CN101406442B - Nanometer lipid sun-prevention microparticle suspending liquid and preparation method thereof - Google Patents
Nanometer lipid sun-prevention microparticle suspending liquid and preparation method thereof Download PDFInfo
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- CN101406442B CN101406442B CN2008102032779A CN200810203277A CN101406442B CN 101406442 B CN101406442 B CN 101406442B CN 2008102032779 A CN2008102032779 A CN 2008102032779A CN 200810203277 A CN200810203277 A CN 200810203277A CN 101406442 B CN101406442 B CN 101406442B
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Abstract
The invention discloses nanometer lipid sunblocking particle suspension fluid and a preparation method thereof. The nanometer lipid sunblocking particle suspension fluid consists of a UVA sunscreen agent, a UVB sunscreen agent, solid lipid, an emulsifier, a preservative and water. The preparation method comprises the following steps: the solid lipid, the emulsifier and the sunscreen agents are melted and dispersed evenly at a temperature of between 65 and 95 DEG C to obtain an evenly dispersed oil phase, and components of the oil phase are mixed evenly with water and then are cooled down to finally form the nanometer lipid sunblocking particle suspension fluid. In order to prevent the permeability of the chemical sunscreen agents on the skin, the particle diameter of lipid particles can not be too small; the lipid particles can be prepared through a common homogenous technology; and the preparation method has a simple process, few steps, and an easily controlled course. The method avoids high-pressure homogenizing and has safer operation. The particle diameter of the particles in the nanometer lipid sunblocking particle suspension fluid is between 80nm and 500nm, wherein the particle diameter between 100nm and 300nm is preferred. The nanometer lipid sunblocking particle suspension fluid has a sunscreen function within the wavelength coverage between 290nm and 400nm.
Description
Technical field
The present invention relates to a kind of nanometer lipid sun-prevention microparticle suspending liquid and preparation method thereof.
Background technology
The chemistry sunscreen mainly is meant the organic compound with the ultraviolet radiation that can be absorbed with injury effect, is commonly referred to chemical ultraviolet absorbent.Different according to the radiating wave band of protection, UV (ultraviolet) absorbent can be divided into UVA (life ultraviolet) and two kinds of absorbent of UVB (outdoor ultraviolet).Can be divided into para-amino benzoic acid and esters, salicylic acid esters and derivant thereof, o-aminobenzoa class, benzophenone and derivant thereof, p-methoxycinnamic acid class, methane Derivatives etc. on the chemical constitution.Be applied to the chemical sunscreen in the cosmetics because its photo-labile property and to the zest of skin can produce certain side effect, belong at European Union's part sunscreen and limit the use of raw material, the part sunscreen then belongs to the forbidding raw material.Simultaneously, general sunscreen only has anti-sunlight function in a kind of wavelength band to UVA or UVB wave band.
Solid lipid microgranule (SLN) is a solid lipid higher with fusing point, good biocompatibility; Like polyunsaturated fatty acid ester, fatty acid, aliphatic alcohol, mixed ester, wherein one or more mixture are carrier material, with the emulsifying agent stably dispersing; A kind of newtype drug slow-released carrier that forms; Mainly be applicable to the coating of close ester property active component, also can coat again after the hydroaropic substance elder generation formation Water-In-Oil system.SLN can effectively control the release of active component; The good biocompatibility of carrier material.Can realize coating, improve the safety of using the skin irritation material.
The solid lipid sun-prevention microparticle is to coat the sun-screening agent that two kinds of chemical sunscreen (sun-proof and a kind of UVB of a kind of UVA is sun-proof) make through the utilization solid lipid nanoparticle, and its anti-sunlight function is formed by two kinds of chemical sunscreen and lipid particles Synergistic.The solid lipid sun-prevention microparticle that has coated chemical sunscreen has the triple function of absorption, scattering and uv reflectance; The chemistry sunscreen is through the coating effect of lipid particles; In being applied to the process of cosmetics; Avoided contacting, can reduce the zest of chemical sunscreen greatly, anti-sunlight function has all been arranged in the broadband scope simultaneously skin with the direct of skin.
The classic methods of preparation solid lipid microgranule is high pressure homogenization method and microemulsion method, and high pressure homogenization method divides thermally homogenising and cold homogenizing, and these two kinds of methods all need high pressure homogenize, complicated steps, but be prone to make the less lipid particles of particle diameter through high pressure homogenize.Microemulsion method equipment is simple, and energy consumption is low, but owing to exist microemulsion dilution dispersive process to make that the dispersion liquid solid content is low, and need to use a large amount of emulsifying agent and coemulsifier.The lipid particles that makes through different preparation technologies respectively has its pluses and minuses.
The preparation of at present domestic disclosed relevant nano-lipid microgranule is mainly used in the coating medicine active component, is used to coat the cosmetic active component seldom, and the Shang Weijian that coats sunscreen is open.
Summary of the invention
A kind of nanometer lipid sun-prevention microparticle suspending liquid and preparation method thereof that provides of the present invention.
The technical scheme that the present invention adopts is:
A kind of nanometer lipid sun-prevention agent microparticle suspending liquid, its composition is following by weight percentage:
UVA sunscreen 0.1~20%
UVB sunscreen 0.1~20%
Solid lipid 2~20%
Emulsifying agent 1~15%
Antiseptic 0.01~1%
Water surplus
Wherein solid lipid is that one or several of fatty acid, aliphatic alcohol, fatty glyceride, native paraffin or synthetic wax is compound; Fatty acid is dodecoic acid, tetradecylic acid or stearic acid; Aliphatic alcohol is hexadecanol, octadecanol or 22 carbon alcohol; Fatty glyceride is glyceryl monostearate, glycerol disterate fat or glycerine tristearate; Native paraffin or synthetic wax are Cera Flava, ceresine, paraffin.
Described emulsifying agent is one of sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, fatty alcohol-polyoxyethylene ether, cithrol, ethoxylated castor oil, glycerine monofatty ester, polyglycerin ester, sucrose monostearate;
Described UVA sunscreen is one of o-aminobenzoa class, benzophenone and derivant thereof, methane Derivatives: wherein the o-aminobenzoa class is one of Antisolaire or N-acetyl group ortho-aminobenzoic acid 3-methyl cyclohexanol ester;
Described benzophenone and derivant thereof are 2-hydroxyl-4-methoxyl group benzophenone, 2; 2 '-dihydroxy-4-methoxyl group benzophenone, 2-hydroxyl-4-methoxyl group benzophenone-5-sulfonic acid, 2,4 '-dihydroxy benzophenone, 2,2 '; 2; 4 '-tetrahydroxybenzophenone, 2,2 '-dihydroxy-4, one of 4 '-dimethoxy benzophenone or 2-hydroxyl-4-N-ethylhexyl benzophenone;
Described methane Derivatives is 4-methyl-4-ethoxybenzene formyl methane or butyl methoxydibenzoylmethise;
Described UVB sunscreen is one of para-amino benzoic acid and esters, salicylic acid esters and derivant, benzophenone and derivant thereof, p-methoxycinnamic acid class, Camphora class;
Wherein para-amino benzoic acid and esters thereof are para-amino benzoic acid, para-amino benzoic acid glyceride, N, N-amyl dimethyl paraaminobenzoic acid, two (hydroxypropyl) Aminobenzoates of ethyl-4-or N, one of N-octyl dimethyl p-aminobenzoic acid;
Described salicylic acid esters and derivant thereof are one of phenyl salicytate, benzyl salicylate, menthyl salicylate or p-isopropyl phenyl salicylate;
Described benzophenone and derivant thereof are 2-hydroxyl-4-methoxyl group benzophenone, 2; 2 '-dihydroxy-4-methoxyl group benzophenone, 2-hydroxyl-4-methoxyl group benzophenone-5-sulfonic acid, 2,4 '-dihydroxy benzophenone, 2,2 '; 2; 4 '-tetrahydroxybenzophenone, 2,2 '-dihydroxy-4, one of 4 '-dimethoxy benzophenone or 2-hydroxyl-4-N-ethylhexyl benzophenone.
Described p-methoxycinnamic acid class is methyl cinnamic acid monooctyl ester or ethylhexyl methoxy cinnamate;
Described antiseptic is parabens, benzyl alcohol, phenyl phenol, 2-bromo-2-nitropropane-1, one of ammediol (Bronopol), imidazolidinyl urea, dehydroacetic acid, sorbic acid, Kazon, glyceryl monolaurate, diazonium ureine, methylol glycolylurea, dihydroxymethyl DMH.
A kind of method for preparing of nanometer lipid sun-prevention agent microparticle suspending liquid is characterized in that comprising being prepared as follows step:
(1) solid lipid, emulsifying agent and sunscreen obtain finely dispersed oil phase 65~95 ℃ of fusions and be uniformly dispersed;
(2) oil-phase component and the water intimate mixing between 65~95 ℃ that step (1) are obtained,
Homogenizing speed during mixing is at 8000~20000 rev/mins, and homogenizing time was at 2~10 minutes;
(3) cooling, the time cooled to 40~60 ℃ at 30 minutes~1 hour, and mixing speed adds antiseptic at 100~700 rev/mins in the cooling procedure;
(4) continue cooling, mixing speed cools to 25~30 ℃ of room temperatures at 100~700 rev/mins in the cooling procedure, finally forms the suspension of nanometer lipid sun-prevention agent microgranule.
The raw material that the present invention adopts like solid lipid, sunscreen, emulsifying agent and antiseptic, is raw material commonly used in the cosmetics, can be used for the raw material of nanometer lipid sun-prevention agent.
Beneficial effect of the present invention
Because for fear of the permeability of chemical sunscreen on skin, the particle diameter of lipid particles is difficult for too little, can use common homogeneous technology to prepare lipid particles; Technology is simple, and step is few, and process is easy to control; Avoided high pressure homogenize, operated safelyr, the particle diameter of microgranule is between 80nm~500nm in the nanometer lipid sun-prevention agent microparticle suspending liquid of gained; Preferred 100nm~300nm has anti-sunlight function in 290nm~400nm wave-length coverage.
Description of drawings
Fig. 1 is the sem photograph of microgranule in the nanometer lipid sun-prevention microparticle suspending liquid
Fig. 2 is the particle size distribution figure of microgranule in the nanometer lipid sun-prevention microparticle suspending liquid
Fig. 3 is the Zeta potential scattergram of microgranule in the nanometer lipid sun-prevention microparticle suspending liquid
The specific embodiment
Below in conjunction with instantiation the present invention is done to further describe, but protection scope of the present invention is not limited in this:
Instance 1:
Take by weighing 3.0g monoglyceride, 5.0g PEG-20 sorbitan monooleate, the sad capric acid triglyceride of 4.0g, 3.0g methyl cinnamic acid monooctyl ester, 2.0g Antisolaire respectively in the oil phase beaker; Take by weighing distilled water 83.0g again in the water beaker, heat oil phase and water to 85 ℃ respectively, in 8000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 2 minutes; Mixing speed is 100 rev/mins; When the system of treating is cooled to 40 ℃, add the 0.2g imidazolidinyl urea, restir is cooled to room temperature and gets final product for 25 ℃.
Instance 2:
Take by weighing 2.0g monoglyceride, 5.0g sorbitan monooleate, 2.0g isopropyl palmitate, 2.0 Antisolaires, 4.0g 2-hydroxyl-4-methoxyl group benzophenone respectively in the oil phase beaker; Take by weighing distilled water 85.0g again in the water beaker, heat oil phase and water to 90 ℃ respectively, in 10000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 3 minutes; Mixing speed is 300 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.2g phenyl phenol, restir is cooled to room temperature and gets final product for 30 ℃.
Instance 3:
Take by weighing 2.0g monoglyceride, 4.0g PEG-20 sorbitan monostearate, 4.0g isopropyl palmitate, 4.0g N respectively, N-octyl dimethyl p-aminobenzoic acid, 2.0g 4-methyl-4-ethoxybenzene formyl methane are in the oil phase beaker; Take by weighing distilled water 84.0g again in the water beaker, heat oil phase and water to 80 ℃ respectively, in 15000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 4 minutes; Mixing speed is 600 rev/mins; When the system of treating is cooled to 60 ℃, add the 0.2g imidazolidinyl urea, restir is cooled to room temperature and gets final product for 25 ℃.
Instance 4:
Take by weighing 4.0g monoglyceride, 2.0g sorbitan monostearate, 2.0g isopropyl myristate, 3.0g butyl methoxydibenzoylmethise, 5.0g 2-hydroxyl-4-methoxyl group benzophenone respectively in the oil phase beaker; Take by weighing distilled water 84.0g again in the water beaker, heat oil phase and water to 90 ℃ respectively, in 20000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 2 minutes; Mixing speed is 700 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.2g imidazolidinyl urea, restir is cooled to room temperature and gets final product for 30 ℃.
Instance 5:
Take by weighing 2.0g hexadecanol, the stearic alcohol ether-2 of 2.0g, the sad capric acid triglyceride of 4.0g, 3.0g butyl methoxydibenzoylmethise, 5.0g N respectively, the N-amyl dimethyl paraaminobenzoic acid is in the oil phase beaker; Take by weighing distilled water 84.0g again in the water beaker, heat oil phase and water to 85 ℃ respectively, in 15000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 2 minutes; Mixing speed is 600 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.2g imidazolidinyl urea, restir is cooled to room temperature and gets final product for 25 ℃.
Instance 6:
Take by weighing 2.0g octadecanol, the stearic alcohol ether-21 of 3.0g, the sad capric acid triglyceride of 3.0g, 4.0gN respectively, N-octyl dimethyl p-aminobenzoic acid, 2.0g 4-methyl-4-ethoxybenzene formyl methane are in the oil phase beaker; Take by weighing distilled water 86.0g again in the water beaker, heat oil phase and water to 85 ℃ respectively, in 15000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 2 minutes; Mixing speed is 600 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.3g Kazon, restir is cooled to room temperature and gets final product for 25 ℃.
Instance 7:
Take by weighing 3.0g hexadecanol, the stearic alcohol ether-25 of 2.0g, the sad capric acid triglyceride of 2.0g, 3.0g benzyl salicylate, 4.0g 2 respectively, 2 '-dihydroxy-4-methoxyl group benzophenone is in the oil phase beaker; Take by weighing distilled water 86.0g again in the water beaker, heat oil phase and water to 90 ℃ respectively, in 13000 rev/mins of following homogenizing waters; Slowly oil phase component is poured into, homogenizing began to stir cooling after 4 minutes; Mixing speed is 600 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.3g imidazolidinyl urea, restir is cooled to room temperature and gets final product for 25 ℃.
Instance 8:
Take by weighing 3.0g octadecanol, 4.0g polyoxyethylene fatty acid ester, the sad capric acid triglyceride of 4.0g, 3.0g methyl cinnamic acid monooctyl ester, 2.0g Antisolaire respectively in the oil phase beaker; Take by weighing distilled water 84.0g again in the water beaker, heat oil phase and water to 80 ℃ respectively, in 13000 rev/mins of following homogenizing waters; Oil phase component is poured into, and homogenizing began to stir cooling after 3 minutes; Mixing speed is 600 rev/mins; When the system of treating is cooled to 50 ℃, add the 0.2g Kazon, restir is cooled to room temperature and gets final product for 30 ℃.
Evaluation to nanometer lipid sun-prevention microparticle particle diameter, Zeta potential and sun-proof performance is implemented as follows:
1. the scanning electron microscope of microgranule in the nanometer lipid sun-prevention microparticle suspending liquid
(accelerating potential 5~30kv) characterizes the microscopic appearance of product to utilization Quanta 200F type scanning electron microscope for Holland, FEI Co., and the result sees accompanying drawing 1.
2. the particle size distribution of microgranule and Zeta potential distribute in the nanometer lipid sun-prevention microparticle suspending liquid
With Zetasizer Nano ZS type nano particle size and Zeta potential analyser, the particle diameter of working sample and Zeta potential distribute with the nano-lipid suspension, and the result sees accompanying drawing 2, Fig. 3.
3. the sun-proof performance of microgranule in the mensuration nanometer lipid sun-prevention microparticle suspending liquid
The mensuration of the sun-proof performance of sunscreen adopts ultraviolet spectrophotometry among the present invention, measures by the evaluation methodology of the sun-proof performance of GB QB/T2410-98.
1) breathable adhesive tape of 3M company being produced is cut into 1cm * 4cm size, sticks on the quartz colorimetric utensil printing opacity and surveys on the surface.
2) energized, the preheating spectrophotometer, setting UVB district detection wavelength is 280nm, 290nm, 300nm, 310nm and 320nm, it is 330nm, 340nm, 350nm, 360nm, 370nm, 380nm, 390nm and 400nm that wavelength is detected in the UVA district.
The quartz colorimetric utensil that 3) will post adhesive tape places sample light path and reference light paths, the adjustment instrument zero.
4) accurately take by weighing testing sample 8mg (error 0.2mg), sample is evenly spread upon on the quartz colorimetric utensil 3M adhesive tape, claim five parallel appearance.
5) the sample cuvette for preparing is placed under the room temperature dry 30min.
6) the testing sample cuvette is placed the sample light path; Another quartz cell that posts adhesive tape places reference light paths; Measure the ultraviolet absorptivity value that 280nm~400nm district sets wavelength respectively, then measured value is asked arithmetic mean of instantaneous value
Five parallel sample of sequentially determining
are asked arithmetic mean of instantaneous value, and ultraviolet absorptivity value
result who is exactly sample sees table 1.
Table 1 is the sun-proof performance measurement data of nanometer lipid sun-prevention microparticle of the inventive method preparation
(test condition: slit: 2.00nm wavelength number: 13)
Claims (5)
1. nanometer lipid sun-prevention microparticle suspending liquid, its composition is following by weight percentage:
Wherein solid lipid is that one or several of aliphatic alcohol, fatty glyceride, native paraffin or synthetic wax is compound; Described aliphatic alcohol is hexadecanol, octadecanol; Described fatty glyceride is glyceryl monostearate, sad capric acid triglyceride, and said native paraffin or synthetic wax are Cera Flava, ceresine, paraffin;
Described emulsifying agent is one of sorbitan monooleate, sorbitan monostearate, stearic alcohol ether, polyoxyethylene fatty acid ester;
Described UVA sunscreen is Antisolaire, 2-hydroxyl-4-methoxyl group benzophenone, 4-methyl-4-ethoxybenzene formyl methane, butyl methoxydibenzoylmethise, 2, in 2 '-dihydroxy-4-methoxyl group benzophenone one or more;
Described UVB sunscreen is methyl cinnamic acid monooctyl ester, N, N-octyl dimethyl p-aminobenzoic acid, N, in N-amyl dimethyl paraaminobenzoic acid, the benzyl salicylate one or more;
Described antiseptic is one of imidazolidinyl urea, phenyl phenol, Kazon.
3. the method for preparing of a nanometer lipid sun-prevention microparticle suspending liquid is characterized in that comprising being prepared as follows step:
(1) by the described solid lipid of claim 1, emulsifying agent and sunscreen 65~95 ℃ of fusions and be uniformly dispersed, obtain finely dispersed oil phase;
(2) oil-phase component and the water intimate mixing between 65~95 ℃ that step (1) are obtained, the homogenizing speed during mixing is at 8000~20000 rev/mins, and homogenizing time was at 2~10 minutes;
(3) cooling, the time cooled to 40~60 ℃ at 30 minutes~1 hour, and mixing speed adds antiseptic at 100~700 rev/mins in the cooling procedure;
(4) continue cooling, the time cooled to 5~30 ℃ at 30 minutes~3 hours, and mixing speed finally forms nanometer lipid sun-prevention microparticle suspending liquid at 100~700 rev/mins in the cooling procedure.
4. the method for preparing of nanometer lipid sun-prevention microparticle suspending liquid as claimed in claim 3, the particle diameter that it is characterized in that microgranule in the resulting nanometer lipid sun-prevention agent suspension is at 80~500nm.
5. the method for preparing of nanometer lipid sun-prevention microparticle suspending liquid as claimed in claim 3 is characterized in that microgranule has anti-sunlight function in the resulting nanometer lipid sun-prevention microparticle suspending liquid in 290nm~400nm wave-length coverage.
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CN102008403A (en) * | 2010-11-30 | 2011-04-13 | 南通新景华企业管理服务有限公司 | Suntan oil |
CN102688152A (en) * | 2012-06-05 | 2012-09-26 | 东南大学 | Composite anti-screening agent nanostructured lipid carrier and preparation method thereof |
CN105408301B (en) * | 2013-07-17 | 2018-02-23 | 亳州市新健康科技有限公司 | With more preferably ultraviolet absorber of ultraviolet protection effectiveness and combinations thereof |
CN103690388A (en) * | 2013-12-12 | 2014-04-02 | 青岛海芬海洋生物科技有限公司 | Sunscreen lotion applied during swimming |
CN103919701A (en) * | 2014-04-10 | 2014-07-16 | 上海应用技术学院 | Sunscreen spray containing solid lipid microparticles and preparation method of sunscreen spray |
CN104000740A (en) * | 2014-05-16 | 2014-08-27 | 上海应用技术学院 | Sun screening agent-coated solid lipid sunscreen particle and preparation method thereof |
WO2018014314A1 (en) * | 2016-07-22 | 2018-01-25 | Beiersdorf Daily Chemical (Wuhan) Co. Ltd. | Cosmetic composition containing hydrophobic flakes comprising fatty alcohols |
CN110613630B (en) * | 2019-09-30 | 2022-08-30 | 汕头大学 | Sunscreen cream containing benzophenone derivative nanocrystals and preparation method thereof |
CN114191325A (en) * | 2021-12-20 | 2022-03-18 | 嘉文丽(福建)化妆品有限公司 | Plant sunscreen composition and preparation method of nanoparticles thereof |
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