WO2022018188A1 - Fibre de carotte colorée activée - Google Patents
Fibre de carotte colorée activée Download PDFInfo
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- WO2022018188A1 WO2022018188A1 PCT/EP2021/070488 EP2021070488W WO2022018188A1 WO 2022018188 A1 WO2022018188 A1 WO 2022018188A1 EP 2021070488 W EP2021070488 W EP 2021070488W WO 2022018188 A1 WO2022018188 A1 WO 2022018188A1
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- carrot
- dye
- fiber
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/09—Mashed or comminuted products, e.g. pulp, purée, sauce, or products made therefrom, e.g. snacks
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/10—Products from fruits or vegetables; Preparation or treatment thereof of tuberous or like starch containing root crops
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/262—Cellulose; Derivatives thereof, e.g. ethers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
- A23L33/22—Comminuted fibrous parts of plants, e.g. bagasse or pulp
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
- A23L33/24—Cellulose or derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
- A23L5/44—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives using carotenoids or xanthophylls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H99/00—Subject matter not provided for in other groups of this subclass, e.g. flours, kernels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/06—Pectin; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L99/00—Compositions of natural macromolecular compounds or of derivatives thereof not provided for in groups C08L89/00 - C08L97/00
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
Definitions
- the present invention relates to an activated colored carrot fiber and a process for its production.
- the invention also relates to the use of the activated colored carrot fiber as a thickening or structuring agent in various industrial products.
- the invention relates to a food product, feed product, dietary supplement, beverage, cosmetic product, pharmaceutical product or medicinal product which has been produced using the activated colored carrot fiber according to the invention.
- the invention relates to a method for coloring activated fruit fibers, in particular citrus, apple or carrot fibers.
- Dietary fibers are largely indigestible food components, mostly carbohydrates, which are mainly found in plant foods.
- dietary fiber is divided into water-soluble dietary fiber such as pectin and water-insoluble dietary fiber such as cellulose. Fiber is considered an important part of human nutrition.
- the consumption of dietary fiber is considered to be good for your health.
- the water-soluble fiber in the diet increases the volume of the food without significantly increasing the energy content. If they are not sufficiently swollen before ingestion, they absorb more water in the stomach. The resulting increase in volume leads to an increase in the feeling of satiety.
- dietary fibers extend the retention time of the chyme in the intestine or stomach. Water-soluble dietary fibers such as pectin bind bile acids from the cholesterol metabolism in the intestine and thus lead to a reduction in cholesterol levels.
- carrot fibers represent a mixture of insoluble roughage such as cellulose and soluble roughage such as pectin and thus ideally result in the health-promoting spectrum of effects listed above. Carrot fibers can thus replace other unacceptable or even harmful additives in food and, as substances that are not E-classified, lead to simpler product labeling and thus to increased product acceptance. Since carrot fibers only contain a small amount of pectin, they only have a limited ability to texturize food to increase viscosity compared to functionalized citrus or apple fibers.
- the object of the present invention is to improve the prior art or to offer an alternative to it.
- the task at hand is a method for producing an activated colored carrot fiber, which comprises the following steps:
- step (c) contacting the wet material from step (a) or the hydrated dry material from step (b) with an extraction composition comprising a water-miscible organic solvent to extract coloring matter from the carrot-containing plant material, followed by incubation for at least 5 minutes and separating the colorant-containing liquid from the carrot-containing vegetable material to obtain an at least partially decolorized material;
- step (d) optionally enzymatically treating the deinked material from step (c) in aqueous suspension with cellulase and/or with pectin methyl esterase to obtain an enzymatically treated material; (e) washing the deinked material from step (c) or the enzymatically treated material from step (d) at least twice with a water-miscible organic solvent and then separating the washed material from the water-miscible organic solvent each time;
- step (f) drying the washed material from step (e) comprising normal pressure drying or vacuum drying, wherein the drying is carried out with addition of a dye-containing solution, to obtain the activated dyed carrot fiber.
- the production process according to the invention leads to colored carrot fibers with a large inner surface, which also increases the water-binding capacity and is associated with good viscosity formation.
- These fibers are activated fibers that have sufficient strength in an aqueous suspension so that no additional shearing forces are required in use in order for the user to obtain the optimum rheological properties such as viscosity or texturing.
- the colored carrot fibers produced by the process according to the invention have good rheological properties.
- the fibers of the invention can be easily rehydrated and the advantageous rheological properties are retained even after rehydration.
- the production process according to the invention leads to colored carrot fibers which are largely tasteless and odorless and are therefore advantageous for use in the food sector.
- the aroma of the other ingredients is not masked and can therefore develop optimally.
- the dyeing process as part of the manufacturing process according to the invention leads to a surprisingly stable dyeing of the fibers.
- the colored activated carrot fibers show no significant signs of discoloration when incubated in a buffer system, even over a broad pH range from pH 2 to pH 9.
- the production process according to the invention allows controlled coloring of the activated carrot fibers, so that in addition to the natural color of the original carrot fibers, lighter or darker colored carrot fibers can also be produced depending on the intended use.
- the intrinsic colorants are broken down or removed from the carrot in the course of the process, so that essentially decolored carrot fibers result.
- the dyes are gently removed before the dye-critical production steps and can be added to produce a controlled-dyed fiber in the final drying step without the process-related fiber activation being seriously impaired.
- the carrot fibers according to the invention are obtained from carrots and are therefore natural ingredients with well-known positive properties.
- Vegetable processing residues such as carrot pomace can be used as raw material in the production process according to the invention. These processing residues are inexpensive, plentiful and provide a sustainable and environmentally sound source of the activated colored carrot fiber of the present invention.
- Carrot fibers are established and accepted in the food industry, so that corresponding compositions can be used immediately and internationally without a lengthy approval process.
- a carrot-containing plant material and preferably processing residues from carrots are used as the raw material.
- This carrot-containing plant material can be used on the one hand as dry material, for example in the form of dried carrot pomace.
- a dry material in the context of the invention is understood to mean a carrot-containing plant material which has less than 15%, preferably less than 10% and more preferably less than 8% moisture. The use of dried plant material allows production independent of the season.
- the carrot-containing plant matter In the event that the carrot-containing plant matter is in the form of dry matter, it must be hydrated by incubation with an aqueous liquid.
- the plant material forms a suspension of the carrot pieces or carrot particles in the aqueous solution.
- This suspension represents a suspension insofar as a heterogeneous mixture of substances is present here, consisting of a liquid and carrot particles (preferably finely) distributed therein. Since the suspension tends to sedimentation and phase separation, the particles are suitably kept in suspension by shaking or stirring. There is therefore no dispersion in which the particles are comminuted by mechanical action (shearing) in such a way that they are finely dispersed.
- the hydrated dry material is separated from the aqueous liquid by a solid-liquid separation. This is preferably done using a decanter. Alternative separation methods are a sieve drum, a separator or a press.
- the carrot-containing plant material is subjected to a dye extraction in step (c). Here it is brought into contact with a water-miscible organic solvent and incubated for a sufficient period of time. This primarily extracts the lipophilic carotenoids, which are the carrot’s coloring agents.
- An extensive class of naturally occurring fat-soluble pigments is referred to as carotenoids, which chemically have a tetraterpene as their basic structure in common. Their system of conjugated double bonds absorbs short-wavelength light and, depending on the number, position and side chain in the carotenoid, gives it a yellowish to reddish hue.
- the now more than 800 known carotenoids are divided into carotenes and the oxygen-containing xanthophylls.
- Carotenoids belong to the isoprenoids.
- the carrot contains numerous carotenoids, the most important carotenoids in decreasing concentration being: ß-carotene (lUPAC nomenclature: ß,ß-carotene), a-carotene (lUPAC nomenclature: b,e-carotene), lutein (lUPAC - Nomenclature: 4-[18-(4-Hydroxy-2,6,6-trimethyl-cyclohex-2-enyl)-3,7,12,16-tetramethyl-octadeca-1,3,5,7,9, 11,13,15,17-nonaenyl]-3,5,5-trimethyl-cyclohex-3-enol E 161b) and zeaxanthin.
