CN111296729B - Water-soluble astaxanthin product and preparation method thereof - Google Patents

Water-soluble astaxanthin product and preparation method thereof Download PDF

Info

Publication number
CN111296729B
CN111296729B CN202010097080.2A CN202010097080A CN111296729B CN 111296729 B CN111296729 B CN 111296729B CN 202010097080 A CN202010097080 A CN 202010097080A CN 111296729 B CN111296729 B CN 111296729B
Authority
CN
China
Prior art keywords
astaxanthin
water
solution
prepared
whey
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010097080.2A
Other languages
Chinese (zh)
Other versions
CN111296729A (en
Inventor
江虹鋭
王富云
王成财
王哲銘
梁舒韵
刘小玲
李树波
姜毅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi University
Original Assignee
Guangxi University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi University filed Critical Guangxi University
Priority to CN202010097080.2A priority Critical patent/CN111296729B/en
Publication of CN111296729A publication Critical patent/CN111296729A/en
Application granted granted Critical
Publication of CN111296729B publication Critical patent/CN111296729B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/44—Freeze-drying
    • 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
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/46—Spray-drying
    • 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/12—Ketones
    • A61K31/122—Ketones having the oxygen directly attached to a ring, e.g. quinones, vitamin K1, anthralin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38—Cellulose; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P27/00—Drugs for disorders of the senses
    • A61P27/02—Ophthalmic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P37/00—Drugs for immunological or allergic disorders
    • A61P37/02—Immunomodulators
    • A61P37/04—Immunostimulants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00—General protective or antinoxious agents
    • A61P39/06—Free radical scavengers or antioxidants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00—Drugs for disorders of the cardiovascular system
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0492—Applications, solvents used

Landscapes

  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Pharmacology & Pharmacy (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Epidemiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Food Science & Technology (AREA)
  • Nutrition Science (AREA)
  • Immunology (AREA)
  • Inorganic Chemistry (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Biochemistry (AREA)
  • Toxicology (AREA)
  • Cardiology (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Ophthalmology & Optometry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Mycology (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention discloses a preparation method of a water-soluble astaxanthin product. The water-soluble astaxanthin product consists of astaxanthin, whey protein and ethyl cellulose, wherein the astaxanthin content is higher than 60%, and the particle size of the product is in the micron order. The preparation method comprises the following steps: the water-soluble astaxanthin is prepared by mixing astaxanthin alcohol solution, ethyl cellulose alcohol solution and whey solution in batches according to a certain proportion, homogenizing and emulsifying, emulsifying secondarily, settling at low temperature, filtering, evaporating in vacuum at low temperature, spraying, freeze drying and the like. The technology of the invention effectively improves the water solubility and stability of the astaxanthin and increases the application range of the astaxanthin, and the invention is widely applicable to a plurality of fields such as food, health care products, medicines and the like.

