CN100577140C - Baicalin nanometer emulsion cosmetics - Google Patents

Baicalin nanometer emulsion cosmetics Download PDF

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Publication number
CN100577140C
CN100577140C CN200610104589A CN200610104589A CN100577140C CN 100577140 C CN100577140 C CN 100577140C CN 200610104589 A CN200610104589 A CN 200610104589A CN 200610104589 A CN200610104589 A CN 200610104589A CN 100577140 C CN100577140 C CN 100577140C
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baicalin
oil
surfactant
nanometer
emulsion cosmetics
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CN1931121A (en
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欧阳五庆
吴旭锦
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Northwest A&F University
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Northwest A&F University
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Abstract

The present invention discloses one kind of nanometer baicalin emulsion cosmetics, which is prepared with surfactant, oil, baicalin, essence and distilled water, and through weighing surfactant with or without co-surfactant, calculating HLB value and selecting oil for reaching emulsifying HLB value near that of the surfactant phase, changing the ratio between the surfactant phase and the oil phase regularly to dissolve baicalin, adding distilled water slowly at 20-25 deg.c to form clear and flowing O/W type stable nanometer baicalin emulsion cosmetics. The nanometer baicalin emulsion cosmetics has excellent transdermal permeability, high solubility of baicalin, high effects of whitening, beautifying, eliminating acne and preventing against sun, and excellent extensibility on skin.

Description

A kind of nanometer baicalin emulsion cosmetics
Technical field
The invention belongs to cosmetic field, relate to a kind of Pear Power, speckle dispelling, remove pox, the oil-in-water baicalin nano-milk cosmetics of the transparent and stable of function such as sun-proof and treatment acne.
Background technology
Baikal skullcap root is the root of Labiatae herbaceous plant Radix Scutellariae, has significantly to whiten, speckle dispelling, remove the effect of pox, sun-proof and treatment acne.At present, product on the market is directly to make an addition in the soft mode powder after Radix Scutellariae is pulverized, result of use is also unsatisfactory, its reason mainly is to contain a large amount of xanthein compositions in the Radix Scutellariae, directly make an addition in the cosmetics and can make dye, simultaneously, the great majority of existing product all are emulsion, its particle diameter is generally all greater than 400nm, and skin is difficult for absorbing.
Summary of the invention
The objective of the invention is at above-mentioned prior art problems and defective, provide a kind of little to the human body zest, have a nanometer baicalin emulsion cosmetics of skin whitening, acne treatment, anti-sunlight function safely and efficiently.
The way that the present invention solves above-mentioned prior art problem in two steps, the first step is that the main effective ingredient baicalin extraction separation from Radix Scutellariae in the Radix Scutellariae is come out, and is adding in the cosmetics according to a certain percentage.Because baicalin has good inhibitory effect to the B16 melanocyte rate of increase, suppression ratio when mass concentration is 1 * 10-5g/mL is 24.19%, suppression ratio when 1 * 10-3g/mL is 85.13%, and the effect of baicalin is more single-minded, only melanocyte there is high inhibition activity, other people somatic cell be there is no any toxic and side effects.Baicalin can also promote the phagocytic function of macrophage in addition, therefore can effectively remove the dead cell in the acne, thalline and other residues, and the recovery from illness of accelerates acne, and do not stay spot more.The ultraviolet of baicalin energy strong absorption 230nm~350nm, its spf value reaches 18, because baicalin itself has anti-allergic effects; Second step was that the dosage form with original cosmetics changes nanoemulsions into by emulsion, and particle diameter is between 10~100nm, easier diffusion and penetrate into skin.
Nanometer baicalin emulsion cosmetics of the present invention comprises that mainly mass percent is:
Surfactant 15.80%~43.99%
Oil 5.10%~6.90%
Baicalin 0.10 ‰~10.00 ‰
Essence 0.16%~0.22%
Surplus is a distilled water
Total component is 100%.
Described surfactant is any or several mixture in lauric acid polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, castor oil hydrogenated polyoxyethylene ether, tween 80 and the Arlacel-80.
Described oil is any or several mixture in isopropyl myristate, isopropyl palmitate, iso-octyl palmitate, Jojoba oil, white mineral oil, liquid paraffin, vitamin E oil, olive oil, Adeps Serpentis, the almond oil.
Can also add cosurfactant in the described surfactant.
Described cosurfactant is ethanol, 1,3 butylene glycol, 1, any in the 2-propylene glycol or several mixture.
Described nanometer baicalin emulsion cosmetics can also the solubilising Pear Power, sun-proof, other active ingredient of removing functions such as acne.