- the plant material decolorized by extraction can be subjected to an enzymatic treatment in step (d).
- This enzymatic treatment involves de-esterification of the highly esterified pectin present in the carrot material by a pectin methyl esterase and/or partial degradation of the cellulose present in the carrot material by a cellulase.
- step (e) the decolorized material from step (c) or the decolorized enzymatically treated material from step (d) is washed several times, ie at least twice, with an organic solvent.
- This multi-stage washing with alcohol initially improves the functional fiber properties and thus contributes contributes decisively to the activation of the carrot fiber.
- disruptive accompanying substances are removed from the material, thus ensuring that the end product is sensorially neutral. This applies to both olfactory and gustatory substances.
- the drying from the alcoholic phase that takes place in step (f) is essential for the subsequent functional properties, since the fibers dry open-pored and result in good swelling and wetting properties that would not be present if they were dried from the aqueous phase, since the individual fibers then crust over hydrogen bonds.
- the dried fiber material produced by the process according to the invention is an activated carrot fiber, insofar as the result is an open-pore fiber with good swelling and wetting properties, which is also expressed in advantageous functional properties such as high viscosity, good water-binding capacity and particular strength.
- a dye-containing solution is added during drying so that the material firmly binds the added dye when the liquid is removed and is to a certain extent impregnated with the dye, so that after the end of drying step (f) an activated colored carrot fiber is present.
- a plant material containing carrots and preferably processing residues from carrots are used as the raw material or starting material.
- the expert can fall back on a wide variety of carrot materials.
- the carrot-containing plant material is selected from the group consisting of carrot pomace, carrot flour, carrot pomace flour, carrot semolina and carrot puree, it also being possible to use a mixture of the aforementioned materials.
- the use of carrot pomace, both in the form of dry pomace and in the form of moist pomace, has proven to be particularly advantageous.
- a “carrot-containing plant material” according to the invention is comminuted carrots, so that no whole carrots are used, but at least carrot grit, or even fine-particle carrots in the form of carrot flour.
- carrot pomace is defined as the comminuted solid residues resulting from carrot processing. Processing typically involves juicing.
- the carrot pomace initially occurs here as moist pomace. In order to achieve a pomace material with an improved shelf life, it is usually dried and can then be stored and processed as dry pomace.
- the dry material is rehydrated by being brought into contact with and incubated with an aqueous liquid and is thus prepared for the subsequent processing steps.
- the mixture of carrot dry material to be hydrated and aqueous liquid is also referred to below as aqueous incubation solution.
- the incubation with the aqueous liquid takes place at a temperature between 20°C and 70°C, advantageously at a temperature between 25°C and 65°C and particularly advantageously at a temperature between 30°C and 60°C. Elevated temperature in particular accelerates rehydration.
- the aqueous liquid used in the hydration can be an aqueous buffer or water.
- demineralized water is preferred.
- hydration is effected by incubation with the aqueous liquid for a period of from 10 minutes to 4 hours, advantageously for a period of from 20 minutes to 3 hours, and most advantageously for a period of from 30 minutes to 2 hours.
- the dry mass in the aqueous incubation solution is expediently between 0.25% by weight and 20% by weight, preferably between 0.5% by weight and 15% by weight, and particularly preferably between 1% by weight and 10% by weight.
- the hydration is advantageously carried out while stirring or shaking the aqueous suspension. This speeds up the hydration process and contributes to more even hydration.
- the hydrated dry material is separated from the aqueous liquid by a solid-liquid separation. This is preferably done using a decanter. Alternative separation methods are a sieve drum, a separator or a press.
- Step 1 First, the wet material from step (a) or the hydrated dry material from step (b) is brought into contact with an extraction composition.
- This extraction composition comprises a water-miscible organic solvent capable of extracting the carotenoid pigments from the plant material containing carrot.
- the wet material from step (a) or the hydrated dry material from step (b) is preferably in the form of a slurry or aqueous suspension. In an alternative embodiment, it can be present as a moist material, as is typically obtained after separation of the aqueous liquid after rehydration of a dry material.
- Step 2 The mixture is then incubated for at least 5 minutes to achieve sufficient extraction of the carotenoids.
- Step 3 The extraction step is completed by a separation step in which the colorant-containing extraction composition is separated as a liquid from the carrot-containing plant matter.
- the material thus decolorized is then further processed to produce the activated carrot fiber.
- the dye-containing liquid obtained can be used elsewhere or returned to the process to dye the fiber again during drying.
- the extraction composition within the scope of the invention is a composition which is liquid at room temperature and comprises a water-miscible organic solvent and preferably consists essentially of this solvent.
- a solvent here means at least one solvent, so that two, three or more water-miscible organic solvents can also be present.
- Water-miscible, thermally stable, volatile solvents containing only carbon, hydrogen and oxygen such as alcohols, ethers, esters, ketones and acetals, are particularly suitable for carrying out the process according to the invention.
- Ethanol, n-propanol, isopropanol, methyl ethyl ketone, 1,2-butanediol-1-methyl ether, 1,2-propanediol-1-n-propyl ether or acetone are preferably used.
- An organic solvent is referred to herein as "water-miscible” if it is in a 1:20 (v/v) mixture with water as a single-phase liquid.
- solvents which are at least 10% water-miscible, have a boiling point below 100° C. and/or have fewer than 10 carbon atoms.
- the organic water-miscible solvent is preferably an alcohol, advantageously selected from the group consisting of methanol, ethanol and isopropanol, and especially isopropanol.
- the incubation with the extraction composition is expediently carried out for a period of 5 minutes to 10 hours, preferably for a period of 15 minutes to 2 hours and particularly preferably for a period of 20 minutes to 40 minutes.
- Incubation with the extraction composition can be at a temperature of between 10°C and 70°C.
- temperatures of >20°C have proven to be particularly suitable, since the improvement in solubility that can be achieved with the organic solvent is even more pronounced at elevated temperatures; the upper limit of the process temperature is of course the boiling point of the solvent in question, but this is generally not reached in terms of process technology.
- the particularly suitable temperature range for the extraction is therefore between 20°C and 60°C and particularly preferably between 30°C and 50°C.
- the extraction conditions are expediently selected such that a +a* value of less than 14, preferably less than 5, more preferably less than 3 and particularly preferably less than 2 is achieved for the plant material to be decolorized in the L*a*b color space . This ensures that most of the dye has been removed and the fiber no longer has any significant red coloration.
- the dye extraction occurs at a pH of between 3.5 to 5.5, and preferably at a pH of between 4.0 to 5.0.
- the dry matter in the extraction batch can be between 3% by weight and 20% by weight, preferably between 4% by weight and 15% by weight, and particularly preferably between 5% by weight and 12% by weight.
- the proportion of the water-miscible organic solvent, which is preferably an alcohol, in the extraction composition is higher than 90% by volume, advantageously more than 95% by volume, particularly advantageously more than 98% by volume and in particular more than 99% by volume.
- the proportion of the water-miscible organic solvent, which is preferably an alcohol, in the extraction mixture is between 70 and 95% by volume, advantageously between 80 and 90% by volume and particularly advantageously between 83 and 88%.
- the dye extraction is preferably carried out while stirring or shaking the extraction batch.
- the separation of the dye-containing liquid, which is a mixture of water and the organic solvent, from the decolorized material takes place by means of a decanter or a separator.
- the carrot material is processed further in the process as an extraction residue, i.e. either treated enzymatically or fed directly to a multi-stage washing process with an organic solvent.
- the carrot-containing plant material can be subjected to an enzymatic treatment with a pectin methyl esterase in step (d) of the method, which is also synonymously referred to as “enzymatic de-esterification”.
- the pectin material contained in the plant fiber is typically high methylester pectin.