Description

Water-soluble astaxanthin product and preparation method thereof
Technical Field
The invention relates to the technical field of marine nutrient water solubility, in particular to a preparation method of a water-soluble astaxanthin product.
Background
Astaxanthin (3, 3' -dihydroxy-4, 4' -diketo-beta, beta ' -carotene) is a fat-soluble carrot-like pigment, has a molecular formula of C40H52O4, is insoluble in water and is easily dissolved in most organic solvents such as ethanol, acetone, diethyl ether, chloroform and the like, and the relative molecular weight is 596.86. Astaxanthin is mainly present in microalgae, yeasts, trout, krill, shrimp and crayfish, and haematococcus pluvialis is a rich source of natural astaxanthin, with astaxanthin content up to 6% of dry matter, seen as a "concentrate" of natural astaxanthin.
The natural astaxanthin is an effective strong antioxidant, has strong oxidation resistance and can effectively remove free radicals in vivo and prevent tissues, cells and DNA from being damaged by oxidation, so that the astaxanthin has the functions of resisting oxidation, improving immunity, preventing tumors, preventing cardiovascular diseases, maintaining eyes and the like, is gradually applied to industries such as medicines, foods, health-care products, cosmetics and the like, and has wide application prospect.
The astaxanthin has a highly unsaturated conjugated double chain in the molecular structure, so that the astaxanthin is extremely easy to be degraded and oxidized by light, oxygen, high temperature, ultraviolet irradiation and the like, and the stability of the astaxanthin is influenced. Astaxanthin is poorly soluble in water, making its bioavailability low. The water solubility and stability of astaxanthin can be improved by microsphere technology. The drug-loaded microsphere is a micron-sized spherical entity formed by dissolving or adsorbing an active ingredient in a polymer matrix. The microsphere not only protects the core active ingredient from the environmental factors such as oxygen, high temperature and pH, but also improves the dispersibility of the active ingredient, covers bad smell and controls release, thereby improving the commercial value of astaxanthin products.
At present, scholars at home and abroad mainly research on improvement of astaxanthin water solubility by means of structure improvement, emulsification or microencapsulation and the like. The invention relates to a method for preparing astaxanthin succinic acid diester-PEG derivative by using astaxanthin, succinic anhydride and polyethylene glycol (PEG), wherein the preparation method is carried out in an organic solvent system, and the organic solvent is remained, so that potential safety hazard exists. The chinese patent publication No. CN101297691a discloses a method for preparing stable water-soluble carotenoid dry powder, which comprises dissolving astaxanthin in acetone, mixing with S-40, acacia, beta-cyclodextrin, xanthan gum, pullulan and other surfactants and stabilizers with a mass 5 times higher than that of astaxanthin, and spray drying. According to the method, the astaxanthin is dispersed in water mainly by adding the stabilizer, and excessive use of the additive is not suitable for processing food and has potential safety hazards of organic solvent residues; in addition, astaxanthin is degraded above 100 ℃, and the spray drying conditions used in the present invention are detrimental to the stability of astaxanthin. The publication P h y s i c o c h e m i c a l properties of whey-protein-stabilized astaxanthin nanodispersion anditstransport via a Caco-2monolayer reports that astaxanthin nano-dispersion is prepared by using isolated whey protein as a stabilizer, but the solvent adopted by the astaxanthin nano-dispersion is an acetone/dichloromethane mixed system, so that potential safety hazards exist, and the product type is inconvenient to transport and store. Publication Astaxanthin from Phaffia rhodozyma: microencapsulationwith carboxymethyl cellulose sodium andmicrocrystalline cellulose and effects of microencapsulated astaxanthin on yogurt properties reports that sodium carboxymethyl cellulose and microcrystalline cellulose are used as wall materials, the water solubility of astaxanthin is improved by a microcapsule technology, and the prepared product has low astaxanthin content and nonuniform particles, and is easy to delaminate when being applied to foods. Publication No. Enca psula tion of an a sta xa n t h i n-c o n ta i n i n g l i p id e x t ra c t f r o m s h r i m p w a s t e by c o m p l e x
coacervation using a novel gelatinecashew gum complex it is reported that the solubility of astaxanthin is improved by complex coacervation using a complex of gelatin and cashew glue as wall material, but the solubility of astaxanthin product obtained by this preparation method is only 28.6%, and the water solubility of astaxanthin is low. The publication Potato protein-basedcarriers for enhancing bioavailability of astaxanthin reports that Potato protein is used as a carrier to improve the solubility of astaxanthin, but the preparation method requires dialysis of Potato protein solution for one week, takes a long time and has a complex production process. Therefore, there is a need to develop a highly viable, simple and effective method for increasing the water solubility of astaxanthin.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a preparation method of a water-soluble astaxanthin product.
The technical scheme for solving the technical problems is as follows:
a preparation method of a water-soluble astaxanthin product is characterized by comprising the following steps: the product is prepared from the following raw materials in percentage by mass: 60-80% of astaxanthin, 20-30% of whey protein and 10-20% of ethyl cellulose; the preparation method comprises the following steps:
mixing an astaxanthin alcohol solution and an ethyl cellulose alcohol solution according to a ratio of 1:1-2:3, stirring for 10-20 min at a speed of 1000 rpm-1500 rpm uniformly, injecting a high-concentration whey solution at a speed of 1mL/s, and continuously homogenizing and emulsifying for 5-10 min at a speed of 1000 rpm-1500 rpm to obtain a water-in-oil emulsion; wherein: the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving the astaxanthin into the astaxanthin alcohol solution with the mass-volume ratio of 3% -5%; the ethyl cellulose alcohol solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4-5 h to prepare 0.5-1% of ethyl cellulose alcohol solution by mass and volume; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water and stirring for 0.5-1 h to prepare a whey solution with the mass-volume ratio of 2% -3%; the volume of the high-concentration whey solution is 10-20 mL;
2, injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at a rate of 35-40 mL/s, mixing at a rotating speed of 1000-1500 rpm, and emulsifying for 5-20 min for the second time to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5-1 h to prepare a whey solution with the mass-volume ratio of 0.1-0.3%; the volume of the low-concentration whey solution is 180-190 mL; the volume ratio of oil phase to water phase in the oil-in-water emulsion is 1:1.9-1:2.1;
3, standing the oil-in-water emulsion prepared in the step 2 at 4 ℃ in a dark place for 12-24 hours, precipitating excessive added ethyl cellulose and astaxanthin, filtering by a 200-mesh gauze, removing ethanol by low-temperature vacuum evaporation, and obtaining an astaxanthin aqueous solution at a rotary evaporation temperature of 35-40 ℃; and (3) carrying out spray freeze drying on the astaxanthin aqueous solution, wherein the spray freeze drying condition is that the condensing temperature is minus 40 ℃, and drying is carried out for 6-8 hours at the temperature of 30 ℃ to obtain the water-soluble astaxanthin product. The astaxanthin content and solubility in the product are 62.7-75.9% and 42.6-56% respectively.
The whey solution is prepared by adding whey protein into distilled water with a certain volume according to the mass-volume ratio of 0.5-3%, and stirring for 0.5-1.0 h.
The water-soluble astaxanthin contains 63% of astaxanthin, has a solubility of 56% and a particle size of 280-320 nm.
The ethyl cellulose used in the invention is purchased from Shanghai Michelia Biochemical technology Co., ltd, and the viscosity is 45-55 mPa.s; the astaxanthin content used in the present invention was 95%.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the water-soluble astaxanthin product provided by the invention adopts a twice emulsification method to prepare the ethyl cellulose-astaxanthin emulsion, so that aggregation of the ethyl cellulose in the water-rich phase emulsion is reduced, and the particle size of the emulsion is reduced; whey protein solution is used as an emulsifier to improve the dispersibility and water solubility of astaxanthin; spray freeze drying maintains the functional activity of astaxanthin at low temperature.
The method has the advantages of strong feasibility, simple operation process, use of food-grade organic solvent and no potential safety hazard, the water-soluble astaxanthin contains 62.7 to 76.9 percent of astaxanthin, the solubility is 42.6 to 56 percent, the raw material astaxanthin has 11.81 percent of solubility, and compared with the raw material astaxanthin, the water-soluble astaxanthin has obviously improved solubility and keeps the bioactivity of the astaxanthin, and can be widely applied to the industries of foods, health care products and medicines.
Drawings
FIG. 1 is a graph showing the particle size distribution of astaxanthin and water-soluble astaxanthin obtained in example 1 of the present invention.
FIG. 2 is a diagram of a water-soluble astaxanthin product obtained in example 1 of the present invention.
FIG. 3 is a graph showing the dispersibility of water-soluble astaxanthin in an aqueous solution obtained in example 1 of the present invention.
FIG. 4 shows Zeta potential of the water-soluble astaxanthin obtained in example 1 according to the present invention after 3 weeks of storage in an aqueous solution having a pH of 2 to 8.
Detailed Description
The invention is further illustrated by the following examples and figures.
Example 1
A method for preparing a water-soluble astaxanthin product, comprising the steps of:
mixing an astaxanthin alcohol solution and an ethyl cellulose alcohol solution according to a ratio of 1:1, uniformly stirring for 20min at a speed of 1500rpm, injecting 10mL of high-concentration whey solution (mass volume is 2%) at a speed of 1mL/s, and continuously homogenizing and emulsifying for 10min at a speed of 1500rpm to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to obtain astaxanthin alcohol solution with mass volume of 5%; the ethyl cellulose alcohol solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4 hours to prepare the ethyl cellulose alcohol solution with the mass volume of 1%; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5h to prepare a whey solution with a mass-volume ratio of 2%; the addition volume of the high concentration whey solution was 10mL;
2, injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at a rate of 40mL/s, mixing at a rotating speed of 1500rpm, and emulsifying for 20min for the second time to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5h to prepare a whey solution with the mass-volume ratio of 0.3%; the volume of the low concentration whey solution is 190mL; the volume ratio of oil to water in the oil-in-water emulsion is 1:2;
