CN111296729A - Water-soluble astaxanthin product and preparation method thereof - Google Patents
Water-soluble astaxanthin product and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a water-soluble astaxanthin product and a preparation method thereof. The water-soluble astaxanthin product is composed of astaxanthin, whey protein and ethyl cellulose, the content of the astaxanthin is higher than 60%, and the particle size of the product is micron-sized. The preparation method comprises the following steps: the water-soluble astaxanthin is prepared by mixing an astaxanthin alcohol solution, an ethyl cellulose alcohol solution and a whey solution in batches according to a certain proportion, homogenizing and emulsifying, secondarily emulsifying, settling at a low temperature, filtering, evaporating at a low temperature in vacuum, spraying, freezing and drying and the like. The technology of the invention effectively improves the water solubility and stability of the astaxanthin, increases the application range of the astaxanthin, and is widely applicable to a plurality of fields of food, health care products, medicines and the like.
Description
Technical Field
The invention relates to the technical field of water solubility of marine nutrients, and particularly relates to a water-soluble astaxanthin product and a preparation method thereof.
Background
Astaxanthin (3,3 ' -dihydroxy-4, 4 ' -diketo- β ' -carotene) is a fat-soluble carotenoid pigment with the molecular formula of C40H52O4 and the relative molecular mass of 596.86, is insoluble in water and is easily soluble in most organic solvents such as ethanol, acetone, diethyl ether, chloroform and the like, is mainly present in microalgae, yeast, trout, krill, shrimp and crayfish, and haematococcus pluvialis is a rich source of natural astaxanthin with the astaxanthin content of up to 6% of the dry matter, which is regarded as a "concentrate" of natural astaxanthin.
The natural astaxanthin is an effective strong antioxidant, has strong inoxidizability, effectively eliminates free radicals in vivo, and prevents tissues, cells and DNA from being damaged by oxidation, so the astaxanthin has multiple physiological 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 molecular structure of astaxanthin has highly unsaturated conjugated double chains, so that the astaxanthin is easily degraded and oxidized by illumination, oxygen, high temperature, ultraviolet irradiation and the like, and the stability of the astaxanthin is influenced. The astaxanthin is insoluble in water, so that the bioavailability of the astaxanthin is low. The water solubility and stability of astaxanthin can be improved by microsphere technology. The drug-loaded microspheres refer to micron-sized spherical entities formed by dissolving or adsorbing active ingredients in a high-molecular matrix. The microspheres not only protect the active ingredients of the core material from the influence of factors such as oxygen, high temperature, pH and the like, but also improve the dispersibility of the active ingredients, cover the bad smell and control the release, thereby improving the commercial value of the astaxanthin product.
The Chinese patent publication No. CN105646869A discloses a preparation method of a stable water-soluble carotenoid dry powder, which is prepared by dissolving Astaxanthin in acetone, then mixing with various surfactants and stabilizers of which the mass is 5 times higher than that of the Astaxanthin, such as S-40, acacia, β -cyclodextrin, xanthan gum and pullulan, and is prepared by spray drying, which is mainly prepared by adding a stabilizer to disperse the Astaxanthin in water, using an excessive amount of additives to process food, and having a safety hazard of the Astaxanthin, and using a water-soluble polysaccharide dispersion as a water-soluble polysaccharide dispersion for preparing Astaxanthin, which is also disclosed as a simple polysaccharide-cellulose dispersion for stabilizing Astaxanthin, which is prepared by using a dispersion of a low-viscosity cellulose dispersion for preparing Astaxanthin, a simple polysaccharide-cellulose dispersion for preparing Astaxanthin, and a simple polysaccharide-cellulose dispersion for preparing Astaxanthin, which is prepared by using a dispersion of a low-viscosity cellulose dispersion of cellulose-cellulose dispersion for preparing Astaxanthin, which is disclosed as a simple polysaccharide-cellulose-polysaccharide complex polysaccharide-polysaccharide.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a water-soluble astaxanthin product and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
a water-soluble astaxanthin product and a preparation method thereof are characterized in that: 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 the astaxanthin alcohol solution and the ethyl cellulose alcohol solution according to a ratio of 1: 1-2: 3, stirring at a rotating speed of 1000-1500 rpm for 10-20 min uniformly, injecting a high-concentration whey solution at a speed of 1mL/s, and continuously homogenizing and emulsifying at a rotating speed of 1000-1500 rpm for 5-10 min to obtain a water-in-oil emulsion; wherein: adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to prepare an astaxanthin alcohol solution with the mass volume ratio of 3-5%; the ethyl cellulose alcoholic solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4-5 hours to prepare the ethyl cellulose alcoholic solution with the mass volume of 0.5-1%; the high whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5-1 h, and preparing into a whey solution with the mass-volume ratio of 2% -3%; the volume of the high 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 the speed of 35-40 mL/s, mixing at the 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, stirring for 0.5-1 h and preparing into 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 the dark for 12-24 hours, precipitating the ethyl cellulose and the astaxanthin which are excessively added, filtering by a 200-mesh gauze, and removing ethanol by low-temperature vacuum evaporation at the rotary evaporation temperature of 35-40 ℃ to obtain an astaxanthin water solution; and (3) carrying out spray freeze drying on the astaxanthin water solution, wherein the spray freeze drying condition is that the condensation temperature is-40 ℃, and drying is carried out for 6-8 h at the temperature of 30 ℃ to obtain the water-soluble astaxanthin product. The astaxanthin content and the solubility in the product are respectively 62.7-75.9% and 42.6-56%.
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 and 56% of solubility, and the particle size of the water-soluble astaxanthin ranges from 280nm to 320 nm.
The ethyl cellulose used in the invention is purchased from Shanghai Michelin Biochemical technology Limited, and the viscosity of the ethyl cellulose 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:
1. according to the water-soluble astaxanthin product and the preparation method thereof, the ethyl cellulose-astaxanthin emulsion is prepared by adopting a twice emulsification method, so that the aggregation of ethyl cellulose in a 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 the astaxanthin; spray freeze drying maintains the functional activity of astaxanthin under low temperature conditions.
2. 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 62.7-76.9 percent of astaxanthin, the solubility is 42.6-56 percent, and the solubility of the raw material astaxanthin is 11.81 percent.
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 obtained in example 1 of the present invention in an aqueous solution.
FIG. 4 shows the pH of water-soluble astaxanthin obtained in example 1 of the present invention2～pH8Zeta-equipotential when stored in aqueous solution after 3 weeks.
Detailed Description
The invention is further illustrated by the following examples and figures.
Example 1
A water-soluble astaxanthin product and a preparation method thereof comprise the following steps:
1. mixing astaxanthin alcohol solution and ethyl cellulose alcohol solution according to a ratio of 1:1, stirring at a rotating speed of 1500rpm for 20min uniformly, injecting 10mL of high-concentration whey solution (the mass volume is 2%) at a speed of 1mL/s, and continuously homogenizing and emulsifying at the rotating speed of 1500rpm for 10min to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to prepare 5% astaxanthin alcohol solution by mass volume; the ethyl cellulose alcoholic solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4h to prepare the ethyl cellulose alcoholic solution with the mass volume of 1%; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5h and preparing into a whey solution with the mass-volume ratio of 2%; the volume of the added high-concentration whey solution was 10 mL;
2. injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at the speed of 40mL/s, simultaneously mixing at the rotating speed of 1500rpm, and carrying out secondary emulsification for 20min to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5h and preparing into a whey solution with the mass-volume ratio of 0.3%; the volume of the low-concentration whey solution is 190 mL; the volume ratio of oil phase to water phase in the oil-in-water emulsion is 1: 2;
3. standing the oil-in-water emulsion prepared in the step 2 at 4 ℃ in the dark for 12h, precipitating the ethyl cellulose and the astaxanthin which are excessively added, filtering by a 200-mesh gauze, and removing ethanol by low-temperature vacuum evaporation at the rotary evaporation temperature of 37 ℃ to obtain an astaxanthin water solution; and (3) carrying out spray freeze drying on the astaxanthin water solution, wherein the spray freeze drying condition is that the condensation temperature is-40 ℃, and drying is carried out for 7 hours at the temperature of 30 ℃ to obtain a water-soluble astaxanthin product. The astaxanthin content and solubility in the product were 75.9% and 56%, respectively.
Example 2
A water-soluble astaxanthin product and a preparation method thereof comprise the following steps:
1. mixing astaxanthin alcohol solution and ethyl cellulose alcohol solution at a ratio of 2:1, stirring at 1500rpm for 20min, injecting 20mL of high-concentration whey solution (3% by mass volume) at a rate of 1mL/s, and homogenizing and emulsifying at 1500rpm for 10min to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to prepare 5% astaxanthin alcohol solution by mass volume; the ethyl cellulose alcoholic solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 5h to prepare the ethyl cellulose alcoholic solution with the mass volume of 0.5%; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5h and preparing into a whey solution with the mass-volume ratio of 2.5%; the volume of the added high concentration whey solution was 15 mL;
2. injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at the speed of 40mL/s, simultaneously mixing at the rotating speed of 1500rpm, and carrying out secondary emulsification for 10min to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5h and preparing into a whey solution with the mass-volume ratio of 0.3%; the volume of the low-concentration whey solution is 190 mL; the volume ratio of oil phase to water phase in the oil-in-water emulsion is 1: 2.1;
3. standing the oil-in-water emulsion prepared in the step 2 at 4 ℃ in the dark for 24h, precipitating the ethyl cellulose and the astaxanthin which are excessively added, filtering by a 200-mesh gauze, and removing ethanol by low-temperature vacuum evaporation at the rotary evaporation temperature of 40 ℃ to obtain an astaxanthin water solution; and (3) carrying out spray freeze drying on the astaxanthin water solution, wherein the spray freeze drying condition is that the condensation temperature is-40 ℃, and drying is carried out for 8 hours at the temperature of 30 ℃ to obtain a water-soluble astaxanthin product. The astaxanthin content and solubility in the product were 68.7% and 53.8%, respectively.
Example 3
A water-soluble astaxanthin product and a preparation method thereof comprise the following steps:
1. mixing astaxanthin alcohol solution and ethyl cellulose alcohol solution according to a ratio of 2:3, stirring at the rotating speed of 1000rpm for 10min uniformly, injecting 10mL of high-concentration whey solution (the mass volume is 2%) at the speed of 1mL/s, and continuously homogenizing and emulsifying at the rotating speed of 1000rpm for 5min to obtain water-in-oil emulsion; wherein the astaxanthin alcohol solution is prepared by adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to prepare the astaxanthin alcohol solution with the mass volume of 3%; the ethyl cellulose alcoholic solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4h to prepare the ethyl cellulose alcoholic solution with the mass volume of 0.5%; the high-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 1h, and preparing into a whey solution with the mass-volume ratio of 3%; the volume of the added high concentration whey solution was 20 mL;
2. injecting the low-concentration whey solution into the water-in-oil emulsion prepared in the step 1 at the speed of 35mL/s, mixing at the rotating speed of 1000rpm, and emulsifying for 5min twice to obtain an oil-in-water emulsion; the low-concentration whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 1h, and preparing into a whey solution with the mass-volume ratio of 0.1%; the volume of the low-concentration whey solution is 180 mL; the volume ratio of oil phase to water phase 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 the dark for 12h, precipitating the ethyl cellulose and the astaxanthin which are excessively added, filtering by a 200-mesh gauze, and removing ethanol by low-temperature vacuum evaporation at the rotary evaporation temperature of 35 ℃ to obtain an astaxanthin water solution; and (3) carrying out spray freeze drying on the astaxanthin water solution, wherein the spray freeze drying condition is that the condensation temperature is-40 ℃, and drying is carried out for 6 hours at the temperature of 30 ℃ to obtain a 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 figure 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 material astaxanthin powder in an aqueous solution are shown in fig. 3.
Example 1 preparation of water-soluble astaxanthin the Zeta potential diagram of water-soluble astaxanthin after storage in aqueous solution at a pH range of 2-8 for 3 weeks is shown in FIG. 4. The solution system is stable according to the surface charge absolute value of more than or equal to 30mV, and the water-soluble astaxanthin solution has good stability.
Claims (3)
1. A water-soluble astaxanthin product and a preparation method thereof are characterized in that: 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 the astaxanthin alcohol solution and the ethyl cellulose alcohol solution according to a ratio of 1: 1-2: 3, stirring at a rotating speed of 1000-1500 rpm for 10-20 min uniformly, injecting a high-concentration whey solution at a speed of 1mL/s, and continuously homogenizing and emulsifying at a rotating speed of 1000-1500 rpm for 5-10 min to obtain a water-in-oil emulsion; wherein: adding astaxanthin into absolute ethyl alcohol, stirring and dissolving to prepare an astaxanthin alcohol solution with the mass volume ratio of 3-5%; the ethyl cellulose alcoholic solution is prepared by adding ethyl cellulose into absolute ethyl alcohol, and stirring for 4-5 hours to prepare the ethyl cellulose alcoholic solution with the mass volume of 0.5-1%; the high whey solution is prepared by dissolving whey protein powder in distilled water, stirring for 0.5-1 h, and preparing into 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 the speed of 35-40 mL/s, mixing at the 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, stirring for 0.5-1 h and preparing into 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 the dark for 12-24 h, precipitating the ethyl cellulose and the astaxanthin which are excessively added, filtering by a 200-mesh gauze, and removing ethanol by low-temperature vacuum evaporation at the rotary evaporation temperature of 35-40 ℃ to obtain an astaxanthin water solution; and (3) carrying out spray freeze drying on the astaxanthin water solution, wherein the conditions of the spray freeze drying are that the condensation temperature is-40 ℃, and the drying is carried out for 6-8 h at the temperature of 30 ℃ to obtain a water-soluble astaxanthin product, and the content and the solubility of the astaxanthin in the product are respectively 62.7-75.9% and 42.6-56%.
2. The water-soluble astaxanthin product and the preparation method thereof according to claim 1, wherein the whey solution is prepared by adding 0.5-3% by mass of whey protein into a certain volume of distilled water and stirring for 0.5-1.0 h.
3. The product of claim 1, wherein the water-soluble astaxanthin comprises 63% astaxanthin and 56% astaxanthin, and the particle size of the water-soluble astaxanthin ranges from 280nm to 320 nm.
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Cited By (2)
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| CN111296729B (en) | 2023-10-03 |
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