- a pectin according to the application is defined as a vegetable polysaccharide which, as a polyuronide, essentially consists of ⁇ -1,4-glycosidically linked D-galacturonic acid units.
- the galacturonic acid units are partially esterified with methanol.
- the degree of esterification describes the percentage of carboxyl groups in the Galacturonic acid units of pectin, which are present in esterified form, eg as methyl ester.
- a highly esterified pectin is a pectin which has a degree of esterification of at least 50%.
- the degree of esterification describes the percentage of the carboxyl groups in the galacturonic acid units of the pectin which are present in the esterified form, e.g. as methyl ester.
- the degree of esterification can be determined using the method according to JECFA (Monograph 19-2016, Joint FAO/WHO Expert Committee on Food Additives).
- the methyl esters of the galacturonic acid groups in the pectin are hydrolyzed by the pectin methyl esterase to form poly-galacturonic acid and methanol.
- the resulting low methylester pectins can form a gel in the presence of polyvalent cations even without sugar and can also be used in a wide pH range.
- a pectin methylesterase (abbreviation: PME, EC 3.1.1.11, also: pectin demethoxylase, pectin methoxylase) is a common enzyme in the cell wall of all higher plants and some bacteria and fungi, which splits the methyl ester of pectins and thereby forms poly-galacturonic acid and methanol releases.
- PME has been isolated in many isoforms, all of which can be used for enzymatic deesterification according to the invention. Many isoforms of PME have been isolated from plant-pathogenic fungi such as Aspergillus foetidus and Phytophthora infestans as well as from higher plants such as tomatoes, potatoes and oranges.
- the fungal PME develop the optimum activity between pH 2.5 and 5.5, while the plant PME exhibit pH optima between pH 5 and 8.
- the molecular weight is between 33,000 and 45,000.
- the enzyme is present as a monomer and is glycosylated.
- the Kiu value is between 11 and 40 mM pectin for fungal PME and 4-22 mM pectin for plant PME.
- the commercially available PME preparations are obtained either from the supernatants of the fungal mycelium cultures or, in the case of plants, from fruits (orange and lemon peels, tomatoes).
- the pectin methylesterases that are preferably used have an optimum pH between 2 and 5 and an optimum temperature of 30 to 50°C, with significant enzyme activity already being observed from 15°C, depending on the enzyme.
- At least one pectin methyl esterase (EC 3.1.1.11) is added to the aqueous suspension for enzymatic deesterification.
- exactly one isoform of a PME is added to the suspension.
- a mixture of different isoforms can also be used.
- the duration of the incubation with the pectin methylesterase is advantageously between one hour and 10 hours, particularly advantageously between 2 hours and 5 hours.
- the pectin methyl esterase is preferably added to the aqueous suspension in such a way that a total PME activity of 1000 to 10,000 units/l, advantageously of 3000 to 7500 units/l, and particularly advantageously of 4000 to 6000 units/l results.
- total PME activity may be 1200, 1400, 1600, 1800, 2000, 2200, 2400, 2600, 2800, 3000, 3200, 3400, 3600, 3800, 4000, 4200, 4400, 4600, 4800, 5000, 5000, 5000, 5600, 5800, 6000, 6200, 6400, 6600, 6800, 7000, 7200 or 7400 units/L.
- the person skilled in the art will adapt the temperature to the PME isoform(s) used.
- the enzymatic treatment is carried out at a temperature of between 10°C and 70°C, preferably between 20°C and 60°C and most preferably between 30°C and 50°C.
- the person skilled in the art will set the optimum pH value for the de-esterification, depending on the pectin methyl esterase used in each case.
- a pH of between 3.5 and 5.5 is preferred here, and particularly preferably between 4.0 and 5.0.
- the pH is adjusted before the enzymatic deesterification by adding an acid or a buffer system working in an acidic environment.
- an acidic buffer solution known to him.
- an organic acid such as citric acid can be used.
- a mineral acid can also be used. Examples which may be mentioned are: sulfuric acid, hydrochloric acid, nitric acid or sulphurous acid. Sulfuric acid is preferably used.
- the solids content of the aqueous suspension must not be too high and advantageously be less than 10% by weight. In one embodiment, the dry matter content is between 0.5% by weight and 6% by weight, preferably between 1% by weight and 4% by weight, and particularly preferably between 2% by weight and 3% by weight.
- the enzymatic deesterification can be carried out while stirring or shaking the aqueous suspension, care being taken that the enzyme does not foam. This is preferably done in a continuous manner to keep the particles in suspension in suspension.
- a suspension is a heterogeneous mixture of substances consisting of a liquid and solids (particles of raw material) finely distributed therein. Since the suspension tends to sedimentation and phase separation, the particles are suitably kept in suspension by shaking or stirring. There is therefore no dispersion in which the particles are comminuted by mechanical action (shearing) in such a way that they are finely dispersed.
- the carrot-containing plant material can be subjected to an enzymatic treatment with a cellulase in step (c) of the method, which is also synonymously referred to as “enzymatic cellulose hydrolysis”.
- a cellulase is an enzyme capable of cleaving the ⁇ -1,4-glycosidic bond of cellulose, releasing glucose.
- Carrot material consists largely of cellulose, which is accordingly fragmented by the cellulase treatment. It has been found that the cellulase treatment surprisingly improves carrot fiber functionality in terms of water binding and viscosity build.
- the group of cellulases consists of three different types of enzymes, the interaction of which enables efficient digestion of the huge cellulose molecules (3000 - 15000 linked glucose molecules): Endoglucanases (EC 3.2.1.4) split cellulose into larger sections.
- Endoglucanases the first type of enzyme, are the only ones that can work within the cellulose chains, but only within what are known as amorphous areas, where the cellulose molecules lie in a disordered manner relative to one another and therefore do not build up any crystalline areas. As a result, they create a larger number of chain ends.
- exoglucanases EC 3.2.1.91
- exoglucanases EC 3.2.1.91
- the molecules of the third enzyme type cellobiase or ß-glucosidase (EC 3.2.1.21) can thus work simultaneously again and, at the end of the decomposition process, finally hydrolyze the ß-glycosidic connection between the two glucose molecules of cellobiose and thus release two glucose molecules.
- Cellulase is added to the aqueous suspension for the enzymatic cellulose hydrolysis.
- exactly one cellulase enzyme type can be added, ie either an endoglucanase (EC 3.2.1.4), an exoglucanase (EC 3.2.1.91) or a ⁇ -glucosidase (EC 3.2.1.21).
- two or more preferably all three cellulase enzyme types are used.
- the cellulase treatment expediently only leads to a partial hydrolysis of the cellulose present in the carrot pulp. Excessive hydrolysis leads to irreversible degradation of the cellulose in the fiber material, which has a negative effect on the fiber functionality.
- the aqueous suspension in the enzymatic cellulose hydrolysis expediently contains the cellulase or the cellulase mixture with a total activity of 100 to 3000 units/l, advantageously 150 to 2000 units/l, furthermore advantageously 200 to 1000 units/l, and especially advantageously from 250 to 400 units/L.
- the total cellulase activity can be, for example, 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850, 900, 950, 1000, 1200, 1400, 1600, 1800, 2000, 2200, 2400, 2600, 2800 or 3000 units/L.
- the incubation with cellulase in the aqueous suspension takes place for a period of 30 minutes to 4 hours and preferably of 1 to 3 hours.
- the person skilled in the art will adapt the temperature to the cellulase used.
- the cellulose hydrolysis occurs at a temperature of between 30°C and 80°C, preferably between 35°C and 75°C and most preferably between 40°C and 70°C.
- the person skilled in the art will set the optimal pH value for the cellulose hydrolysis, depending on the particular cellulase used.
- a pH of between 3.0 and 7.0 and particularly preferably of between 3.5 and 6.0 is preferably provided here.
- the pH is adjusted before the enzymatic cellulose hydrolysis by adding an acid or a buffer system working in an acidic medium.
