase to be used with the methods of the present invention are described in US patent applications US2005/037391 , US2005/1 12237, US2006/008888, US2007/141693 and
  • the variants of Pseudomonas saccharophila maltotetraohydrolase to be used with the methods of the present invention are any of the variants described in US patent applications US2005/037391 , US2005/1 12237, US2006/008888, US2007/141693 and US2009/202675 as well as in the section "Polypeptide variants of SEQ ID NO:1 on international patent application WO2010/133644.
  • Pilot-scale preparation of haze ingredient from barley starch 25 kg barley starch (obtained from Altia, Finland) was dispersed in 250 L demineralised water in a mash kettle at a temperature of 24°C. 25 mL of a commercial preparation of amylase (PDN 17/6, obtained from Biocatalysts, UK) was added. Partial sequence information indicates that this enzyme is an enzyme of SEQ ID NO:1 .
  • the temperature was then increased at a rate of 1 °C/minute to 66°C and kept at this level for 45 minutes.
  • the temperature was then increased to 90 °C, again at a rate of 1 °C/minute, and kept at this level for 60 minutes.
  • the temperature was then increased to 100°C, again at a rate of 1 °C/minute, and the mixture was boiled for 60 minutes. Throughout these steps, the mixture was stirred vigourously.
  • the contents of the mash kettle were transferred hot to another tank, taking care not to let the temperature drop below 80 °C at any time during transfer.
  • the mixture was then allowed to cool to 80 °C and left without stirring at this temperature for 20 hours.
  • the mixture separated into an opaque top phase and a milky bottom phase.
  • the top phase about 70% of the total volume, was then transferred to storage containers using a pump and allowed to cool to 5°C. During this stage, the top phase turned milky white.
  • the top phase was then left to retrograde at 5°C for at least 20 hours.
  • starch fragment particles providing a stable haze were separated from small sugars, larger starch fragments, and undigested starch by step-wise precipitation with ethanol.
  • the retrograded top phase was attemperated to 22 °C.
  • 96% ethanol was added to obtain a final concentration of 28% ABV.
  • the mixture was then centrifuged twice, at 22 °C, for 15 minutes at 3000 xG. After each centrifugation, sediments were discarded.
  • the concentration of ethanol in the supernatant was then brought to 50% ABV by addition of more 96% ethanol, and the preparation was left for at least 20 hours at 22 °C. After this period, the almost clear supernatant was decanted off and discarded.
  • the remaining sediment was at first air-dried, then freeze-dried to remove remaining traces of ethanol, and finally ball-milled to a fine powder.
  • the recovery of haze ingredient from several individual mashings was 12-13%.
  • the purified, dried, and ball-milled haze ingredient was dispersed in water by boiling essentially as described in Example 3.
  • the dispersed haze ingredient was added to a regular lager beer of 5% ABV to obtain a final concentration of 1 g/L, 2 g/L, 4 g/L or 6 g/L and stored either 22 °C or 37 °C for more than 50 days, and the haze intensity was measured on a LabScat instrument from Sigrist at both 90 ° and 25° angle using light at 650 nm. The outcome is provided as EBC UNITs.
  • the results are shown in figures 1 A and 1 B.
  • a similar experiment was conducted with storage at 60 °C for 35 days, and also under those conditions the haze ingredient provided a stable haze.
  • Haze ingredient was prepared from barley starch essentially as described in Example 1 i.e. the ingredient was prepared using ethanol precipitation for the size separation.
  • Another haze ingredient was prepared from barley starch essentially as described in Example 4, i.e. the ingredient was prepared using centrifugation for the size separation.
  • Two more haze ingredients were prepared from maize starch and potato starch essentially as described in Example 3, i.e. the ingredients were prepared using ethanol precipitation for the size separation. All haze ingredients were freeze-dried and finally ball-milled to fine powders.
  • each of the four haze ingredients obtained as described above were dispersed in water by boiling essentially as described in Example 3, and diluted in water to obtain a final concentration of 2 g/L.
  • the samples were then stored at approx. 22 °C until next day, when the hydrodynamic diameters of the starch fragment particles were measured by Particle Analytical, Horsholm, Denmark.
  • the size distributions are shown in fig. 2A, 2B, 2C, and 2D. All four preparations contain starch fragment particles with hydrodynamic diameters in the range 0.03 ⁇ to 1 ⁇ . In addition the preparations also contain larger particles.
  • top phases and bottom phases were collected separately and allowed to retrograde at 8°C for 16 hours.
  • Haze ingredients were then purified by step-wise precipitations with ethanol at 28% ABV and 50% ABV, essentially as described in example 1 , from the retrograded top phases obtained from barley, wheat, maize, potato and pea starch, and from retrograded bottom phase obtained from pea starch.
  • the recoveries are listed in table 2.
