CN104905270A - Astaxanthin lipid microemulsion and preparation method thereof - Google Patents
Astaxanthin lipid microemulsion and preparation method thereof Download PDFInfo
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
- A61K9/1075—Microemulsions or submicron emulsions; Preconcentrates or solids thereof; Micelles, e.g. made of phospholipids or block copolymers
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- 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
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Abstract
The invention relates to an astaxanthin lipid microemulsion and a preparation method thereof, wherein the liquid ingredients comprise an oil phase, an aqueous phase, a surfactant, a co-surfactant, and an ingredient. The steps comprise: 1) mixing the lipid ingredients such as the oil phase, the surfactant and the co-surfactant in the formula, heating to a temperature of 28-45 DEG C, and melting to obtain a liquid-state oily solution; 2) adding the formula amount of astaxanthin to the liquid-state oily solution; 3) adding the aqueous phase required by complementing to the emulsified emulsion; and 4), and finally cooling to a room temperature to obtain the astaxanthin lipid microemulsion product. According to the present invention, the preparation method is simple, the process is easy to learn and easy to understand, the while technology is easy to master, other advantages are provided, and the microemulsion of the present invention can be dissolved in water in any proportions, has characteristics of high stability and high bioavailability, and can be widely used as the main material or ingredient in the fields of medicine, food, health products, and the like.
Description
Technical field
The present invention relates to the technical field that astaxanthin carries out deep processing, specifically
oneplant astaxanthin lipid micro emulsion formula and emulsification preparation thereof thereof.
Background technology
Astaxanthin (astaxanthin), have another name called astaxanthin, Astaxanthin, being a Carotenoids, is also the highest level product of carrotene synthesis, in rediance, chemical constitution is similar to beta carotene, astaxanthin chemical name: 3,3 '-dihydroxy-4,4 '-diketo β, β '-carotenoid, pigment molecular formula C
40h
52o
4, molecular weight is 596.86.Due to hydroxyl (-OH) the optical activity reason at two ends, astaxanthin has 3S-3 ' S, 3R-3'S, 3R-3'R(also referred to as left-handed, meso, dextrorotation) these 3 kinds of isomery kenels.
The source of astaxanthin: the approach such as shrimp, crab, fish, frond, yeast, bird plumage, Prof. Du Yucang, wherein Prof. Du Yucang astaxanthin is that the mixture of 3 kinds of structure astaxanthins (left-handedly accounts for 25%, dextrorotation accounts for 25%, meso about 50%), astaxanthin (based on transconfiguration 3S-3 S type) in the organism of salmon, salmon and algae etc., the astaxanthin in saccharomycete source is 100% dextrorotation (3R-3'R).
Astaxanthin existence: dibasic acid esters, monoesters, free three kinds, the wherein carboxyl (COOH) at single dibasic acid esters mainly astaxanthin hydroxyl (-OH) long-chain and unrighted acid two ends, generated by esterification, another kind of dissociating is exactly be not combined with any aliphatic acid, astaxanthin run into as: under the conditions such as high temperature, intense light irradiation, strong acid, highly basic, ozone, oxygen, ultraviolet, active oxygen, proterties is all unstable, and be very easily decomposed, it is all have very high technical requirement that all preservations or development and usage contain astaxanthin product.
About the progress situation of astaxanthin is summarized as follows:
1, astaxanthin is a kind of superpower antioxidant, its superpower oxidation resistance: 550 times of vitamin E, 25 times of Co-Q10,50 times of bata-carotene, 200 times of lutein, 450 times of luteole.
2, the physiological function of astaxanthin: the protective effect of antioxidation, antitumaous effect, eye central nervous system, delay jet lag, strengthen immunization, prevent ultraviolet radiation, protection cardiovascular health etc.The application of astaxanthin in aquaculture: raising fish and poultry propagation ability, the effect of showing signs of anger of cultured fishes brilliance, the nutritive value improving cultivation object, improvement cultivate object physiological function.