- an acid or acidic buffer solution known to him.
- an organic acid such as citric acid can be used.
- a mineral acid can also be used. Examples which may be mentioned are: sulfuric acid, hydrochloric acid, nitric acid or sulphurous acid. Sulfuric acid is preferably used.
- the dry matter content of the aqueous suspension must not be too high and should advantageously be less than 10% by weight.
- the dry matter content is between 0.5% by weight and 6% by weight, preferably between 1% by weight and 4% by weight, and particularly preferably between 2% by weight and 3% by weight.
- the enzymatic cellulose hydrolysis can be carried out while stirring or shaking the aqueous suspension, care being taken to ensure that the enzyme does not foam. This is preferably done in a continuous manner to keep the particles in suspension in suspension.
- a suspension is a heterogeneous mixture of substances consisting of a liquid and solids (particles of raw material) finely distributed therein. Since the suspension tends to sedimentation and phase separation, the particles are suitably kept in suspension by shaking or stirring. There is therefore no dispersion in which the particles are comminuted by mechanical action (shearing) in such a way that they are finely dispersed.
- the carrot-containing plant material can be enzymatically treated with either pectin methyl esterase or alternatively with cellulase.
- the carrot-containing plant material is enzymatically treated with both pectin methyl esterase and cellulase.
- the enzymatic treatment with cellulase and pectin methylesterase can be carried out simultaneously or sequentially.
- step (e) a washing step then takes place, which is carried out with an organic solvent.
- the organic solvent is advantageously an alcohol, which can preferably be selected from the group consisting of methanol, ethanol and isopropanol. Isopropanol is particularly preferably used here.
- the washing step suitably takes place at a temperature between 40°C and 75°C, preferably between 50°C and 70°C and particularly preferably between 60°C and 65°C.
- the period of contacting with the organic solvent is advantageously for a period of between 60 minutes and 10 hours and preferably between 2 hours and 8 hours.
- Each organic solvent washing step involves contacting the material with the organic solvent for a specified period of time followed by separating the material from the organic solvent.
- a decanter or a press is preferably used for this separation.
- the dry mass in the washing solution is advantageously between 0.5% by weight and 15% by weight, preferably between 1.0% by weight and 10% by weight, and particularly preferably between 1.5% by weight. % and 5.0% by weight.
- the washing with the organic solvent is preferably carried out with mechanical agitation of the washing mixture.
- the washing is preferably carried out in a tank with an agitator.
- a device for making the suspension more uniform is advantageously used.
- This device is preferably a toothed ring disperser.
- the washing with the organic solvent takes place in a countercurrent process.
- washing with the organic solvent involves partial neutralization by adding Na or K salts, NaOH or KOH.
- decolorization of the material can also be carried out.
- This decolorization can be done by adding one or more oxidizing agents.
- the oxidizing agents chlorine dioxide and hydrogen peroxide, which can be used alone or in combination, should be mentioned here as examples.
- the final concentration of the organic solvent in the solution increases with each washing step.
- This incrementally increasing proportion of organic solvent reduces the proportion of water in the fiber material in a controlled manner, so that the rheological properties of the fibers are retained in the subsequent steps for solvent removal and drying and the activated fiber structure does not collapse.
- the final concentration of the organic solvent is preferably between 60 and 70% by volume in the first washing step, between 70 and 85% by volume in the second washing step and between 80 and 90% by volume in an optional third washing step.
- step (f) the washed material from step (e) is dried, in one embodiment drying comprising vacuum drying and preferably consisting of vacuum drying.
- vacuum drying the washed material is exposed to a negative pressure as drying material, which reduces the boiling point and thus leads to evaporation of the water even at low temperatures.
- the heat of vaporization continuously withdrawn from the material to be dried is suitably fed from the outside until the temperature is constant.
- Vacuum drying has the effect of lowering the equilibrium vapor pressure, which favors capillary transport. This has proven to be particularly advantageous for the present carrot fiber material, since the activated, open fiber structures and thus the rheological properties resulting therefrom are retained.
- the vacuum drying preferably takes place at a vacuum of less than 400 mbar, preferably of less than 300 mbar, more preferably less than 250 mbar and particularly preferably less than 200 mbar.
- step (f) can be carried out at a jacket temperature of between 40°C and 100°C, preferably between 50°C and 90°C and more preferably between 60°C and 80°C. After drying, the product is expediently cooled to room temperature.
- the drying in step (f) comprises drying under atmospheric pressure.
- suitable drying methods are fluidized bed drying, moving bed drying, belt dryers, drum dryers or paddle dryers.
- Fluid bed drying is particularly preferred here. This has the advantage that the product is dried loosely, which simplifies an optional subsequent grinding step.
- this type of drying avoids damage to the product due to local overheating thanks to the easily adjustable heat input.
- step (f) can be carried out at a temperature of between 50°C and 130°C, preferably between 60°C and 120°C and particularly preferably between 70°C and 110°C. After drying, the product is expediently cooled to room temperature.
- the drying step according to the invention is characterized in that the dissolved dye is supplied to the activated fibers and the fiber is impregnated with the dye as a result of the drying of the dye solution on the fiber that has not yet dried completely.
- the functionality of the fiber is essentially retained when a dye is added as part of fiber drying. The activation state of the fiber is not seriously affected.
- the dye-containing solution meets a partially dried or moist fiber material, which on the one hand has good absorbency for the dye-containing solution and on the other hand, as a material that has not yet dried completely, the open fiber structure does not collapse due to the lack of wetting.
- the fiber material preferably has a moisture content of more than 80%, preferably more than 85%, particularly preferably more than 90% and particularly preferably between 90 and 95%.
- the dye-containing solution is a carotenoid-containing solution. These represent the fruit's own color class of the carrot and can give the carrot its original appearance again. According to the invention, it has proven to be particularly suitable if this dye-containing solution is the dye solution extracted in step (c) or is derived from it.
- non-carrot carotenoids can also be used or added to the colorant solution extracted from carrots.
- Other possible carotenoids are annatto (main components: bixin, norbixin), paprika extract (main components: capsanthin, capsorubin), lycopene and beta-apo-8'-carotenal (E 160 a).
- dyes other than the carotenoids disclosed above are also used. These are preferably soluble in a water-miscible organic solvent and are approved as a food coloring. Without claiming to be complete, the following are mentioned here as examples: Allura red AC (E 129), amaranth (E 123), anthocyanins (E 163), azorubine (E 122), betanine (E 162), brown HAT (E 155), brilliant blue FCF ( E 133), brilliant black BN (E 151), canthaxanthin (E 161), quinoline yellow (E 104), chlorophyll (E 140), cochineal red A (E 124), curcumin (E 100), erythrosine (E 127), sunset yellow S (E 110), green S (E 142), indigo carmine (E 132), cochineal (E 120), copper-containing complexes of chlorophylls and chlorophyllins (E 141), lithol rubin BK (E 180),
- the substance class of “coloring foods” should also belong to the dyes.
- These are lipophilic plant extracts and/or concentrates from vegetables, such as carrots, paprika, spinach or apples, which have a coloring effect and can therefore also be used as part of a dye-containing solution within the scope of the method according to the invention.
- mixtures of dyes can also be used.
- an apple extract containing polyphenols can be used, which leads to a dark brown coloration in a concentrated form.
- Such an extract has the advantage that it is stable in storage, does not crystallize and is obtained from apples and, depending on the extract, also contains the flavorings of the apple, so that the fiber can be colored and its taste adapted.
- Such an extract is for example commercially available under the name “Herbarom®” (Herbrasih & Fox, Neuenbürg, Germany).
- a "dye-containing solution” is defined as a liquid in which the dye or dyes are in dissolved form. It is therefore not a suspension or dispersion of pigment particles in a liquid. A dissolved dye is necessary for a homogeneous, permanent and activity-retaining dyeing of the fibres.