3, standing the oil-in-water emulsion prepared in the step 2 at 4 ℃ in a dark place for 12 hours, precipitating excessive added ethylcellulose and astaxanthin, filtering by a 200-mesh gauze, removing ethanol by low-temperature vacuum evaporation, and obtaining an astaxanthin aqueous solution at 37 ℃; and (3) carrying out spray freeze drying on the astaxanthin aqueous solution, wherein the spray freeze drying condition is that the condensing temperature is-40 ℃, and drying is carried out for 7 hours at the temperature of 30 ℃ to obtain the water-soluble astaxanthin product. The astaxanthin content and solubility in the product were 75.9% and 56%, respectively.
Example 2
A method for preparing a water-soluble astaxanthin product, comprising the steps of:
mixing an astaxanthin alcohol solution and an ethyl cellulose alcohol solution according to a ratio of 2:1, stirring for 20min at a rotating speed of 1500rpm uniformly, injecting 20mL of high-concentration whey solution (mass volume is 3%) at a rate of 1mL/s, and continuously homogenizing and emulsifying for 10min at a rotating speed of 1500rpm to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to obtain astaxanthin alcohol solution with mass volume of 5%; the ethyl cellulose alcohol solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 5 hours to prepare 0.5% of ethyl cellulose alcohol solution by mass and volume; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5h to prepare a whey solution with a mass-volume ratio of 2.5%; the addition volume of the high concentration whey solution was 15mL;
2, injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at a rate of 40mL/s, mixing at a rotating speed of 1500rpm, and emulsifying for 10min for the second time to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5h to prepare a whey solution with the mass-volume ratio of 0.3%; the volume of the low concentration whey solution is 190mL; the volume ratio of oil to water in the oil-in-water emulsion is 1:2.1;
3, standing the oil-in-water emulsion prepared in the step 2 for 24 hours at 4 ℃ in a dark place, precipitating excessive added ethylcellulose and astaxanthin, filtering by a 200-mesh gauze, removing ethanol by low-temperature vacuum evaporation, and obtaining an astaxanthin aqueous solution at 40 ℃; and (3) carrying out spray freeze drying on the astaxanthin aqueous solution, wherein the spray freeze drying condition is that the condensing temperature is-40 ℃, and drying is carried out for 8 hours at the temperature of 30 ℃ to obtain the water-soluble astaxanthin product. The astaxanthin content and solubility in the product were 68.7% and 53.8%, respectively.
Example 3
A method for preparing a water-soluble astaxanthin product, comprising the steps of:
mixing an astaxanthin alcohol solution and an ethyl cellulose alcohol solution according to a ratio of 2:3, stirring for 10min at a speed of 1000rpm uniformly, injecting 10mL of high-concentration whey solution (mass volume is 2%) at a speed of 1mL/s, and continuously homogenizing and emulsifying for 5min at a speed of 1000rpm to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to obtain astaxanthin alcohol solution with mass volume of 3%; the ethyl cellulose alcohol solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4 hours to prepare 0.5% of ethyl cellulose alcohol solution by mass and volume; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 1h to prepare a whey solution with a mass-volume ratio of 3%; the addition volume of the high concentration whey solution was 20mL;
2, injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at a rate of 35mL/s, mixing at a rotating speed of 1000rpm, and emulsifying for 5min for the second time to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 1h to prepare a whey solution with the mass-volume ratio of 0.1%; the volume of the low-concentration whey solution is 180mL; the volume ratio of oil to water in the oil-in-water emulsion is 1:1.9;
3, standing the oil-in-water emulsion prepared in the step 2 at 4 ℃ in a dark place for 12 hours, precipitating excessive added ethylcellulose and astaxanthin, filtering by a 200-mesh gauze, removing ethanol by low-temperature vacuum evaporation, and obtaining an astaxanthin aqueous solution at a rotary evaporation temperature of 35 ℃; and (3) carrying out spray freeze drying on the astaxanthin aqueous solution, wherein the spray freeze drying condition is that the condensing temperature is-40 ℃, and drying is carried out for 6 hours at the temperature of 30 ℃ to obtain the water-soluble astaxanthin product. The astaxanthin content and solubility in the product were 62.7% and 42.6%, respectively.
The average particle sizes of the astaxanthin alcohol solution and the water-soluble astaxanthin prepared in example 1 are 231.7 + -1.88 nm and 307.30 + -11.36 nm, respectively, and the specific particle size distribution is shown in FIG. 1.
The water-soluble astaxanthin product prepared in example 1 is shown in FIG. 2.
The dispersibility of the water-soluble astaxanthin prepared in example 1 and the raw astaxanthin powder in an aqueous solution is shown in FIG. 3.
Example 1 preparation of water-soluble astaxanthin the Zeta potential diagram of water-soluble astaxanthin after 3 weeks of storage in aqueous solution at a pH in the range of 2-8 is shown in FIG. 4. The solution system is stable according to the absolute value of the surface charge of more than or equal to 30mV, and the water-soluble astaxanthin solution has good stability.