Astaxanthin has so powerful function, domestic and international Ge great scientific research institutions are become in recent years, colleges and universities and enterprise try to be the first the scientific research project of research and probe, but resting on the source that how to expand astaxanthin as shrimp toward contact, crab, fish, frond, yeast, bird plumage, the approach such as Prof. Du Yucang, output is accomplished maximize, what produce is all that some contain the pulvis of astaxanthin or the primary product of finish, but astaxanthin is a kind of fat-soluble material, if product directly directly eats as the mankind or animal, or as skin care item, so astaxanthin in vivo or body surface will form a large amount of oil droplet vacuole shape, only has part by solution environmental solution absorption immediately, major part can only be leaned on by for a long time or more complicated Physiology and biochemistry decomposition reaction, last just to be absorbed by the approach such as permeating or engulf by cell, because the effect after utilizing astaxanthin like this can not timely and effectively display, need to adhere to for a long time feeding, take and smear.But along with the fast development of social life rhythm, if the effect of astaxanthin can not manifest fast, astaxanthin product is with one to twice, will be considered to no effect, can not re-use, businessman or consumer will successively decrease gradually, finally the phenomenon causing production astaxanthin R&D institution or enterprise's production capacity atrophy even to occur closing down are occurred.
So how to improve the utilization rate of astaxanthin and set up astaxanthin Application way, will be the most crucial technical problem of at present and in the future astaxanthin industry, it be by the development scale of guiding whole industry and process.
At present, for some polarity or the insoluble material of nonpolar extreme, by the front line science technical finesse such as compression, cut-out, emulsification of strand, obtain ideal utilizing status.Wherein lipid nano particle (Solid lipid nanoparticles, SLN) be the submicron delivery system of new generation grown up early 1990s, refer to that particle diameter is at 10 ~ 1000 nm, with the lipoid of solid natural or synthesis as lecithin, triacylglycerols etc. are carrier, medicine is wrapped up or clamps the solid micelle delivery system made in lipoid core, low with toxicity, good biocompatibility, the lipoid of biodegradable solid natural or synthesis is carrier, by Drug absorbability or be wrapped in the nanoparticle delivery system of new generation made in lipid film, having can Drug controlled release, avoid the degraded of medicine or the advantage such as leakage and good targeting.Large-scale production is carried out by high-pressure stripping.
SLN advantage is as follows: 1, Drug controlled release and target; 2, medicine stability is increased; 3, drugloading rate is high; 4, a year Lipophilicity medicine can be wrapped; 5, carrier toxicity is little; 6, some method (high-pressure stripping) can avoid the use of organic solvent; 7, produce and can amplify, can be used for industrial production.
Summary of the invention
Order of the present invention is the problem in order to solve existing for above-mentioned prior art, in conjunction with lipid nano particle technology, invents a kind of astaxanthin lipid micro emulsion and preparation method thereof, thoroughly solves the Utilizing question of astaxanthin product.