- a dye solution derived therefrom is understood as meaning a solution which has been chemically and/or physically treated starting from the dye solution obtained in step (c).
- Possible physical treatment methods are concentration, dilution or filtration.
- Possible chemical treatment methods are oxidation or reduction of the dyes.
- the addition of further dyes or the targeted extraction of dyes from a mixture also falls under the derivation of the dye solution according to the invention.
- a carotenoid-containing solution as the dye-containing solution, which is a concentrate of the dye solution extracted in step (c) of the process according to the invention. This represents an ecologically and economically advantageous recycling step and the dye has also been freshly isolated and is therefore of optimal quality.
- the dye-containing solution is expediently based on a solvent which is a water-miscible organic solvent.
- the organic solvent which is preferably a water-miscible organic solvent and particularly preferably an alcohol, is in the dye-containing solution in a concentration of 70 to 95% by volume, preferably between 80 and 90% by volume and particularly preferably between 83 and 87% by volume in the dye-containing solution.
- the dye-containing solution consists essentially of an organic solvent, in the sense that it represents at least 95% by volume of the solvent.
- the dye-containing solution particularly advantageously consists of an organic solvent.
- a solvent here means at least one solvent, so that two, three or more water-miscible organic solvents can also be present.
- Water-miscible, thermally stable, volatile solvents containing only carbon, hydrogen and oxygen, such as alcohols, ethers, esters, ketones and acetals, are particularly suitable for carrying out the process according to the invention.
- Ethanol, n-propanol, isopropanol, methyl ethyl ketone, 1,2-butanediol-1-methyl ether, 1,2-propanediol-1-n-propyl ether or acetone are preferably used.
- An organic solvent is referred to herein as “water-miscible” when it is in a 1:20 (v/v) mixture with water as a single-phase liquid.
- solvents which are at least 10% water-miscible, have a boiling point below 100° C. and/or have fewer than 10 carbon atoms.
- the organic water-miscible solvent is preferably an alcohol, advantageously selected from the group consisting of methanol, ethanol and isopropanol, and especially isopropanol.
- the degree of staining can be set in a targeted manner in a simple manner by the ratio of liquid containing dye to fiber material. It has proven particularly suitable here if the dye-containing solution, which is preferably a carotenoid-containing solution, is added in a weight ratio of between 4:1 and 1:2.5, based on the material to be colored.
- the dye-containing solution which is preferably a carotenoid-containing solution
- the dye-containing solution is added between two drying stages in such a way that remoistening of the material to be dyed results.
- the dye-containing solution encounters a partially dried fiber material which, on the one hand, has good absorbency for the dye-containing solution and, on the other hand, as a material that has not yet dried through, does not show any collapse of the open fiber structure due to rewetting.
- vacuum drying which can be carried out as an alternative, the dye-containing solution can be added before or during vacuum drying. Addition before vacuum drying is preferred here.
- the method additionally comprises a comminuting, grinding or screening step.
- a comminuting, grinding or screening step This is advantageously designed in such a way that, as a result, 90% of the particles have a particle size of less than 400 ⁇ m, preferably a particle size of less than 350 ⁇ m and in particular a particle size of less than 300 ⁇ m. With this particle size, the fiber is easy to disperse and shows an optimal swelling capacity.
- the invention provides an activated colored carrot fiber obtained or obtainable by the production process according to the invention.
- the invention provides an activated colored carrot fiber which, due to the activation, has advantageous properties, especially with regard to rheological parameters such as yield point, dynamic Weissenberg number, strength, water binding capacity and viscosity.
- the fiber also qualifies for a wide range of uses in the manufacture of food and non-food products in terms of moisture, grain size and brightness value.
- This activated colored carrot fiber according to the third aspect of the invention has one or more of the following properties:
- the activated colored carrot fiber has a yield point II (rotation) of between 15 and 30 Pa, advantageously between 17.5 and 27.5 Pa and particularly advantageously between 20 and 25 Pa.
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a yield point I (rotation) of between 15 and 30 Pa, advantageously between 17.5 and 27.5 Pa and particularly advantageously between 20 and 25 Pa.
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a yield point II (Cross Over) of between 20 and 35 Pa, advantageously of between 22.5 and 32.5 Pa and more advantageously between 25 and 30 Pa.
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a yield point I (Cross Over) of between 25 and 35 Pa, advantageously between 20 and 30 Pa and particularly advantageously between 22.5 and 27.5 Pa .
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a dynamic Weissenberg number of between 5 and 11 Pa, advantageously between 6 and 10 Pa and particularly advantageously between 7 and 9 Pa, in a 2.5% by weight aqueous suspension.
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a dynamic Weissenberg number of between 5 and 11 Pa, advantageously between 6 and 10 Pa and particularly advantageously between 7 and 9 Pa.
- this activated colored carrot fiber is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a strength of between 320 g and 510 g, preferably between 350 g and 480 g and particularly preferably between 380 and 450 g in a 4% by weight aqueous suspension.
- the activated colored carrot fiber characterized by this strength is obtainable or obtained by the process of the present invention.
- the activated colored carrot fiber has a viscosity of 800 to 5000 mPas.
- the activated carrot fiber preferably has a viscosity of 800 to 4800 mPas, preferably 1000 to 4500 mPas, and particularly preferably 1200 to 4000 mPas, the activated colored carrot fiber being dispersed in water as a 2.5% by weight solution and the Viscosity is measured at a shear rate of 50 s_1 at 20°C.
- the activated colored carrot fiber can have a viscosity of 1100, 1200, 1300, 1400, 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500, 2600, 2700, 2800, 290000, 290000, 3100, 3200, 3300, 3400, 3500, 3600, 3700, 3800, 3900, 4000, 4100, 4200, 4300 or 4400 mPas.
- the activated colored carrot fiber characterized by this viscosity is obtainable or obtained by the manufacturing process described above.
- An activated carrot fiber with this high viscosity has the advantage that smaller amounts of fibers are required to thicken the end product. The fiber also creates a creamy texture.
- the activated colored carrot fiber advantageously has a water binding capacity of between 25 and 50 g/g, preferably between 30 and 45 g/g, particularly preferably between 32.5 and 42.5 g/g, and particularly preferably between 35 and 40 g /G.
- a water binding capacity of between 25 and 50 g/g, preferably between 30 and 45 g/g, particularly preferably between 32.5 and 42.5 g/g, and particularly preferably between 35 and 40 g /G.
- Such an advantageously high water-binding capacity leads to a high viscosity and, as a result, to lower fiber consumption with a creamy texture.
- the activated colored carrot fiber characterized by the water-binding capacity can preferably be obtained by the process according to the invention or is obtained thereby.
- the activated colored carrot fiber has a moisture content of less than 15%, preferably less than 10% and more preferably less than 8%.
- the activated colored carrot fiber characterized by this moisture is obtainable or obtained by the process of the present invention.
- the activated dyed carrot fiber has a pH of 3.5 to 5.0 and preferably 3.9 to 4.5 in 1.0% aqueous suspension.
- the activated colored carrot fiber characterized by this pH range is obtainable or obtained by the process of the invention.
- the activated colored carrot fiber advantageously has a particle size in which at least 90% of the particles are smaller than 400 ⁇ m, preferably smaller than 350 ⁇ m and in particular smaller than 300 ⁇ m.
- this grain size characterized activated colored carrot fiber obtainable by the process of the invention or is obtained thereby.
- the activated carrot fiber has a dietary fiber content of 80 to 95%.
- the activated carrot fiber characterized by this dietary fiber content is preferably obtainable or obtained by the process according to the invention.
- the invention relates to the use of the activated colored carrot fiber according to the invention as a thickening or structuring agent in a food product, a feed product, a drink or food supplement, a cosmetic product, a pharmaceutical product or a medicinal product.
- the invention relates to a mixture comprising the activated carrot fiber according to the invention and a soluble pectin, which is preferably a low ester pectin, a high ester pectin or a low ester amidated pectin, or a mixture thereof.
- the invention relates to a food product, a dietary supplement, a feed product, a drink, a cosmetic product, a pharmaceutical product or a medicinal product which has been produced using the activated colored carrot fiber according to the invention.
- the invention relates to a method for dyeing activated fruit fibers, in particular citrus, apple or carrot fibers, comprising the following steps:
- step D Contacting the suspension from step A or the wet activated fruit fiber from step B with the colorant-containing liquid from step C to obtain colored fruit fiber; E. Drying the colored fruit fibers under normal pressure or under vacuum to obtain activated colored fruit fibers.
- This aspect of the invention is based on the finding that moist or not thoroughly dried activated fruit fibers can be dyed in an efficient and lasting manner by bringing them into contact with a dye-containing solution, without the activation as a functionalization being impaired in any relevant way.
- a suspension of activated fruit fibers in a solution comprising water and a water-miscible organic solvent, which is preferably an alcohol, is provided. It is preferred here if the solution essentially consists of the water-miscible organic solvent or alcohol. In the presence of this solvent, the functionalization is preserved and the dye can stain the fiber without precipitating.
- the fiber can be provided as moist activated fruit fiber.
- the activated fruit fiber preferably has a moisture content of more than 80%, preferably more than 85%, particularly preferably more than 90% and particularly preferably between 90 and 95%.
- a dye-containing solution comprising a water-soluble organic solvent and at least one dissolved dye.
- a "dye-containing solution” is defined as a liquid in which the dye or dyes are in dissolved form. It is therefore not a suspension or dispersion of pigment particles in a liquid. A dissolved dye is necessary for a homogeneous, permanent and activity-retaining dyeing of the fibres.
- step C the suspension from step A or the moist activated fruit fiber from step B is brought into contact with the colorant-containing liquid from step C in order to color the activated fruit fibers.
- step D the colored fruit fibers are dried under normal pressure or under vacuum to form the activated colored fruit fibers.
- a "fruit fiber” according to the present invention is a plant fiber isolated from a fruit.
- the term “fruit” means all of the organs of a plant that emerge from a flower, including both the classic fruit fruits and fruit vegetables.
- the term “fruit” on its own also includes mixtures of fruits from two or more different plants, such as e.g. B. apple tree and cherry tree, so plant species, and / or mixtures of two or more different varieties of a fruit, such as two or more strawberry varieties.
- fruit fibers that can be replaced according to the invention are mentioned here by way of example: citrus fiber, apple fiber, carrot fiber, sugar beet fiber, oat fiber, bran fiber, barley fiber, wheat fiber, rye fiber, rice fiber, corn fiber, pea fiber, pear fiber, plum fiber, tomato fiber and psyllium fiber and sunflower fiber.
- Citrus fiber can be isolated from a wide variety of citrus fruits.
- Mandarin (Citrus reticulata), Clementine (Citrus c aurantium Clementine group, syn.: Citrus clementina), Satsuma (Citrus x aurantium Satsuma group, syn.: Citrus unshiu), Mangshan (Citrus mangshanensis), orange (Citrus c aurantium orange group, syn.: Citrus sinensis), bitter orange (Citrus c aurantium bitter orange group), bergamot (Citrus c limon bergamot group, syn.: Citrus bergamia), grapefruit (Citrus maxima) , grapefruit ( Citrus x aurantium grapefruit group, syn.: Citrus paradisi) pomelo ( Citrus c aurantium pomelo group), lime ( Citrus c aurantiifolia), common lime ( Citrus c aurantiifolia, syn.
- Apple fibers can be obtained from all cultivated apples (malus domesticus) known to those skilled in the art. Processing residues from apples can advantageously be used here as the starting material, namely apple peel, core casing, cores or pulp, or a combination thereof.
- apple pomace is used as the starting material, i.e. the pressed residue from apples, which typically also contain the above-mentioned components in addition to the peel.
- the dye-containing solution is a carotenoid-containing solution. Carotenoids represent the carrot's own class of pigments and can give the carrot its original appearance again. According to the invention, it has proven to be particularly suitable if this dye-containing solution is an extracted dye solution, as is generated in step (c) of the present method for producing activated carrot fibers.
- carotenoids are annatto (main components: bixin, norbixin), paprika extract (main components: capsanthin, capsorubin), lycopene and beta-apo-8'-carotenal (E 160 a).
- dyes other than the carotenoids disclosed above are also used. These are preferably soluble in a water-miscible organic solvent and are approved as a food coloring. Without claiming to be complete, the following are mentioned here as examples: Allura red AC (E 129), amaranth (E 123), anthocyanins (E 163), azorubine (E 122), betanine (E 162), brown HAT (E 155), brilliant blue FCF ( E 133), brilliant black BN (E 151), canthaxanthin (E 161), quinoline yellow (E 104), chlorophyll (E 140), cochineal red A (E 124), curcumin (E 100), erythrosine (E 127), sunset yellow S (E 110), green S (E 142), indigo carmine (E 132), cochineal (E 120), copper-containing complexes of chlorophylls and chlorophyllins (E 141), lithol rubin BK (E 180),
- the substance class of “coloring foods” should also belong to the dyes.
- These are lipophilic plant extracts and/or concentrates from vegetables, such as carrots, paprika, spinach or apples, which have a coloring effect and can therefore also be used as part of a dye-containing solution within the scope of the method according to the invention.
- mixtures of dyes can also be used.
- an apple extract containing polyphenols can be used, which leads to a dark brown coloration in a concentrated form.
- Such an extract has the advantage that it is stable in storage, does not crystallize and is obtained from apples and, depending on the extract, also contains the flavorings of the apple, so that the fiber can be colored and its taste adapted.
- Such an extract is for example commercially available under the name “Herbarom®” (Herbrasih & Fox, Neuenbürg, Germany).
- a "dye-containing solution” is defined as a liquid in which the dye or dyes are in dissolved form. So it is not a suspension or dispersion of pigment particles in a liquid. A dissolved dye is necessary for a homogeneous, permanent and activity-retaining dyeing of the fibres.
- a dye solution derived therefrom means a solution which is chemically and/or physically treated starting from the dye solution obtained in step (c) of the process for the production of activated colored carrot fibers.
- Possible physical treatment methods are concentration, dilution or filtration.
- Possible chemical treatment methods are oxidation or reduction of the dyes.
- the addition of further dyes or the targeted extraction of dyes from a mixture also falls under the derivation of the dye solution according to the invention.
- a carotenoid-containing solution as the coloring agent-containing solution, which is a concentrate of the coloring agent solution extracted in step (c) of the process according to the invention. This represents an ecologically and economically advantageous recycling step and the dye has also been freshly isolated and is therefore of optimal quality.
- the dye-containing solution is expediently based on a solvent which is a mixture comprising water and an organic solvent.
- the organic solvent which is preferably a water-miscible organic solvent and particularly preferably an alcohol, is in the dye-containing solution in a concentration of 70 to 95% by volume, preferably between 80 and 90% by volume and particularly preferably between 83 and 87% by volume in the dye-containing solution.
- the dye-containing solution consists essentially of an organic solvent, in the sense that it represents at least 95% by volume of the solvent.
- the dye-containing solution particularly advantageously consists of an organic solvent.
- a solvent here means at least one solvent, so that two, three or more water-miscible organic solvents can also be present.
- Water-miscible, thermally stable, volatile solvents containing only carbon, hydrogen and oxygen, such as alcohols, ethers, esters, ketones and acetals, are particularly suitable for carrying out the process according to the invention.
- Ethanol, n-propanol, isopropanol, methyl ethyl ketone, 1,2-butanediol-1-methyl ether, 1,2-propanediol-1-n-propyl ether or acetone are preferably used.
- An organic solvent is referred to herein as "water-miscible” if it is in a 1:20 (v/v) mixture with water as a single-phase liquid.
- solvents which are at least 10% water-miscible, have a boiling point below 100° C. and/or have fewer than 10 carbon atoms.