Claims (1)

1. A preparation method of a water-soluble astaxanthin product is characterized by comprising the following steps: the product is prepared from the following raw materials in percentage by mass: 60-80% of astaxanthin, 20-30% of whey protein and 10-20% of ethyl cellulose; the preparation method comprises the following steps:
(1) Mixing astaxanthin alcohol solution and ethyl cellulose alcohol solution according to a ratio of 1:1-2:3, stirring for 10-20 min uniformly at a speed of 1000 rpm-1500 rpm, injecting high-concentration whey solution at a speed of 1mL/s, and continuously homogenizing and emulsifying for 5-10 min at a speed of 1000 rpm-1500 rpm to obtain water-in-oil emulsion; wherein: the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving the astaxanthin into the astaxanthin alcohol solution with the mass-volume ratio of 3% -5%; the ethyl cellulose alcohol solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4-5 h to prepare 0.5-1% of ethyl cellulose alcohol solution by mass and volume; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water and stirring for 0.5-1 h to prepare a whey solution with the mass-volume ratio of 2% -3%; the volume of the high-concentration whey solution is 10-20 mL;
(2) Injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step (1) at a rate of 35-40 mL/s, mixing at a rotating speed of 1000-1500 rpm, and emulsifying for 5-20 min for the second time to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, and stirring for 0.5-1 h to prepare a whey solution with the mass-volume ratio of 0.1-0.3%; the volume of the low-concentration whey solution is 180-190 mL; the volume ratio of oil phase to water phase in the oil-in-water emulsion is 1:1.9-1:2.1;
(3) Standing the oil-in-water emulsion prepared in the step (2) at 4 ℃ in a dark place for 12-24 hours, precipitating excessive added ethyl cellulose and astaxanthin, filtering by a 200-mesh gauze, removing ethanol by low-temperature vacuum evaporation, and obtaining an astaxanthin aqueous solution at a rotary evaporation temperature of 35-40 ℃; and (3) carrying out spray freeze drying on the astaxanthin aqueous solution, wherein the spray freeze drying condition is that the condensing temperature is minus 40 ℃, and the astaxanthin aqueous solution is dried for 6 to 8 hours at the temperature of 30 ℃ to obtain a water-soluble astaxanthin product, and the astaxanthin content and the astaxanthin solubility in the product are respectively 62.7 to 75.9 percent and 42.6 to 56 percent.
CN202010097080.2A 2020-02-17 2020-02-17 Water-soluble astaxanthin product and preparation method thereof Active CN111296729B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010097080.2A CN111296729B (en) 2020-02-17 2020-02-17 Water-soluble astaxanthin product and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010097080.2A CN111296729B (en) 2020-02-17 2020-02-17 Water-soluble astaxanthin product and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111296729A CN111296729A (en) 2020-06-19
CN111296729B true CN111296729B (en) 2023-10-03

Family

ID=71152891

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010097080.2A Active CN111296729B (en) 2020-02-17 2020-02-17 Water-soluble astaxanthin product and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111296729B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111793014B (en) * 2020-07-27 2021-07-13 中国海洋大学 Method for preparing water-soluble astaxanthin and astaxanthin aqueous solution prepared by method
CN113527530B (en) * 2021-08-06 2022-04-29 青岛职业技术学院 Preparation method of water-soluble astaxanthin fucoidin ester

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1656178A (en) * 2002-05-30 2005-08-17 化尔氏制药研究公司 Oil-soluble pigment compositions
CN104839688A (en) * 2015-04-20 2015-08-19 华北制药秦皇岛有限公司 Eye care preparation and preparation method thereof
CN105769820A (en) * 2016-04-08 2016-07-20 华南理工大学 Method for preparing astaxanthin sustained release microsphere preparation through supercritical elution technology
CN105832569A (en) * 2016-05-31 2016-08-10 中国农业大学 Water-dispersible transparent astaxanthin emulsion and preparation method
CN106172894A (en) * 2016-07-18 2016-12-07 马鞍山市黄池食品（集团）有限公司 A kind of astaxanthin Semen Sesami gel oil and preparation method thereof
CN108403666A (en) * 2018-03-16 2018-08-17 深圳大学 A kind of preparation method of novel astaxanthin capsule of nano
CN109198382A (en) * 2018-07-24 2019-01-15 湖北工业大学 A kind of preparation method of water soluble beta-caroten powder
CN110693945A (en) * 2019-11-27 2020-01-17 上海海洋大学 Astaxanthin self-microemulsion preparation and preparation method and application thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9622970B2 (en) * 2014-05-08 2017-04-18 Yaguang Liu Pharmaceutical composition containing lutein and antioxidant for treating and preventing human disease