The present invention is achieved by the following technical solution:
A kind of astaxanthin lipid micro emulsion, lipid ingredient of the present invention comprises oil phase, aqueous phase, surfactant, cosurfactant, batching; Wherein oil phase is, saturated fatty acid: adopt palmitic acid or stearic acid; Unrighted acid: adopt the one or more combination comprised in oleic acid, linoleic acid, leukotrienes, omega-3 aliphatic acid, omega-6 aliphatic acid, omega-9 aliphatic acid, DHA, eicosapentaenoic acid, arachidonic acid to form, content is 10% ~ 30% of whole micro emulsion formulation weight percentage.;
Wherein aqueous phase is: the one or more combination of being steamed in water by pure water, ultra-pure water, distilled water, kind is formed, and content is 10% ~ 35% of whole micro emulsion formulation weight percentage;
Wherein surfactant is: anion surfactant adopts stearic acid or neopelex, cationic surfactant adopts quaternary ammonium compound or zwitterionic surfactant: any one in lecithin, amino acid pattern, betaine type; Non-ionic surface active agent adopts that fatty glyceride, aliphatic acid sorb are smooth, one or more combination in polysorbate is formed; Content is 0.1% ~ 0.15% of whole micro emulsion formulation weight percentage;
Wherein cosurfactant is: ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, 1-hexanol, 2-hexanol, 1-octanol, sec-n-octyl alcohol, 1, one or more any combination in 2 propane diols, glycerine, fusel oil, n nonylphenol etc., content is more than 30% of whole micro emulsion formulation weight percentage;
Wherein batching is astaxanthin, and described astaxanthin comprises: the one or more combination in shrimp and crab shells extract, microalgae extract, yeast extract, artificial chemical industry synthetic is formed, and content is 5% ~ 20% of whole micro emulsion formulation weight percentage;
A kind of emulsification processing preparation according to above-mentioned a kind of astaxanthin lipid micro emulsion formula: step is:
1) after lipid ingredient oil phase, surfactant and cosurfactant mixing in formula, be heated to 28 to 45 degrees Celsius, after molten molten, obtain liquid oily solution;
2), the astaxanthin of formula consumption is joined in liquid oily solution, and be uniformly mixed, by one or more in high energy emulsion process (in high-speed cutting or pressure homogeneous or sonic oscillation one or more), low-energy emulsification method (in phase temperature-switching method or phase inversion one or both) with the use of (one-level emulsification), the time of process is stage batch (-type): 1 second to 50 seconds, 1 little of more than the 2 times circular treatment such as 1.5 hours, is all in the water bath with thermostatic control of 30 ~ 40 degrees Celsius in whole emulsion process;
3), then need the aqueous phase supplied to join in the good emulsion of emulsification by formula, and carry out secondary emulsification treatment, the processing time is 1 ~ 5 time, each 50 seconds;
4), last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
the present invention has the following advantages compared with the prior art:
Preparation method of the present invention is simple, and flow process is easily learnt well and understood, the advantage that a whole set of technology is easily grasped etc.
Micro emulsion of the present invention can dissolve each other with the water of arbitrary proportion, and stability is high, bioavailability is high, and the fields such as medicine, food, health products that can be widely used in use as major ingredient or batching.
The present invention is applicable to family's workshop trial-production or industrial-scale production.
The present invention uses batching to be badly in need of indispensable source material in organism, all applicable to the organism of any physique, can not produce any side effect.
The particle size range of lipid micro emulsion grain of the present invention: 10 ~ 100 nanometers.
The present invention the processing instrument and equipment that is suitable for be all conventional common, be very beneficial to industrialization development.
Below in conjunction with the drawings and specific embodiments, the present invention is further explained.
Accompanying drawing explanation
Fig. 1 is preparation method's schematic diagram of invention.
Detailed description of the invention
Order of the present invention is the problem in order to solve existing for above-mentioned prior art, in conjunction with lipid nano particle technology, invents a kind of astaxanthin lipid micro emulsion and preparation method thereof, thoroughly solves the Utilizing question of astaxanthin product.
the present invention is achieved by the following technical solution:
A kind of astaxanthin lipid micro emulsion, lipid ingredient of the present invention comprises oil phase, aqueous phase, surfactant, cosurfactant, batching; Wherein oil phase is, saturated fatty acid: adopt palmitic acid or stearic acid; Unrighted acid: adopt the one or more combination comprised in oleic acid, linoleic acid, leukotrienes, omega-3 aliphatic acid, omega-6 aliphatic acid, omega-9 aliphatic acid, DHA, eicosapentaenoic acid, arachidonic acid to form, content is 10% ~ 30% of whole micro emulsion formulation weight percentage.;
Wherein aqueous phase is: the one or more combination of being steamed in water by pure water, ultra-pure water, distilled water, kind is formed, and content is 10% ~ 35% of whole micro emulsion formulation weight percentage;
Wherein surfactant is: anion surfactant adopts stearic acid or neopelex, cationic surfactant adopts quaternary ammonium compound or zwitterionic surfactant: any one in lecithin, amino acid pattern, betaine type; Non-ionic surface active agent adopts that fatty glyceride, aliphatic acid sorb are smooth, one or more combination in polysorbate is formed; Content is 0.1% ~ 0.15% of whole micro emulsion formulation weight percentage;
Wherein cosurfactant is: ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, 1-hexanol, 2-hexanol, 1-octanol, sec-n-octyl alcohol, 1, one or more any combination in 2 propane diols, glycerine, fusel oil, n nonylphenol etc., content is more than 30% of whole micro emulsion formulation weight percentage;
Wherein batching is astaxanthin, and described astaxanthin comprises: the one or more combination in shrimp and crab shells extract, microalgae extract, yeast extract, artificial chemical industry synthetic is formed, and content is 5% ~ 20% of whole micro emulsion formulation weight percentage;
A kind of emulsification processing preparation according to above-mentioned a kind of astaxanthin lipid micro emulsion formula: step is:
1) after lipid ingredient oil phase, surfactant and cosurfactant mixing in formula, be heated to 28 to 45 degrees Celsius, after molten molten, obtain liquid oily solution;
2), the astaxanthin of formula consumption is joined in liquid oily solution, and be uniformly mixed, by one or more in high energy emulsion process (in high-speed cutting or pressure homogeneous or sonic oscillation one or more), low-energy emulsification method (in phase temperature-switching method or phase inversion one or both) with the use of (one-level emulsification), the time of process is stage batch (-type): 1 second to 50 seconds, 1 little of more than the 2 times circular treatment such as 1.5 hours, is all in the water bath with thermostatic control of 30 ~ 40 degrees Celsius in whole emulsion process;
3), then need the aqueous phase supplied to join in the good emulsion of emulsification by formula, and carry out secondary emulsification treatment, the processing time is 1 ~ 5 time, each 50 seconds;
4), last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
embodiment one
1, the lipid micro emulsion 1000 grams that prescription is 2% content astaxanthin is designed.
2, the oil phase in prescription chooses sour palmitic acid 50 grams, linoleic acid 150 grams, omega-fatty acid 100 grams.
3, the activating agent in prescription: Fabaceous Lecithin 10 grams chosen by surfactant, glycerine 300 grams chosen by cosurfactant.
4, the astaxanthin in prescription: select 10% haematococcus pluvialis extract astaxanthin 200 grams.
5, by after batching mixing selected by above-mentioned oil phase, activating agent, be heated to 40 degrees Celsius, after molten molten, obtain liquid oily solution.
6, astaxanthin is joined in liquid oily solution, and be uniformly mixed, be stage batch (-type) by the time of high energy emulsion process high speed cutting process (one-level emulsification), process: and batch process 3 times is each 50 seconds, is all in the water bath with thermostatic control of 35 degrees Celsius in whole emulsion process.
7, then supply the super purified water of surplus normal temperature by prescription 1 kilogram quantities, and carry out secondary emulsification treatment, the processing time is 1 to 5 time, each 50 seconds.
8, last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
embodiment two
1, the lipid micro emulsion 500 grams that prescription is 3% content astaxanthin is designed.
2, the oil phase in prescription chooses sour stearic acid 10 grams, leukotrienes 15 grams, omega-fatty acid 25 grams;
3, the activating agent in prescription: Fabaceous Lecithin 3 grams chosen by surfactant, and cosurfactant chooses 1,2 propane diols 150 grams;
4, the astaxanthin in prescription: select 10% haematococcus pluvialis extract astaxanthin 150 grams.
5, by after batching mixing selected by above-mentioned oil phase, activating agent, are heated to 40 degrees Celsius, obtain liquid oily solution after molten molten.