- the organic water-miscible solvent is preferably an alcohol, advantageously selected from the group consisting of methanol, ethanol and isopropanol. In a particularly preferred manner, it is isopropanol.
- the degree of staining can be set in a targeted manner in a simple manner by the ratio of liquid containing dye to fiber material. It has proven particularly suitable here if the dye-containing solution, which is preferably a carotenoid-containing solution, is added in a weight ratio of between 4:1 and 1:2.5, based on the material to be colored.
- the dye-containing solution which is preferably a carotenoid-containing solution
- the dye-containing solution is added between two drying stages in such a way that remoistening of the material to be dyed results.
- the dye-containing solution encounters a partially dried fiber material which, on the one hand, has good absorbency for the dye-containing solution and, on the other hand, as material that has not yet dried through, does not show any collapse of the open fiber structure as a result of rewetting.
- vacuum drying which can be carried out as an alternative, the dye-containing solution can be added before or during vacuum drying. Addition before vacuum drying is preferred here.
- step D the colored material from step C is dried, in one embodiment drying comprising vacuum drying and preferably consisting of vacuum drying.
- vacuum drying the washed material is exposed to a negative pressure as drying material, which reduces the boiling point and thus leads to evaporation of the water even at low temperatures.
- the heat of vaporization continuously withdrawn from the material to be dried is suitably fed from the outside until the temperature is constant.
- Vacuum drying has the effect of lowering the equilibrium vapor pressure, which favors capillary transport. This has proven to be particularly advantageous for the present carrot fiber material, since the activated, open fiber structures and thus the rheological properties resulting therefrom are retained.
- the vacuum drying preferably takes place at a reduced pressure of less than 400 mbar, preferably less than 300 mbar, further preferably less than 250 mbar and particularly preferably less than 200 mbar.
- the drying in step D comprises drying under atmospheric pressure.
- suitable drying methods are fluidized bed drying, moving bed drying, belt dryers, drum dryers or paddle dryers.
- Fluid bed drying is particularly preferred here. This has the advantage that the product is dried loosely, which simplifies an optional subsequent grinding step.
- this type of drying avoids damage to the product due to local overheating thanks to the easily adjustable heat input.
- the dissolved dye is added to the activated fruit fibers and the fiber is impregnated with the dye as a result of the drying of the dye solution on the fiber that has not yet dried completely.
- the functionality of the fiber is essentially retained when a dye is added during fiber drying. The activation state is not seriously affected.
- a carrot fiber according to the application is a primarily fibrous component isolated from a nonlignified vegetable cell wall of a carrot and consists mainly of cellulose.
- the term fiber is somewhat misnomer because carrot fibers do not appear macroscopically as fibers but are a powdered product.
- Other components of carrot fiber include hemicellulose and pectin.
- An activated carrot fiber according to the present application is defined by the yield point of the fiber in 2.5% dispersion or by the viscosity.
- a pectin according to the application is defined as a vegetable polysaccharide which, as a polyuronide, essentially consists of ⁇ -1,4-glycosidically linked D-galacturonic acid units.
- the galacturonic acid units are partially esterified with methanol.
- the degree of esterification describes the proportion of carboxyl groups in the galacturonic acid units of the pectin which are present in esterified form, e.g. as methyl ester.
- a highly esterified pectin is a pectin which has a degree of esterification of at least 50%.
- a low ester pectin on the other hand, has a degree of esterification of less than 50%.
- the degree of esterification describes the percentage of the carboxyl groups in the galacturonic acid units of the pectin which are present in the esterified form, e.g. as methyl ester.
- the degree of esterification can be determined using the method according to JECFA (Monograph 19-2016, Joint FAO/WHO Expert Committee on Food Additives).
- FIG. 1 a process according to the invention for the production of the colored activated carrot fiber is shown schematically as a flow diagram.
- the pomace is subjected to colorant extraction (“colorant isolation”) in the first step.
- the dyes extracted using isopropanol are concentrated by driving off the isopropanol in a rotary evaporator.
- the decolorized fibers (“decolorization”) occurring after the extraction are washed (“washing”) by carrying out two alcohol washing steps, each with subsequent solid-liquid separation (not shown separately here) using a decanter.
- the fibers are partially dried by fluidized bed drying and then the partially dried fibers are remoistened with the above-described concentrated dye-containing solution.
- the fibers are then dried completely (i.e. to a moisture content of less than 10%). Finally, the colored fibers are further comminuted by a grinding step to then obtain the activated colored carrot fiber of the present invention.
- FIG. 2 shows a schematic flow diagram of an alternative process according to the invention for the production of the colored activated carrot fiber.
- the pomace is subjected to colorant extraction (“isolation of colorants”).
- the dyes extracted using isopropanol are used as a dye solution without concentration in the subsequent drying step.
- the decolorized fibers (“decolorization”) occurring after the extraction are washed (“washing”) by carrying out two alcohol washing steps, each with subsequent solid/liquid separation (not shown separately here) using a decanter.
- the drying of the alcohol-moist fibers from the washing step takes place in a rotary evaporator with the addition of the previously extracted dye-containing solution.
- the colored fibers are further comminuted by a grinding step to then obtain the activated colored carrot fiber of the present invention.
- the sample is carefully filled into the measuring system of the rheometer after exactly 1 hour and the respective measurement is started. If the sample settles, it is carefully stirred with a spoon immediately before filling.
- the sample is carefully filled into the measuring system of the rheometer after exactly 1 hour and the respective measurement is started. If the sample settles, it is carefully stirred with a spoon immediately before filling.
- This yield point provides information about the structural strength and is determined in the rotation test by increasing the shear stress acting on the sample over time until the sample begins to flow.
- Shear stresses that are below the yield point only cause an elastic deformation, which only leads to yielding if the shear stresses are above the yield point. In this determination, this is recorded by measuring when a specified minimum shear rate t is exceeded. According to the present method, the yield point t 0 [Pa] is exceeded at the shear rate t > 0.1 s _1.
- Measuring device Rheometer Physica MCR series (e.g. MCR 301, MCR 101)
- Measuring system Z3 DIN or CC25
- Measuring cup CC 27 P06 (ribbed measuring cup)
- the yield point x 0 (unit [Pa] is read in Section 2 and is the shear stress (unit: [Pa]) at which the shear rate is ⁇ 0.10 s _1 for the last time.
- yield point (rotation) The yield point measured with the rotation method is also referred to as “yield point (rotation)”.
- This yield point also provides information about the structural strength and is determined in the oscillation test by increasing the amplitude at a constant frequency until the sample is destroyed by the ever-increasing deflection and then begins to flow.
- the substance behaves like an elastic solid below the yield point, i.e. the elastic parts (G') are above the viscous parts (G"), while at If the yield point is exceeded, the viscous components of the sample increase and the elastic components decrease.
- Measuring device Rheometer Physica MCR series (e.g. MCR 301, MCR 101)
- Measuring system Z3 DIN or CC25
- Measuring cup CC 27 P06 (ribbed measuring cup)
- the shear stress at the cross-over is evaluated after exceeding the linear-viscoelastic range.
- yield point (cross over) The yield point measured with the oscillation method is also known as the “yield point (cross over)”.
- yield point II crossover
- the dynamic Weissenberg number W' (Windhab E, Maier T, Anlagentechnik 1990, 44: 185f) is a derived variable in which the elastic components (G') determined in the oscillation test in the linear viscoelastic range are compared with the viscous parts (G") are put into relation: w, _ G'(o>) _ 1 i) tan d
- the dynamic Weissenberg number one obtains a variable that correlates particularly well with the sensory perception of the consistency and is relatively independent of the absolute strength of the sample can be viewed.
- a high value for W means that the fibers have built up a predominantly elastic structure, while a low value for W indicates structures with clearly viscous parts.
- the creamy texture that is typical of fibers is achieved when the W values are in the range of approx. 6 - 8, with lower values the sample is assessed as watery (less thick).