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1656178A (en) * 2002-05-30 2005-08-17 化尔氏制药研究公司 Oil-soluble pigment compositions
CN104839688A (en) * 2015-04-20 2015-08-19 华北制药秦皇岛有限公司 Eye care preparation and preparation method thereof
CN105769820A (en) * 2016-04-08 2016-07-20 华南理工大学 Method for preparing astaxanthin sustained release microsphere preparation through supercritical elution technology
CN105832569A (en) * 2016-05-31 2016-08-10 中国农业大学 Water-dispersible transparent astaxanthin emulsion and preparation method
CN106172894A (en) * 2016-07-18 2016-12-07 马鞍山市黄池食品（集团）有限公司 A kind of astaxanthin Semen Sesami gel oil and preparation method thereof
CN108403666A (en) * 2018-03-16 2018-08-17 深圳大学 A kind of preparation method of novel astaxanthin capsule of nano
CN109198382A (en) * 2018-07-24 2019-01-15 湖北工业大学 A kind of preparation method of water soluble beta-caroten powder
CN110693945A (en) * 2019-11-27 2020-01-17 上海海洋大学 Astaxanthin self-microemulsion preparation and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Astaxanthin encapsulation in ethyl cellulose carriers by continuoussupercritical emulsions extraction: A study on particle size,encapsulation efficiency, release profile and antioxidant activity;activityDiego F. Tiradoa，等;《The Journal of Supercritical Fluids》;20190501(第150期);第128-136页 *
Preventing the thermal degradation of astaxanthin through nanoencapsulation;Sensor Research Unit,等;《International Journal of Pharmaceutics》;20090314(第374期);第119-124页 *

Also Published As

Publication number Publication date
CN111296729A (en) 2020-06-19

Similar Documents

Publication Publication Date Title
CN105902401B (en) A kind of method preparing H- aggressiveness or J- aggressiveness astaxanthin polymer nanometer disperse systems and application
Paramera et al. Yeast cells and yeast-based materials for microencapsulation
CN105832569B (en) A kind of transparent astaxanthin lotion of water-dispersion type and preparation method thereof
Chen et al. Tumor microenvironment-responsive, high internal phase Pickering emulsions stabilized by lignin/chitosan oligosaccharide particles for synergistic cancer therapy
CN100399941C (en) Process for producing one or more kinds of dry powder of carotenoid
CN111296729B (en) Water-soluble astaxanthin product and preparation method thereof
Villalobos‐Castillejos et al. Production and stability of water‐dispersible astaxanthin oleoresin from Phaffia rhodozyma
JP3595300B2 (en) Preparation of dry powder of one or more oxidized carotenoids
CN109588721B (en) Carotenoid-protein particle and preparation method and application thereof
CN104856963A (en) Astaxanthin-sodium alginate sustained release microspheres as well as preparation method and application thereof
CN108850790A (en) A kind of monascorubin microcapsules and preparation method thereof
Cai et al. An integration study of microalgae bioactive retention: From microalgae biomass to microalgae bioactives nanoparticle
CN109419819B (en) Cold water-soluble haematococcus pluvialis pigment nano freeze-dried powder and preparation and application thereof
US11470861B2 (en) Preparation method and application of astaxanthin H1-, or H2- or J-aggregate water dispersion system
CN108578385B (en) Carotenoid-albumin compound and preparation method and application thereof
CN1302559A (en) Curcumin preparation
KR20200132584A (en) Stabilized astaxanthin nanoparticles and its manufacturing method
Li et al. Microfluidic spinning of fucoxanthin-loaded nanofibers for enhancing antioxidation and clarification of fruit juice
Camara et al. Alternative methods for gibberellic acid production, recovery and formulation: A case study for product cost reduction
CN113575945B (en) Preparation method of nanoscale all-trans carotenoid dry powder
CN109864244B (en) Method for improving stability of beta-carotene liposome by naringin
CN113812615A (en) Water-soluble protein-based astaxanthin product and preparation method thereof
US20200000736A1 (en) Oil-free carotenoid composition
CN104434824A (en) Method for preparing xanthophylls solid dispersion
Kou et al. Biodegradable materials as nanocarriers for drugs and nutrients

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant