CN101971984A - Preparation method of DHA microemulsion - Google Patents

Preparation method of DHA microemulsion Download PDF

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Publication number
CN101971984A
CN101971984A CN2010102732186A CN201010273218A CN101971984A CN 101971984 A CN101971984 A CN 101971984A CN 2010102732186 A CN2010102732186 A CN 2010102732186A CN 201010273218 A CN201010273218 A CN 201010273218A CN 101971984 A CN101971984 A CN 101971984A
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China
Prior art keywords
dha
emulsifying agent
preparation
microemulsion
percent
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CN2010102732186A
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肖小年
易醒
侯小晶
刘媛洁
胡少华
曾海龙
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Nanchang University
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Nanchang University
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  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention relates to a preparation method of a DHA microemulsion which comprises the following components in percent by mass of 2-20 percent of DHA algae oil, 0-5 percent of dispersing agent, 15-35 percent of compound emulsifying agent, 5-15 percent of assisting emulsifying agent and the balance of deionized water. The preparation method comprises the steps of: uniformly stirring the algae oil, the dispersing agent, the compound emulsifying agent and the assisting emulsifying agent by using a magnetic stirrer according to the proportion; slowly dropping the deionized water at a temperature of 25-80 DEG C under the stirring and regulating the optimal stirring speed with the generation of phase change to obtain the DHA microemulsion. The prepared DHA microemulsion has less consumption of the emulsifying agent, particle diameter of 43nm-50nm, loading rate of 2-20 percent and entrapment rate of 75 percent.

Description

The preparation method of DHA microemulsion
Technical field
The present invention relates to a kind of preparation method of product novel form of the DHA of containing composition, belong to the health food preparation field.
Background technology
DHA i.e. 22 carbon, 60 olefin(e) acids, it is the polyunsaturated fatty acid of needed by human, it is a fatty acid composition important in brain, nerve and the cellula visualis, the normal performance of human body physiological function and the control of multiple disease there are important function, particularly in infant's brain and development of vision system process, occupy crucial status.To the adult, DHA keeps the indispensable material of the normal performance of cerebral function.Low DHA content diet can be accelerated the aging speed of human body, and causes suffering from senile dementia easily.But DHA also angiocardiopathy preventing takes place, and can play hypotensive function, and can regulate the eubolism of interior blood fat of human body and lipoprotein, reduces cholesterol levels in blood viscosity and the blood, increases hdl concentration.Prevention and treatment atherosclerotic can suppress tumor growth, and anti-inflammatory suppresses allergic reaction.
Owing to contain six unsaturated double-bonds in the molecular structure of DHA, therefore to oxygen, light and heat all are very responsive, oxidation takes place easily, and the DHA oxidation at first is exactly to cause content to reduce, and its effect is affected, secondly, oxidation product is harmful to health, and takes in the body to cause lipid peroxidation, thereby brings out various physically different diseases induced.In order to control the oxidation of DHA, improve its stability, make it be applied to easily go in normal food and the health food, the measure of taking at present mainly is to use antioxidant and microencapsulation.Traditional microcapsule formulation exists with solid form usually, can not use in liquid food, cosmetics, medicine, in addition, because the particle diameter of microcapsules is bigger, its biological utilisation is not very high, under the less situation of addition, is unfavorable for being implemented in the even distribution in the product yet.Simultaneously since microcapsules in the process of spray-dired preparation, the duration of high temperature and bigger contact area have promoted the fast oxidative generation of DHA.
Modern study shows, if employing nanoscale science and technology, DHA is made particle less than 100nm, the DHA nano particle can be directly by the oral cavity, mucous membranes such as nasal cavity directly absorb, thereby increase substantially the absorption of human body to DHA, especially the elderly that metabolic function is failed to some extent and metabolic function are grown perfect inadequately infant then effect are more obvious.
Chinese patent CN1466944A " preparation of the nano suspending liquid of DHA " discloses the preparation method of the nano suspending liquid of a kind of DHA: the solution of earlier DHA being made pure and mild polyalcohol, and with this solution stir and the ultrasonic vibration effect under slowly be added drop-wise in the big water gaging, after depositing, adopts certain hour the method for decompression distillation again, remove the organic solvent in the DHA suspension, can obtain the nano suspending liquid of DHA.This background technology exists the technological operation temperature higher, organic solvent residual, preparation method's complexity, the shortcoming that particle diameter is big.
Summary of the invention
The objective of the invention is to provide the preparation method of the water oil-packaging type micro-emulsion agent of a kind of DHA at the shortcoming of background technology.Its emulsifying agent consumption is less; the preparation method is simple; the medicine carrying amount is bigger, and particle is uniformly dispersed, and particle diameter is less; less than 50nm; stability better makes micro emulsion can cover the distinctive smell of algae oil preferably, and well protects DHA to avoid undesirable element influence in the environment; thereby produce harmful oxidation product, smaller particles can improve bioavilability.
Technical scheme of the present invention is: preparation DHA microemulsion used raw-material mass percent is: DHA algae oil 2%-20%, dispersant 0%-5%, compound emulsifying agent 15%-35%, assistant for emulsifying agent 5%-15%, all the other are deionized water.With algae oil, dispersant, compound emulsifying agent, assistant for emulsifying agent stirring and evenly mixing under magnetic stirring apparatus, slowly drip deionized water down by said ratio, stir while dripping at 25 ℃-80 ℃, generation along with phase transformation, accelerate mixing speed, finally obtain the DHA micro emulsion, its particle diameter is less than 50nm.
Compound emulsifying agent can be matched in Tween 80 (Tween80), polyoxyethylene (40) castor oil (Cremophor EL-40), polyoxyethylene (35) castor oil (Cremophor EL-35), polyoxyethylene (40) rilanit special (Cremophor RH-40), polyethylene glycol stearate 15 (HS-15), APEO rilanit special (CO-40), sorbester p17 (Span 80), lecithin, poloxamer, as: Tween 80 and Span 80, HS-15 and lecithin, EL-35 and Span 80.
Above-mentioned assistant for emulsifying agent is PEG400 (PEG-400), glycerine, 1,2-propane diols, absolute ethyl alcohol or n-butanol.
Above-mentioned dispersant is isopropyl myristate (IPM), ethyl acetate, ethyl oleate, peanut oil, olive oil or VE.
The invention has the beneficial effects as follows: technical process is simple, be convenient to tissue production, cost is low, the medicine carrying amount of the DHA of this microemulsion formulation reaches as high as 20%, the best medicine carrying scope that forms micro emulsion is at 10%-15%, micro emulsion particle diameter little (less than 50nm) and being evenly distributed can improve its bioavilability well, and centrifugal stability, high-temperature stability and intense light irradiation stability are all good.
The specific embodiment
Embodiment 1
DHA algae oil 0.1 gram, Tween80 0.85 gram, Span80 0.17 gram, n-butanol 0.2 gram, deionized water 2.2 grams.Get DHA algae oil 0.1 gram, Tween80 0.85 gram, Span80 0.17 gram, n-butanol 0.2 gram places same container, stirs under magnetic stirring apparatus, dropwise drips deionized water under 30 ℃, stirs while dripping, and adds deionized water 2.2 grams, promptly gets micro emulsion.
Embodiment 2
DHA algae oil 0.5 gram, Tween80 2.85 grams, Span80 0.60 gram, PEG-400 1.14 grams, deionized water 4.65 grams.Get DHA algae oil 0.5 gram, Tween80 2.85 grams, Span80 0.60 gram, PEG-400 1.14 grams place same container, stir under magnetic stirring apparatus, dropwise drip deionized water under 30 ℃, stir while dripping, add deionized water 4.65 grams, promptly get micro emulsion.
Embodiment 3
DHA algae oil 0.2 gram, EL-40 0.38 gram, Span80 0.13 gram, glycerine 0.5 gram, deionized water 1.55 grams.Get algae oil 0.2 gram, EL-40 0.38 gram, Span80 0.13 gram, glycerine 0.5 gram places same container, stirs under magnetic stirring apparatus, dropwise drips deionized water under 30 ℃, stirs while dripping, and adds deionized water 1.55 grams, promptly gets micro emulsion.
Embodiment 4
DHA algae oil 0.13 gram, HS-15 0.42 gram, EL-35 0.22 gram, PEG-400 0.2 gram, deionized water 3.71 grams.Get DHA algae oil 0.13 gram, HS-15 0.42 gram, EL-35 0.22 gram, PEG-400 0.2 gram places same container, stirs under magnetic stirring apparatus, dropwise drips deionized water under 30 ℃, stir while dripping, add deionized water 3.71 grams, promptly get micro emulsion.
Embodiment 5
DHA algae oil 0.1 gram, IPM oil 0.15 gram, RH-40 0.4 gram, EL-40 0.2 gram, absolute ethyl alcohol 0.2 gram, deionized water 2.45 grams.Get algae oil 0.1 gram, IPM oil 0.15 gram, RH-40 0.4 gram, EL-40 0.2 gram, absolute ethyl alcohol 0.2 gram places same container, stirs under magnetic stirring apparatus, dropwise drips deionized water under 50 ℃, stir while dripping, add deionized water 2.45 grams, promptly get micro emulsion.

Claims (4)

1. the preparation method of a DHA microemulsion is characterized in that:
(1) preparation DHA microemulsion used raw-material mass percent is: DHA algae oil 2%-20%, dispersant 0%-5%, compound emulsifying agent 15%-35%, assistant for emulsifying agent 5%-15%, all the other are deionized water;
(2) mass percent by (1) stirs DHA algae oil, dispersant, compound emulsifying agent, assistant for emulsifying agent under magnetic stirring apparatus, is under 25 ℃-80 ℃ in temperature, slowly drips deionized water, stir while dripping, along with phase transformation takes place, accelerate mixing speed, obtain the DHA micro emulsion.
2. according to the preparation method of right 1 described a kind of DHA microemulsion, it is characterized in that: compound emulsifying agent can be at Tween 80 (Tween80), polyoxyethylene (40) castor oil (Cremophor EL-40), polyoxyethylene (35) castor oil (CremophorEL-35), polyoxyethylene (40) rilanit special (Cremophor RH-40), polyethylene glycol stearate 15 (HS-15), APEO rilanit special (CO-40), sorbester p17 (Span80), lecithin, match in the poloxamer, as: Tween80 and Span80, HS-15 and lecithin, EL-35 and Span80.
3. the preparation method of a kind of DHA microemulsion according to claim 1 is characterized in that: assistant for emulsifying agent is polyethylene glycol-400 (PEG-400), glycerine, 1,2-propane diols, absolute ethyl alcohol or n-butanol.
4. the preparation method of a kind of DHA microemulsion according to claim 1 is characterized in that: dispersant is isopropyl myristate (IPM), ethyl acetate, ethyl oleate, peanut oil, olive oil or VE.
CN2010102732186A 2010-09-06 2010-09-06 Preparation method of DHA microemulsion Pending CN101971984A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102132882A (en) * 2011-03-01 2011-07-27 厦门汇盛生物有限公司 DHA (Docosahexaenoic Acid) emulsion, production method and application thereof
CN103230002A (en) * 2013-04-19 2013-08-07 浙江大学舟山海洋研究中心 DHA (docosahexaenoic acid) liposome preparation method
CN104287053A (en) * 2014-09-30 2015-01-21 杭州娃哈哈科技有限公司 Oil-in-water type water-soluble antioxidant compound and preparation method thereof
CN104920642A (en) * 2015-07-03 2015-09-23 山东省分析测试中心 Food-grade peony seed blend oil microemulsion and preparing method thereof
CN105534745A (en) * 2015-12-24 2016-05-04 杨永 Emulsified composition and application of emulsified composition to preparation of oil-water mutual-dissolution type natural rosemary antioxidant
CN105832666A (en) * 2016-04-15 2016-08-10 国家海洋局第三海洋研究所 Preparation method for DHA algae oil nanoemulsion
CN106072611A (en) * 2016-06-20 2016-11-09 威海百合生物技术股份有限公司 A kind of heterogeneous diluted composition containing unsaturated fatty acid
CN108576820A (en) * 2018-03-30 2018-09-28 广州富诺营养科技有限公司 A kind of algae oil DHA composite particles and preparation method thereof
CN109939068A (en) * 2019-05-06 2019-06-28 中国海洋大学 One kind having antioxidative nano-lipid emulsion and preparation method thereof
CN118104824A (en) * 2024-02-03 2024-05-31 王叔和生物医药(武汉)有限公司 Algae oil DHA liposome and preparation method thereof
CN118104824B (en) * 2024-02-03 2024-11-05 王叔和生物医药(武汉)有限公司 Algae oil DHA liposome and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1895222A (en) * 2006-06-16 2007-01-17 齐红 Production and use for micro-emulsion and its medicine-carrier preparation
CN101816420A (en) * 2010-03-12 2010-09-01 江南大学 Microemulsion polyunsaturated fatty acid product and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1895222A (en) * 2006-06-16 2007-01-17 齐红 Production and use for micro-emulsion and its medicine-carrier preparation
CN101816420A (en) * 2010-03-12 2010-09-01 江南大学 Microemulsion polyunsaturated fatty acid product and preparation method thereof

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102132882A (en) * 2011-03-01 2011-07-27 厦门汇盛生物有限公司 DHA (Docosahexaenoic Acid) emulsion, production method and application thereof
CN103230002A (en) * 2013-04-19 2013-08-07 浙江大学舟山海洋研究中心 DHA (docosahexaenoic acid) liposome preparation method
CN104287053B (en) * 2014-09-30 2018-05-29 杭州娃哈哈科技有限公司 A kind of emulsifying Water Soluble Compound antioxidant and preparation method thereof
CN104287053A (en) * 2014-09-30 2015-01-21 杭州娃哈哈科技有限公司 Oil-in-water type water-soluble antioxidant compound and preparation method thereof
CN104920642A (en) * 2015-07-03 2015-09-23 山东省分析测试中心 Food-grade peony seed blend oil microemulsion and preparing method thereof
CN104920642B (en) * 2015-07-03 2017-12-12 山东省分析测试中心 Food-grade peony seeds mediation oil Microemulsions For Use and preparation method thereof
CN105534745B (en) * 2015-12-24 2018-05-11 杨永 A kind of emulsification composition and its in the application for preparing grease and dissolving each other in the natural rosemary antioxidant of type
CN105534745A (en) * 2015-12-24 2016-05-04 杨永 Emulsified composition and application of emulsified composition to preparation of oil-water mutual-dissolution type natural rosemary antioxidant
CN105832666A (en) * 2016-04-15 2016-08-10 国家海洋局第三海洋研究所 Preparation method for DHA algae oil nanoemulsion
CN106072611A (en) * 2016-06-20 2016-11-09 威海百合生物技术股份有限公司 A kind of heterogeneous diluted composition containing unsaturated fatty acid
CN108576820A (en) * 2018-03-30 2018-09-28 广州富诺营养科技有限公司 A kind of algae oil DHA composite particles and preparation method thereof
CN109939068A (en) * 2019-05-06 2019-06-28 中国海洋大学 One kind having antioxidative nano-lipid emulsion and preparation method thereof
CN118104824A (en) * 2024-02-03 2024-05-31 王叔和生物医药(武汉)有限公司 Algae oil DHA liposome and preparation method thereof
CN118104824B (en) * 2024-02-03 2024-11-05 王叔和生物医药(武汉)有限公司 Algae oil DHA liposome and preparation method thereof

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Application publication date: 20110216