6, astaxanthin is joined in liquid oily solution, and be uniformly mixed, be stage batch (-type) by the time of the cutting process of high energy emulsion process high speed, process: 50 seconds and batch process 3 times, be all in the water bath with thermostatic control of 35 degrees Celsius in whole emulsion process.
7, then supply ultra-pure water by prescription 500 gram quantity, and carry out secondary emulsification treatment, the processing time is 1 to 3 time, each 50 seconds.
8, last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
embodiment three
1, the lipid micro emulsion 1000 grams that prescription is 5% content astaxanthin is designed.
2, the oil phase in prescription chooses sour stearic acid 5 grams, palmitic acid 10 grams, leukotrienes 10 grams, linoleic acid 10 grams, omega-fatty acid 10 grams;
3, the activating agent in prescription: Fabaceous Lecithin 3 grams chosen by surfactant, glycerine 350 grams chosen by cosurfactant;
4, the astaxanthin in prescription: select 10% haematococcus pluvialis extract astaxanthin 500 grams.
5, by after batching mixing selected by above-mentioned oil phase, activating agent, be heated to 40 degrees Celsius, after molten molten, obtain liquid oily solution.
6, astaxanthin is joined in liquid oily solution, and be uniformly mixed, be stage batch (-type) by the time of the cutting process of high energy emulsion process high speed, process: and batch process 5 times 50 seconds, be all in the water bath with thermostatic control of 35 degrees Celsius in whole emulsion process.
7, then supply normal temperature ultra-pure water by prescription 1000 gram quantity, and carry out secondary emulsification treatment, the processing time is 1 to 5 time, each 50 seconds.
8, last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
Execute result astaxanthin lipid of the present invention micro emulsion of example and preparation method thereof, process stabilizing, method is reliable, technology maturation, strong technical support is provided for applying astaxanthin lipid micro emulsion product, the bioavilability of astaxanthin improves the order of magnitude of several geometry level simultaneously, promotes the quick healthy growth of whole astaxanthin industry.
Claims (2)
1. an astaxanthin lipid micro emulsion, lipid ingredient of the present invention comprises oil phase, aqueous phase, surfactant, cosurfactant, batching;
Wherein oil phase is, saturated fatty acid: adopt palmitic acid or stearic acid; Unrighted acid: adopt the one or more combination comprised in oleic acid, linoleic acid, leukotrienes, omega-3 aliphatic acid, omega-6 aliphatic acid, omega-9 aliphatic acid, DHA, eicosapentaenoic acid, arachidonic acid to form, content is 10% ~ 30% of whole micro emulsion formulation weight percentage;
Wherein aqueous phase is: the one or more combination of being steamed in water by pure water, ultra-pure water, distilled water, kind is formed, and content is 10% ~ 35% of whole micro emulsion formulation weight percentage;
Wherein surfactant is: anion surfactant adopts stearic acid or neopelex, cationic surfactant adopts quaternary ammonium compound or zwitterionic surfactant: any one in lecithin, amino acid pattern, betaine type; Non-ionic surface active agent adopts that fatty glyceride, aliphatic acid sorb are smooth, one or more combination in polysorbate is formed; Content is 0.1% ~ 0.15% of whole micro emulsion formulation weight percentage;
Wherein cosurfactant is: ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, 1-hexanol, 2-hexanol, 1-octanol, sec-n-octyl alcohol, 1, one or more any combination in 2 propane diols, glycerine, fusel oil, n nonylphenol etc., content is more than 30% of whole micro emulsion formulation weight percentage;
Wherein batching is astaxanthin, and described astaxanthin comprises: the one or more combination in shrimp and crab shells extract, microalgae extract, yeast extract, artificial chemical industry synthetic is formed, and content is 5% ~ 20% of whole micro emulsion formulation weight percentage.