- Measuring device Rheometer Physica MCR series, e.g. MCR 301, MCR 101 Measuring system: Z3 DIN or CC25
- Measuring cup CC 27 P06 (ribbed measuring cup) Measurement parameters:
- phase shift angle d is read in the linear viscoelastic range.
- dynamic Weissenberg number W is then calculated using the following formula:
- Test method/option Measurement of the force in the direction of compression / simple test Parameters:
- the strength corresponds to the force that the measuring body needs to penetrate 10 mm into the suspension. This force is read from the force-time diagram. It should be noted that from the history of strength measurement, the unit of strength measured was in grams (g).
- a set of screens In a screening machine, a set of screens, the mesh size of which constantly increases from the bottom screen to the top, is arranged one above the other. The sample is placed on the top sieve - the one with the largest mesh size. The sample particles with a diameter larger than the mesh size remain on the sieve; the finer particles fall through to the next sieve. The proportion of the sample on the different sieves is weighed out and reported as a percentage.
- the sample is weighed to two decimal places.
- the screens are provided with screening aids and built up one on top of the other with increasing mesh size.
- the sample is quantitatively transferred to the top sieve, the sieves are clamped and the sieving process proceeds according to defined parameters.
- the individual sieves are weighed with sample and sieve aid and empty with sieve aid. If only a limit value in the particle size spectrum is to be checked for a product (e.g. 90% ⁇ 250 ⁇ m), then only a sieve with the appropriate mesh size is used.
- the screen construction consists of the following mesh sizes in pm: 1400, 1180, 1000, 710, 500, 355, 300 followed by the bottom.
- the grain size is calculated using the following formula:
- the sample is allowed to swell with an excess of water at room temperature for 24 hours. After centrifugation and subsequent decanting of the supernatant, the water binding capacity in g HO / g sample can be determined gravimetrically. The pH value in the suspension must be measured and documented.
- Plant fiber 1.0 g (in centrifuge tube)
- the supernatant water is separated from the swollen sample.
- the sample with the bound water is weighed out.
- WBV water binding capacity
- Measuring device Physica MCR series (e.g. MCR 301, MCR 101) Measuring system: Z3 DIN or CC25
- the moisture content of the sample is understood to mean the decrease in mass determined according to defined conditions after drying.
- the moisture content of the sample is determined by means of infrared drying using the Sartorius MA-45 moisture analyzer (from Sartorius, Goettingen, Germany).
- the color and brightness measurements are carried out with the Minolta Chromameter CR 300 or CR 400.
- the spectral properties of a sample are determined using standard color values.
- the color of a sample is described in terms of hue, lightness and saturation. With these three basic properties, the color can be represented three-dimensionally:
- the hues lie on the outer shell of the color body, the lightness varies on the vertical axis and the degree of saturation runs horizontally.
- L*a*b* measurement system pronounced L-star, a-star, b-star
- L* represents lightness
- a* and b* represent both hue and saturation for a* and b * indicate the positions on two color axes, where a* is assigned to the red-green axis and b* to the blue-yellow axis.
- the device converts the standard color values into L*a*b* coordinates. Carrying out the measurement:
- the sample is sprinkled on a white sheet of paper and leveled with a glass stopper.
- the measuring head of the chromameter is placed directly on the sample and the trigger is pressed.
- a triplicate measurement is carried out on each sample and the mean value is calculated.
- the L*, a*, b* values are specified by the device with two decimal places.
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Abstract
La présente invention concerne une fibre de carotte colorée activée et un procédé pour sa fabrication. L'invention concerne en outre l'utilisation de la fibre de carotte colorée activée comme agent épaississant ou structurant dans différents produits industriels. L'invention concerne en outre un produit alimentaire, un produit alimentaire pour animaux, un complément alimentaire, une boisson, un produit cosmétique, un produit pharmaceutique ou un produit médical fabriqués au moyen de la fibre de carotte colorée activée selon l'invention. Enfin, l'invention concerne un procédé de coloration de fibres de fruits activées, en particulier de fibres d'agrume, de pomme ou de carotte.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP21755897.2A EP4185128A1 (fr) | 2020-07-22 | 2021-07-22 | Fibre de carotte colorée activée |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102020119365.3A DE102020119365A1 (de) | 2020-07-22 | 2020-07-22 | Aktivierte gefärbte Karottenfaser |
| DE102020119365.3 | 2020-07-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2022018188A1 true WO2022018188A1 (fr) | 2022-01-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2021/070488 Ceased WO2022018188A1 (fr) | 2020-07-22 | 2021-07-22 | Fibre de carotte colorée activée |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP4185128A1 (fr) |
| DE (1) | DE102020119365A1 (fr) |
| WO (1) | WO2022018188A1 (fr) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003015537A1 (fr) * | 2001-08-13 | 2003-02-27 | Dsm Ip Assets B.V. | Compositions comprenant de la pectine de betterave a sucre et des carotenoides |
| US20040086626A1 (en) * | 2002-11-06 | 2004-05-06 | Fiberstar, Inc. | Highly refined fiber mass, process of their manufacture and products containing the fibers |
| US20080233238A1 (en) * | 2007-02-08 | 2008-09-25 | Grimmway Enterprises, Inc. | Supercritical co2 carrot feedstock extraction |
| EP2597968A2 (fr) * | 2010-07-30 | 2013-06-05 | Cargill, Incorporated | Procédé pour modifier les propriétés de fibre d'agrume |
| WO2019005915A1 (fr) * | 2017-06-27 | 2019-01-03 | Dupont Nutrition, Usa Inc. | Agents de texturisation colorants d'origine végétale |
-
2020
- 2020-07-22 DE DE102020119365.3A patent/DE102020119365A1/de active Pending
-
2021
- 2021-07-22 EP EP21755897.2A patent/EP4185128A1/fr active Pending
- 2021-07-22 WO PCT/EP2021/070488 patent/WO2022018188A1/fr not_active Ceased
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003015537A1 (fr) * | 2001-08-13 | 2003-02-27 | Dsm Ip Assets B.V. | Compositions comprenant de la pectine de betterave a sucre et des carotenoides |
| US20040086626A1 (en) * | 2002-11-06 | 2004-05-06 | Fiberstar, Inc. | Highly refined fiber mass, process of their manufacture and products containing the fibers |
| US20080233238A1 (en) * | 2007-02-08 | 2008-09-25 | Grimmway Enterprises, Inc. | Supercritical co2 carrot feedstock extraction |
| EP2597968A2 (fr) * | 2010-07-30 | 2013-06-05 | Cargill, Incorporated | Procédé pour modifier les propriétés de fibre d'agrume |
| WO2019005915A1 (fr) * | 2017-06-27 | 2019-01-03 | Dupont Nutrition, Usa Inc. | Agents de texturisation colorants d'origine végétale |
Non-Patent Citations (2)
| Title |
|---|
| CLEMENTZ ADRIANA ET AL: "Novel method for valorization of by-products from carrot discards", LWT- FOOD SCIENCE AND TECHNOLOGY, vol. 100, 27 October 2018 (2018-10-27), United Kingdom, pages 374 - 380, XP055857517, ISSN: 0023-6438, DOI: 10.1016/j.lwt.2018.10.085 * |
| XIA LIANGJUN ET AL: "Environmentally friendly dyeing of cotton in an ethanol-water mixture with excellent exhaustion", GREEN CHEMISTRY, vol. 20, no. 19, 28 August 2018 (2018-08-28), GB, pages 4473 - 4483, XP055857990, ISSN: 1463-9262, Retrieved from the Internet <URL:https://pubs.rsc.org/en/content/articlepdf/2018/gc/c8gc01814f> DOI: 10.1039/C8GC01814F * |
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| Publication number | Publication date |
|---|---|
| EP4185128A1 (fr) | 2023-05-31 |
| DE102020119365A1 (de) | 2022-01-27 |
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