Cosmetics of the present invention are in the selection of surfactant, select nonionic surfactant for use, its toxicity is less relatively, more stable in solution, be not subject to the influence of strong electrolyte, inorganic salts, be not subject to the influence of soda acid yet, and good with the compatibility of other surfactants, and haemolysis is less.Consider preparation technology's simplicity, be the stability of the easy formation of nano-emulsion and the nano-emulsion for preparing, the present invention selects the liquid nonionic surfactant of HLB between 10~15 for use, and is perhaps composite with the non-ionic surface active agent of a kind of HLB<10.Available surfactant has: lauric acid polyoxyethylene ether, castor oil polyoxyethylene ether (as EL-40), castor oil hydrogenated polyoxyethylene ether (as RH-40), alkylphenol polyoxyethylene (as TX-8,10 etc.).More than several surfactants can use separately, also can be respectively during with the 80 composite uses of class of department.
The present invention is according to when the HLB of the required surfactant of emulsifying oil phase is close with surfactant, the principle that formed emulsion is stable, the oils and fats of selecting for use have isopropyl myristate, isopropyl palmitate, Jojoba oil, white mineral oil, liquid paraffin, vitamin E oil, almond oil, Adeps Serpentis, one or more mixture of Fructus Canarii albi wet goods.These oils and fatss are little to skin irritation, be in a liquid state, do not have bad abnormal smells from the patient under the room temperature, have good wetting property, and infiltration is made skin lubrication glossy by skin absorbs easily.
The present invention selects bland cosurfactant, mainly contains ethanol, 1,3 butylene glycol, and 1,2-propylene glycol etc.Cosurfactant can be adjusted HLB VALUE OF SURFACTANTS (HLB), can further reduce interfacial tension, increases the compliance and the rigidity of film, is inserted in the interfacial film, promotes the formation of the film that radius of curvature is very little, enlarges nano-emulsion and forms the zone.
Another object of the present invention provides preparation nanometer baicalin emulsion cosmetics method, comprises that step is as follows:
1) preparation of surfactant phase takes by weighing surfactant by formula proportion, use separately or with help surface activity composite in proportion, calculate the HLB value of this system, stir.
The HLB value of common emulsifying agent can be found in some chemical industry handbooks, as " the chemical products handbook of chemical industry publishing house.Because hydrophile-lipophile balance (HLB) value of surfactant has additive properties, the available quality averaging method is obtained the HLB value of surfactant.For example, after two kinds of surfactant A, B mixed, the hydrophile-lipophile balance HLBAB value of its mixed surfactant was
HLBAB=(WAHLBA+WBHLBB)/(WA+WB)
WA in the formula, WB---the quality of blend surfactants A, B;
HLBA, the HLB value of HLBB---surfactant A, B.
2) preparation of oil phase is selected one or more oil according to the HLB value of surfactant phase, transfers its ratio, makes the required HLB value of its emulsifying close with surfactant HLB mutually.
3) baicalin with formula proportion dissolves in the surfactant as the surfactant phase, change the ratio of surfactant phase and oil phase in 9: 1~1: 9 rule, 20 ℃~25 ℃ down slow adding distil waters fully stir, until form clear, viscosity is little and tool is mobile outward appearance is glassy yellow or colourless O/W type nanometer emulsion.
The present invention detects through transmission electron microscope, and droplet diameter distribution is between 10~100nm, and outward appearance is transparent glassy yellow or colourless liquid, has good stability:
1, ageing stability
Ageing stability is meant when nanoemulsions is preserved under room temperature nature change condition, and the nanoemulsions outward appearance prolongs and the degree that changes in time.This nanometer baicalin emulsion cosmetics is transparent lastingly, does not find muddy or precipitation, illustrates that then ageing stability is good.This is an important indicator estimating nanoemulsions.
2, heat storage stability
This nanometer baicalin emulsion cosmetics is placed test tube, and sealing places 37 ℃ of constant water bath box to store 14 days, this liquid heat storage back appearance transparent.
3, anti-freeze-stable
With this nanometer baicalin emulsion cosmetics in refrigerator-4 ℃ preserve a week after.Return to room temperature.If nanoemulsions becomes solids at-4 ℃, return to room temperature, return to transparent, and place one week the back continue transparently, think that then freezing-resistance is good.
4, accelerated stability
This nanometer baicalin emulsion cosmetics is placed test tube, and sealing under the rotating speed of 15000r/min centrifugal 20 minutes, does not have layering, still clear.
Nanometer baicalin emulsion cosmetics of the present invention has better percutaneous permeability, can strengthen the dissolubility of baicalin, that improves baicalin whitens, goes acne, sun-proof effect, improve the ductility of cosmetics on skin, can also the solubilising Pear Power, sun-proof, other active ingredient of removing functions such as acne.Be applicable to that face is dark yellow, the sedimentary butterfly spot of pigment is arranged, mottle, chloasma etc., the back of washing one's face sooner or later every day is dipped in cotton swab and is got the position that evenly is applied in speckle in right amount.For anti-ultraviolet is shot wounded, also can after washing one's face, get and evenly spread upon face in right amount.
Nanometer baicalin emulsion cosmetics of the present invention compared with prior art has the following advantages:
(1) thermodynamic stability height.Operation is fairly simple during preparation, not phase-splitting, do not precipitate, and bin stability improves;
(2) light transmission is good, and sensible quality improves;
(3) antiseptic property improves, because decentralized photo liquid is smaller, can prevent the intrusion of antibacterial, increases the dissolubility of some active ingredients simultaneously;
(4) than have higher diffusibility and percutaneous permeability in general emulsion, the product result of use improves in nanoemulsions in active ingredient.
(5) simple, the good stability of technology, available water infinite dilution can be widely used in and whiten, and be sun-proof, controls the cosmetic field of acne.
The specific embodiment
Below further sets forth the beneficial effect of cosmetics of the present invention by testing example, these test examples comprised medicine of the present invention to animal irritation test, antibacterial activity test, effect observation tests and contrast test.
Test example 1 nanometer baicalin emulsion cosmetics animal irritation test
8 of New Zealand tower rabbits are divided 2 groups, and one group is carried out the skin irritation test, adopting each 0.3ml of nanometer baicalin emulsion cosmetics of 0.5%, 1%, 5%, 10% respectively observes one group eye dripping, do not occur tangible zest behind the 24h, eyelid is not rubescent, and eyeball does not have the abnormal secretion thing; Adopt each 3ml of nanometer baicalin emulsion cosmetics of 0.5%, 1%, 5%, 10% that another group is carried out the skin irritation test more respectively, tangible zest does not all appear in observation behind the 24h.
The test of test example 2 nanometer baicalin emulsion cosmetics antibacterial activities
Show that this nanometer baicalin emulsion cosmetics has broad-spectrum antibacterial activity, thalline such as staphylococcus aureus, Hemolytic streptococcus, streptococcus pneumoniae, meningococcus, vibrio cholera and diphtheria, anthrax, green pus, typhoid fever and Bu Shi all there is in various degree inhibitory action, isolated experiment shows, nanometer baicalin emulsion cosmetics suppresses propionibacterium acnes under same concentrations effect is 2 times of metronidazole, is 115 times of red syphilis.
Test example 3 nanometer baicalin emulsion cosmetics whitening effect viewing tests
Subjects is my school student 25 examples, and wherein 10 examples have chloasma, and 5 examples have freckle, and 5 examples have acne, and 5 example no obvious mottles but skin is more black are the women.Sooner or later coat the nanometer baicalin emulsion cosmetics that experiment makes at face after washing one's face every day, used continuously 1 month, experimental result finds have 8 examples to be produce effects among the 10 routine mottle patients, and obvious effective rate is that 80%, 2 example is effective, and effective percentage is 20%; 5 routine freckle patients all have remarkable result, and obvious effective rate is 100%; 5 routine patients with acne 3 examples have remarkable result, and obvious effective rate is 60%; 4 routine melanin all obviously reduced after the black person of 5 routine skins had used and tested the product that makes, and it is white touched with red that skin becomes, and total effective rate is 80%.Show that obviously nanometer baicalin emulsion cosmetics has good whitening effect.