2. the emulsification preparation thereof of a kind of astaxanthin lipid micro emulsion according to claim 1, it is characterized in that, step is:
1) after lipid ingredient oil phase, surfactant and cosurfactant mixing in formula, be heated to 28 to 45 degrees Celsius, after molten molten, obtain liquid oily solution;
2), the astaxanthin of formula consumption is joined in liquid oily solution, and be uniformly mixed, by one or more in high energy emulsion process, low-energy emulsification method with the use of, the time of process is stage batch (-type): 1 second to 50 seconds, 1 little of more than the 2 times circular treatment such as 1.5 hours, is all in the water bath with thermostatic control of 30 ~ 40 degrees Celsius in whole emulsion process;
3), then need the aqueous phase supplied to join in the good emulsion of emulsification by formula, and carry out secondary emulsification treatment, the processing time is 1 ~ 5 time, each 50 seconds;
4), last cool to room temperature can obtain astaxanthin lipid micro emulsion product.
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CN105123990A (en) * | 2015-10-08 | 2015-12-09 | 河南工业大学 | Method for preparing stable type sesamol microemulsion |
CN107048405A (en) * | 2017-03-03 | 2017-08-18 | 武汉锶博睿医药技术有限公司 | Aliphatic acid component microcapsules and preparation method thereof |
CN108578365A (en) * | 2018-05-22 | 2018-09-28 | 潍坊医学院 | A kind of astaxanthin enteral nutrition emulsion, dried emulsifier and its preparation method and application |
CN109771374A (en) * | 2019-03-29 | 2019-05-21 | 广东现代汉方科技有限公司 | Compound Astaxanthin In Haematococcus Pluvialis fat emulsion formulation and the preparation method and application thereof |
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CN112586624A (en) * | 2020-12-24 | 2021-04-02 | 日照职业技术学院 | Pet nutrition paste prepared from euphausia superba lipid and preparation method thereof |
CN113616537A (en) * | 2021-09-03 | 2021-11-09 | 中国海洋大学 | Astaxanthin nanoemulsion freeze-dried powder and preparation method and application thereof |
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CN105123990A (en) * | 2015-10-08 | 2015-12-09 | 河南工业大学 | Method for preparing stable type sesamol microemulsion |
CN105123990B (en) * | 2015-10-08 | 2021-08-06 | 河南工业大学 | Method for preparing stable sesamol microemulsion |
CN107048405A (en) * | 2017-03-03 | 2017-08-18 | 武汉锶博睿医药技术有限公司 | Aliphatic acid component microcapsules and preparation method thereof |
CN108578365A (en) * | 2018-05-22 | 2018-09-28 | 潍坊医学院 | A kind of astaxanthin enteral nutrition emulsion, dried emulsifier and its preparation method and application |
CN109771374A (en) * | 2019-03-29 | 2019-05-21 | 广东现代汉方科技有限公司 | Compound Astaxanthin In Haematococcus Pluvialis fat emulsion formulation and the preparation method and application thereof |
CN109771374B (en) * | 2019-03-29 | 2021-07-20 | 广东现代汉方科技有限公司 | Composite haematococcus pluvialis astaxanthin fat emulsion preparation and preparation method and application thereof |
CN110151668A (en) * | 2019-06-28 | 2019-08-23 | 日照职业技术学院 | A kind of high biological value astaxanthin cosmetics |
CN112586624A (en) * | 2020-12-24 | 2021-04-02 | 日照职业技术学院 | Pet nutrition paste prepared from euphausia superba lipid and preparation method thereof |
CN113616537A (en) * | 2021-09-03 | 2021-11-09 | 中国海洋大学 | Astaxanthin nanoemulsion freeze-dried powder and preparation method and application thereof |
CN113616537B (en) * | 2021-09-03 | 2022-08-30 | 中国海洋大学 | Astaxanthin nanoemulsion freeze-dried powder and preparation method and application thereof |
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