CN113509444A - Preparation method of high-water-dispersion astaxanthin ester microspheres - Google Patents
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- CN113509444A CN113509444A CN202110947392.2A CN202110947392A CN113509444A CN 113509444 A CN113509444 A CN 113509444A CN 202110947392 A CN202110947392 A CN 202110947392A CN 113509444 A CN113509444 A CN 113509444A
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- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
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Abstract
The invention relates to the technical field of astaxanthin ester microspheres, in particular to a preparation method of high-water-dispersion astaxanthin ester microspheres, which comprises the following steps: s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1: 20-1: 60 g/ml; s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1: 20-1: 25 g/ml; s3, adding an emulsifier into the oil phase obtained in the S1, homogenizing for 1-3 times at 6000-8000 psi, adding the water phase obtained in the S2, mixing the oil phase and the water phase according to the volume ratio of 1: 16-1: 35, and dispersing for 2-4 min at 13000-15000 rpm/min to obtain a mixed solution; s4, preparing the astaxanthin-sucrose cocoate emulsion, wherein the astaxanthin ester microspheres prepared by the method have high water dispersibility, overcome the defects of liquid self-microemulsifying, have certain oxidation resistance and improve the stability of astaxanthin ester.
Description
Technical Field
The invention relates to the technical field of astaxanthin ester microspheres, in particular to a preparation method of high-water-dispersion astaxanthin ester microspheres.
Background
Natural astaxanthin is one of the strongest natural antioxidants in the world, and reduces the ability of free radicals to damage tissue cells and DNA by scavenging free radicals in the body. Experiments show that astaxanthin has the effects of resisting oxidation, aging and cancer, enhancing the immunologic function, preventing and treating cardiovascular diseases and the like, so that astaxanthin is widely applied to the fields of food, medicine, cosmetics and the like and plays an extremely important role in the health of human bodies.
In recent years, astaxanthin is regarded by consumers as a nutrient and medicine ingredient more and more, however, astaxanthin is easy to react with light, heat and oxide, is degraded into other substances, and the antioxidant activity of astaxanthin is seriously reduced. Secondly, the characteristics of small solubility of the astaxanthin under physiological conditions and instability of the astaxanthin under acid-base conditions severely restrict the development of the astaxanthin in the fields of medicines and foods. Experiments and clinical researches show that the preparation of the new preparation based on the drug delivery systems such as microspheres, liposomes and the like can improve the water solubility of the drug, improve the utilization rate of the drug, improve the stability and realize controlled slow release, and has profound significance for improving the medicinal value of the astaxanthin.
Therefore, we propose a method for preparing highly water-dispersible astaxanthin ester microspheres to solve the above problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method of high-water-dispersion astaxanthin ester microspheres.
A preparation method of high-water-dispersion astaxanthin ester microspheres comprises the following steps:
s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1: 20-1: 60 g/ml;
s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1: 20-1: 25 g/ml;
s3, adding an emulsifier into the oil phase obtained in the S1, homogenizing for 1-3 times at 6000-8000 psi, adding the water phase obtained in the S2, mixing the oil phase and the water phase according to the volume ratio of 1: 16-1: 35, and dispersing for 2-4 min at 13000-15000 rpm/min to obtain a mixed solution;
s4, homogenizing the mixed solution obtained in the step S3 at 9000-12000 psi for 3-5 times to obtain an astaxanthin-sucrose cocoate emulsion;
s5, adding a high polymer carrier into the astaxanthin-sucrose cocoate emulsion obtained in the step S4, uniformly stirring at 20-25 ℃, dispersing at 14000-16000 rpm/min for 2-3 min, dropwise adding the dispersed liquid into a salt solution with the concentration of 0.2-3 mol/L after uniform dispersion, uniformly stirring at 20-25 ℃ in the dropwise adding process, stopping stirring after dropwise adding is finished, and standing for 30-60 min to coagulate and solidify the dispersed liquid;
s6, collecting the agglomerated pellets, cleaning, filtering and drying to prepare the high-water-dispersion astaxanthin ester microspheres.
Preferably, the oil phase is one or more of sweet orange flower oil, olive oil and soybean oil.
Preferably, the emulsifier is selected from one or more of monoglyceride, tween, lecithin, sucrose fatty acid ester, polyglycerol ester, sodium stearoyl lactylate and diacetyl tartaric acid monoglyceride and diglyceride.
Preferably, the mass ratio of the astaxanthin ester to the emulsifier is 1: 6-1: 15.
Preferably, the polymer carrier is a mixture of sodium alginate and one or more of gelatin, modified starch, pectin and cyclodextrin.
Preferably, the weight volume ratio of the high polymer carrier to the astaxanthin-sucrose cocoate emulsion is 1: 0.3-1: 5 g/L.
Preferably, solutes in the salt solution are sodium hypophosphite, magnesium aspartate and calcium chloride, and the mass ratio of the sodium hypophosphite to the magnesium aspartate to the calcium chloride is 1 (0.3-0.8) to 2-5.
Preferably, in step S5, ultrasonic treatment is performed before standing, and the ultrasonic treatment time is 1-3 min.
Preferably, in step S5, the stirring speed is 250 to 350 rpm.
Preferably, in step S6, the drying temperature is 35 to 55 ℃.
The invention has the beneficial effects that: the astaxanthin ester microspheres prepared by the method have high water dispersibility, overcome the defects of liquid self-microemulsion, have certain oxidation resistance and improve the stability of astaxanthin ester; the astaxanthin ester microspheres have good compatibility with water, are beneficial to the application of the astaxanthin ester in water-phase medium products, and the preparation method has the advantages of simple process, mild conditions, low production cost and convenience for industrial popularization.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
In example 1, a method for preparing highly water-dispersible astaxanthin ester microspheres includes the following steps:
s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1:20 g/ml;
s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1:20 g/ml;
s3, adding an emulsifier into the oil phase obtained in the step S1, homogenizing for 1 time at 6000psi, adding the water phase obtained in the step S2, mixing the oil phase and the water phase according to the volume ratio of 1:16, and dispersing for 2min at 13000rpm/min to obtain a mixed solution;
s4, homogenizing the mixed solution obtained in the step S3 at 9000psi for 3 times to obtain an astaxanthin-sucrose cocoate emulsion;
s5, adding a high polymer carrier into the astaxanthin-sucrose cocoate emulsion obtained in the step S4, uniformly stirring at 20 ℃, dispersing at 14000rpm/min for 2min, dropwise adding the dispersed liquid into a salt solution with the concentration of 0.2mol/L, uniformly stirring at 20 ℃ in the dropwise adding process, stopping stirring after dropwise adding, and standing for 30min to coagulate and solidify the dispersed liquid;
s6, collecting the agglomerated pellets, cleaning, filtering and drying to prepare the high-water-dispersion astaxanthin ester microspheres.
Further, the oil phase is one or more of sweet orange flower oil, olive oil and soybean oil.
Further, the emulsifier is selected from one or more of monoglyceride, tween, lecithin, sucrose fatty acid ester, polyglycerol ester, sodium stearyl lactate and diacetyl tartaric acid monoglyceride and diglyceride.
Further, the mass ratio of the astaxanthin ester to the emulsifier is 1: 6.
Further, the polymer carrier is a mixture of sodium alginate and one or more of gelatin, modified starch, pectin and cyclodextrin.
Further, the weight-volume ratio of the high molecular carrier to the astaxanthin-sucrose cocoate emulsion is 1:0.3 g/L.
Furthermore, solutes in the salt solution are sodium hypophosphite, magnesium aspartate and calcium chloride, and the mass ratio of the sodium hypophosphite to the magnesium aspartate to the calcium chloride is 1:0.3: 2.
Further, in step S5, ultrasonic treatment is performed before standing, and the ultrasonic treatment time is 1 min.
Further, in step S5, the stirring speed is 250 rpm.
Further, in step S6, the drying temperature was 35 ℃.
In example 2, a method for preparing a high water-dispersible astaxanthin ester microsphere includes the following steps:
s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1:60 g/ml;
s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1:25 g/ml;
s3, adding an emulsifier into the oil phase obtained in the S1, homogenizing for 3 times at 8000psi, adding the water phase obtained in the S2, mixing the oil phase and the water phase according to the volume ratio of 1:35, and dispersing for 4min at 15000rpm/min to obtain a mixed solution;
s4, homogenizing the mixed solution obtained in the step S3 for 5 times at 12000psi to obtain an astaxanthin-sucrose cocoate emulsion;
s5, adding a high molecular carrier into the astaxanthin-sucrose cocoate emulsion obtained in the step S4, uniformly stirring at 25 ℃, dispersing at 16000rpm/min for 3min, dropwise adding the dispersed liquid into a salt solution with the concentration of 3mol/L, uniformly stirring at 25 ℃ in the dropwise adding process, stopping stirring after dropwise adding, standing for 60min, and coagulating and solidifying;
s6, collecting the agglomerated pellets, cleaning, filtering and drying to prepare the high-water-dispersion astaxanthin ester microspheres.
Further, the oil phase is one or more of sweet orange flower oil, olive oil and soybean oil.
Further, the emulsifier is selected from one or more of monoglyceride, tween, lecithin, sucrose fatty acid ester, polyglycerol ester, sodium stearyl lactate and diacetyl tartaric acid monoglyceride and diglyceride.
Further, the mass ratio of the astaxanthin ester to the emulsifier is 1: 15.
Further, the polymer carrier is a mixture of sodium alginate and one or more of gelatin, modified starch, pectin and cyclodextrin.
Further, the weight-volume ratio of the high molecular carrier to the astaxanthin-sucrose cocoate emulsion is 1:5 g/L.
Furthermore, solutes in the salt solution are sodium hypophosphite, magnesium aspartate and calcium chloride, and the mass ratio of the sodium hypophosphite to the magnesium aspartate to the calcium chloride is 1:0.8: 5.
Further, in step S5, ultrasonic treatment is performed before standing, and the ultrasonic treatment time is 3 min.
Further, in step S5, the stirring speed is 350 rpm.
Further, in step S6, the drying temperature was 55 ℃.
In example 3, a method for preparing highly water-dispersible astaxanthin ester microspheres includes the following steps:
s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1:40 g/ml;
s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1:22 g/ml;
s3, adding an emulsifier into the oil phase obtained in the S1, homogenizing for 2 times at 7000psi, adding the water phase obtained in the S2, mixing the oil phase and the water phase according to the volume ratio of 1:25, and dispersing for 3min at 14000rpm/min to obtain a mixed solution;
s4, homogenizing the mixed solution obtained in the step S3 for 4 times at 10500psi to obtain an astaxanthin-sucrose cocoate emulsion;
s5, adding a high molecular carrier into the astaxanthin-sucrose cocoate emulsion obtained in the step S4, uniformly stirring at 22 ℃, dispersing for 2min at 15000rpm/min, dropwise adding the dispersed liquid into a salt solution with the concentration of 2mol/L, uniformly stirring at 22 ℃ in the dropwise adding process, stopping stirring after dropwise adding, and standing for 45min to coagulate and solidify;
s6, collecting the agglomerated pellets, cleaning, filtering and drying to prepare the high-water-dispersion astaxanthin ester microspheres.
Further, the oil phase is one or more of sweet orange flower oil, olive oil and soybean oil.
Further, the emulsifier is selected from one or more of monoglyceride, tween, lecithin, sucrose fatty acid ester, polyglycerol ester, sodium stearyl lactate and diacetyl tartaric acid monoglyceride and diglyceride.
Further, the mass ratio of the astaxanthin ester to the emulsifier is 1: 9.
Further, the polymer carrier is a mixture of sodium alginate and one or more of gelatin, modified starch, pectin and cyclodextrin.
Further, the weight-volume ratio of the high molecular carrier to the astaxanthin-sucrose cocoate emulsion is 1:3 g/L.
Furthermore, solutes in the salt solution are sodium hypophosphite, magnesium aspartate and calcium chloride, and the mass ratio of the sodium hypophosphite to the magnesium aspartate to the calcium chloride is 1:0.5: 3.
Further, in step S5, ultrasonic treatment is performed before standing, and the ultrasonic treatment time is 2 min.
Further, in step S5, the stirring speed is 300 rpm.
Further, in step S6, the drying temperature was 42 ℃.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of high-water-dispersion astaxanthin ester microspheres is characterized by comprising the following steps:
s1, dissolving astaxanthin ester in an oil phase to prepare an oil phase, wherein the weight-volume ratio of the astaxanthin ester to the oil phase is 1: 20-1: 60 g/ml;
s2, dissolving sucrose cocoate in water to prepare a water phase; the feed-liquid ratio of the sucrose cocoate to the water is 1: 20-1: 25 g/ml;
s3, adding an emulsifier into the oil phase obtained in the S1, homogenizing for 1-3 times at 6000-8000 psi, adding the water phase obtained in the S2, mixing the oil phase and the water phase according to the volume ratio of 1: 16-1: 35, and dispersing for 2-4 min at 13000-15000 rpm/min to obtain a mixed solution;
s4, homogenizing the mixed solution obtained in the step S3 at 9000-12000 psi for 3-5 times to obtain an astaxanthin-sucrose cocoate emulsion;
s5, adding a high polymer carrier into the astaxanthin-sucrose cocoate emulsion obtained in the step S4, uniformly stirring at 20-25 ℃, dispersing at 14000-16000 rpm/min for 2-3 min, dropwise adding the dispersed liquid into a salt solution with the concentration of 0.2-3 mol/L after uniform dispersion, uniformly stirring at 20-25 ℃ in the dropwise adding process, stopping stirring after dropwise adding is finished, and standing for 30-60 min to coagulate and solidify the dispersed liquid;
s6, collecting the agglomerated pellets, cleaning, filtering and drying to prepare the high-water-dispersion astaxanthin ester microspheres.
2. The method for preparing high-water-dispersibility astaxanthin ester microspheres according to claim 1, wherein the oil phase is one or more of sweet orange flower oil, olive oil and soybean oil.
3. The method for preparing high-water-dispersion astaxanthin ester microspheres according to claim 1, wherein the emulsifier is one or more selected from monoglyceride, tween, lecithin, sucrose fatty acid ester, polyglycerol ester, sodium stearoyl lactylate and diacetyl tartaric acid monoglyceride and diglyceride.
4. The preparation method of the high-water-dispersion astaxanthin ester microspheres according to claim 1, wherein the mass ratio of the astaxanthin ester to the emulsifier is 1: 6-1: 15.
5. The method for preparing high-water-dispersibility astaxanthin ester microspheres according to claim 1, wherein the high-molecular carrier is a mixture of sodium alginate and one or more of gelatin, modified starch, pectin and cyclodextrin.
6. The preparation method of the high-water-dispersion astaxanthin ester microspheres according to claim 1, wherein the weight-volume ratio of the high-molecular carrier to the astaxanthin-sucrose cocoate emulsion is 1: 0.3-1: 5 g/L.
7. The preparation method of the high-water-dispersion astaxanthin ester microspheres according to claim 1, wherein solutes in the salt solution are sodium hypophosphite, magnesium aspartate and calcium chloride, and the mass ratio of the sodium hypophosphite to the magnesium aspartate to the calcium chloride is 1 (0.3-0.8) to 2-5.
8. The method for preparing high-water-dispersion astaxanthin ester microspheres according to claim 1, wherein in the step S5, ultrasonic treatment is performed before standing, and the ultrasonic treatment time is 1-3 min.
9. The method for preparing highly water-dispersible astaxanthin ester microspheres according to claim 1, wherein in the step S5, the stirring speed is 250-350 rpm.
10. The method for preparing highly dispersed astaxanthin ester microspheres according to claim 1, wherein the drying temperature in step S6 is 35-55 ℃.
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| CN2020114600209 | 2020-12-11 | ||
| CN202011460020.9A CN112494432A (en) | 2020-12-11 | 2020-12-11 | Preparation method of high-water-dispersion astaxanthin ester microspheres |
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| CN202110947392.2A Withdrawn CN113509444A (en) | 2020-12-11 | 2021-08-18 | Preparation method of high-water-dispersion astaxanthin ester microspheres |
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| CN113170885A (en) * | 2021-04-06 | 2021-07-27 | 大连工业大学 | Preparation method of microspheres for improving astaxanthin release rate based on fucoidin |
| CN113527530B (en) * | 2021-08-06 | 2022-04-29 | 青岛职业技术学院 | Preparation method of water-soluble astaxanthin fucoidin ester |
| CN114522139B (en) * | 2022-01-28 | 2023-09-15 | 深圳玉莱漫生物科技有限公司 | Herbal anti-inflammatory transdermal absorption microemulsion gel and preparation method thereof |
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