  • Starches from barley, wheat, maize, and pea were mashed with amylase PDN 17/6 essentially as described in example 3. After boiling, the mashes were immediately cooled to 8°C and kept at this temperature for 16 hours. The mashes were then attemperated to 22 °C and centrifuged multiple times to remove larger starch fragments. Centrifugations were performed three times for 10 minutes at 3000 G, once for 20 minutes at 3000 G, and once for 20 minutes at 4500 G. After each centrifugation step, precipitated material was discarded. After these five centrifugations, 25-mL aliquots of the cloudy supernatants were added to regular lager beer (5% ABV) in 250-mL bottles.
  • Example 5 All samples were then stored at 22 °C for 100 days in order to test haze intensity and haze stability.
  • the haze intensity was determined as described in Example 3.
  • the haze intensity varied among the preparations, but all preparations gave a stable haze. Results are shown in figure 4.
  • Example 5 Example 5
  • 2,5 g haze ingredient prepared from barley starch essentially as described in Example 1 , was dissolved in 50 mL water by boiling for 20 minutes. 10-mL aliquots were then added to either apple juice or a non-alcoholic malt beverage in 250-mL bottles. The final concentration of ingredient in the beverages was thus 2 g/L in all bottles. Samples were stored at 22 or 37 °C for almost 60 days, and haze was measured on a LabScat instrument from Sigrist, at both 90° and 25° angle at 650 nm several times during storage. The haze ingredient gave a stable haze in these beverages throughout the storage period. Results are shown in figure 5 A and B.
  • Example 6 Haze ingredients were prepared from barley starch and maize starch as described in Example 3. The molecular weights of the starch fragments of the haze ingredient were then determined using asymmetric flow field-flow fractionation, multi angle laser light scattering, and refractive index detection set up to measurement of starch. Molar mass can be obtained by MALLS, combined with detection by refractive index for concentration measurements, by applying the Rayleigh-Debye approximation:
  • R(9) is the excess Rayleigh scattering over and above that of the solvent due to a solute of concentration c, for a slice i of the fractionated sample.
  • K * is an instrumental constant dependent on the wavelength and the refractive index increment (dn/dc) of the solute in the particular solvent.
  • M is the molar mass for the solute.
  • ⁇ ( ⁇ ) is the scattering function that describes the angular dependence of the scattered light intensity.
  • a 2 is the second virial coefficient and captures non-ideality due to solvent- solute interactions.
  • the number average molecular weight (Mn) and weight average molecular weight (Mw) is derived by measuring R(9) at multiple angles for each slice i of the fractionated sample: V r- M-
  • the concentration of each slice, q is conveniently measured by Rl detection.
  • the dried haze ingredients prepared from barley starch and maize starch as described in Example 3 were dispersed in the eluent (50mM NaN0 3 ) at concentrations 2.5 mg/ml and heated at 100 °C for 30 min. and subsequently centrifuged at 7000 rpm for 5 min. 1 0-50 ul aliquots of the supernatants were analysed on an AF4-MALLS system from Wyatt Technology.
  • AF4 flow control was maintained with a Wyatt Eclipse AF4 with Frit Inlet channel, which was in the thermos temperature control for Eclipse (kept at 60 °C).
  • the spacer for the Frit Inlet channel was the model 490W.
  • a regenerated cellulose membrane from Millipore was used (MWCO 1 0 kDa). Detection was accomplished with a Wyatt DAWN EOS 1 8-angle MALS (50 °C) and an Optilab T-rEX refractive index detector (Rl) (40 ⁇ ).
  • the flow gradient was set as indicated in Table 3.
  • the MALLS detector was calibrated with toluene. Data were collected and processed with ASTRA software (V6.1 .2.84). ). Degree of polynomial function was not used in the Zimm fit method for all the samples.
  • a refractive index increment (dn/dc) of 0, 1454 ml/g and a second virial coefficient (A 2 ) of 10 ⁇ 4 mol » ml/g 2 were used for all the starch samples in the processing of the data.
  • the results are provided in Table 4 below and in figure 6.
  • Figure 6 shows the molecular weight as a function of eluted volume (left hand axis and dotted line), as well as the relative amount as a function of eluted volume (right hand axis and normal line).
  • the molecular weight range of the samples (barley in figure 6A and maize in figure 6B) can be found from the analysis and the weight average and number average calculated.
  • Table 4 shows the molecular weight of a fractionation containing at least 60% of the sample.
  • Example 7 Haze ingredients were prepared from starches from barley, maize, potato, and pea as described in Example 3 and analysed by NMR. The samples were dispersed in D20. For each ingredient, a proton spectrum was obtained on a Bruker Avance 800 instrument, using 5 mm tubes and a run temperature of 37°C. The average ratios between reducing ends, oc-1 ,4 glycosidic linkages, and oc-1 ,6 glycosidic linkages in the haze ingredients were determined by integration of the NMR signals. Figure 7 shows the proton spectrum obtained for haze ingredient prepared from barley starch. Table 5 below summarises the average ratios between reducing ends, oc-1 ,4 glycosidic linkages, and oc-1 ,6 glycosidic linkages calculated for various haze ingredients. Table 5
  • oc-1 , 4 red. ends oc-1 ,6 : red. ends oc-1 ,4 : oc-1 ,6

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Abstract

L'invention concerne un procédé de production d'ingrédients produisant un effet de turbidité à utiliser pour la production de boissons troubles. L'invention concerne également des procédés pour la production de boissons troubles. Les procédés consistent à traiter de l'amidon avec une α-amylase pouvant hydrolyser des liaisons (1→4)-α glucosidiques internes de l'amidon, puis à séparer les particules de fragment d'amidon en fonction de leur taille.
PCT/DK2014/050420 2013-12-09 2014-12-09 Turbidité stable pour boissons WO2015086027A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019207063A1 (fr) * 2018-04-25 2019-10-31 Carlsberg A/S Boissons à base d'orge
BE1026176B1 (de) * 2018-08-21 2019-11-04 György Pintz Bierkomposition mit verbesserten gesundheitsschützenden Wirkung

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US4187326A (en) * 1977-10-25 1980-02-05 General Foods Corporation Dry beverage mix containing a clouding agent
US4349577A (en) * 1980-10-06 1982-09-14 National Starch And Chemical Corp. Starch-protein clouds and preclouds
US4971828A (en) * 1989-07-13 1990-11-20 American Maize-Products Company Beverage clouding agent
US5089171A (en) * 1988-10-14 1992-02-18 National Starch And Chemical Investment Holding Corporation Partially debranched starch clouds
EP0553368A1 (fr) * 1992-01-27 1993-08-04 National Starch and Chemical Investment Holding Corporation Amidon partiellement déramifié comme agent opacifiant
US5482560A (en) 1994-07-27 1996-01-09 American Maize Technology, Inc. Beta-limit dextrin from dull waxy starch
US20050037391A1 (en) 2003-06-13 2005-02-17 Kragh Karsten Mathias Polypeptide
US20050112237A1 (en) 2003-07-07 2005-05-26 Kragh Karsten M. Polypeptide
US20060008888A1 (en) 2004-07-07 2006-01-12 Kragh Karsten M Polypeptide
US20070141693A1 (en) 2005-07-07 2007-06-21 Berg Casper T Polypeptide
US20090202675A1 (en) 2006-06-19 2009-08-13 Patrick Maria Franciscus Derkx Polypeptide
WO2010133644A2 (fr) 2009-05-19 2010-11-25 Danisco A/S Polypeptides amylase

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US4187326A (en) * 1977-10-25 1980-02-05 General Foods Corporation Dry beverage mix containing a clouding agent
US4349577A (en) * 1980-10-06 1982-09-14 National Starch And Chemical Corp. Starch-protein clouds and preclouds
US5089171A (en) * 1988-10-14 1992-02-18 National Starch And Chemical Investment Holding Corporation Partially debranched starch clouds
US4971828A (en) * 1989-07-13 1990-11-20 American Maize-Products Company Beverage clouding agent
EP0553368A1 (fr) * 1992-01-27 1993-08-04 National Starch and Chemical Investment Holding Corporation Amidon partiellement déramifié comme agent opacifiant
US5482560A (en) 1994-07-27 1996-01-09 American Maize Technology, Inc. Beta-limit dextrin from dull waxy starch
US20050037391A1 (en) 2003-06-13 2005-02-17 Kragh Karsten Mathias Polypeptide
US20050112237A1 (en) 2003-07-07 2005-05-26 Kragh Karsten M. Polypeptide
US20060008888A1 (en) 2004-07-07 2006-01-12 Kragh Karsten M Polypeptide
US20070141693A1 (en) 2005-07-07 2007-06-21 Berg Casper T Polypeptide
US20090202675A1 (en) 2006-06-19 2009-08-13 Patrick Maria Franciscus Derkx Polypeptide
WO2010133644A2 (fr) 2009-05-19 2010-11-25 Danisco A/S Polypeptides amylase

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CHRISTOPHERSEN ET AL.: "enzymatic characterization of Novamyl, a thermostable alpha-amylase", STARCH/STARKE, vol. 50, no. 1, 1998, pages 39 - 45

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019207063A1 (fr) * 2018-04-25 2019-10-31 Carlsberg A/S Boissons à base d'orge
CN112118745A (zh) * 2018-04-25 2020-12-22 嘉士伯有限公司 基于大麦的饮料
BE1026176B1 (de) * 2018-08-21 2019-11-04 György Pintz Bierkomposition mit verbesserten gesundheitsschützenden Wirkung

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