Test example 4 nanometer baicalin emulsion cosmetics whiten, sun-proof, control the test of acne effect observation
Select my school schoolgirl 40 examples, wherein 10 examples have chloasma (to be equally divided into a at random, two groups of b, the a group is used the nanometer baicalin emulsion cosmetics of this test invention, the accurate word Z44023031 of the traditional Chinese medicines Margarita layer powder that the b group uses the fine pharmaceutical Co. Ltd in Guangdong to produce is done contrast), 10 examples have acne (to be equally divided into c at random, two groups of d, the c group is used the nanometer baicalin emulsion cosmetics of this test invention, the 11-XK-0190 number new FUMANLING frost that the d group uses Jinan City, Shandong Province east wind pharmaceutical factory to produce done contrast), 10 routine skins are black (to be equally divided into m at random, two groups of n, the m group is used the nanometer baicalin emulsion cosmetics of this test invention, n group uses lot number that Jianong Bio-Chemical Co Ltd, Nanjing produces should the whitening skin and preserving moisture emulsion to do contrast as the fourth of H010302Y is man), the 10 routine colours of skin are evenly pale (to be equally divided into s at random, two groups of t, the s group is used the nanometer baicalin emulsion cosmetics of this test invention, the lot number that the t group uses Jianong Bio-Chemical Co Ltd, Nanjing to produce should the whitening sun protection emulsion be done contrast as H020613B fourth man, do not adopt other sun-proof measures after smearing), through 30 days observing effects.Wherein a group has 3 routine chloasma almost all to disappear, and 2 routine speckles are thin out, and the colour of skin makes moderate progress; B organizes all desalinations to some extent of 5 routine speckles, does not all disappear but there is 1 routine speckle.C organizes 5 routine acne recoveries from illness, and colour of skin change is even; The 3 example recoveries from illness of d group, 2 examples have change slightly.M organizes the 5 routine colours of skin all bigger improvement, and melanin all obviously reduces, and it is white touched with red that skin becomes, glossy and careful; N organizes 5 examples also all improvement, and skin bleaches a little.S organizes 5 routine skins and does not have too big variation before; T organizes dark and coarse that 3 routine skins become, and colour of skin jaundice has mottle to produce, the blackening slightly of 2 examples, and skin lacks brightness.The result obviously show nanometer baicalin emulsion cosmetics have well whiten, sun-proof, control the acne effect.
Below the embodiment that provides by the inventor further specify the preparation method of nanometer baicalin emulsion cosmetics of the present invention.
Embodiment 1
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing alkylphenol polyoxyethylene 3.0g, 1,3-butanediol 1.0g (wherein being dissolved with baicalin 0.1g), iso-octyl palmitate 0.44g, vitamin E oil 0.07g, essence 0.02g, put into beaker, under 25 ℃ of room temperature conditions, manually stir its abundant mix homogeneously, then to wherein slowly adding distilled water, the limit adds the waterside manually stirs, and the system viscosity is less during beginning, with the increase of rate of water added, it is sticky that system can become, this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, when system thinning suddenly, what produced this moment promptly is glassy yellow transparent water oil-packaging type nanometer baicalin emulsion cosmetics, claims that its gross weight is 10.00g.
Embodiment 2
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing castor oil polyoxyethylene ether 1.5g, ethanol 0.78g (wherein being dissolved with baicalin 0.05g), isopropyl myristate 0.46g, liquid paraffin 0.07g, vitamin E oil 0.05g, essence 0.02g, put into beaker, under 20 ℃ of room temperature conditions, manually stir its abundant mix homogeneously, then to wherein slowly adding distilled water, the limit adds the waterside manually stirs, and the system viscosity is less during beginning, with the increase of rate of water added, it is sticky that system can become, this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, when system thinning suddenly, what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its gross weight is 10.00g.
Embodiment 3
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing castor oil polyoxyethylene ether 1.12g, 1,2-propylene glycol 0.46g (wherein being dissolved with baicalin 0.04g), isopropyl palmitate 0.5g, liquid paraffin 0.1g, vitamin E oil 0.06g, essence 0.02g puts into beaker, under 24 ℃ of room temperature conditions, manually stir its abundant mix homogeneously, to wherein slowly adding distilled water, the limit adds the waterside and manually stirs then, the system viscosity is less during beginning, with the increase of rate of water added, it is sticky that system can become, and this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, thinning suddenly when system, what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its gross weight is 10.00g.
Embodiment 4
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing tween 80 2.360g, Arlacel-80 0.433g, ethanol 0.078g (wherein being dissolved with baicalin 0.001g), isopropyl myristate 1.062g, white mineral oil 0.092g, vitamin E oil 0.046g, essence 0.02g puts into beaker, under 24 ℃ of room temperature conditions, manually stir its abundant mix homogeneously, to wherein slowly adding distilled water, the limit adds the waterside and manually stirs then, the system viscosity is less during beginning, with the increase of rate of water added, it is sticky that system can become, and this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, thinning suddenly when system, what produced this moment promptly is glassy yellow transparent water oil-packaging type nanometer baicalin emulsion cosmetics, claims that its gross weight is 10.002g.
Embodiment 5
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing lauric acid polyoxyethylene ether 1.12g, 1,2-propylene glycol 0.46g (wherein being dissolved with baicalin 0.01g), isopropyl myristate 0.5g, liquid paraffin 0.1g, vitamin E oil 0.09g, essence 0.02g puts into beaker, under 25 ℃ of room temperature conditions, manually stir its abundant mix homogeneously, to wherein slowly adding distilled water, the limit adds the waterside and manually stirs then, the system viscosity is less during beginning, with the increase of rate of water added, it is sticky that system can become, and this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, thinning suddenly when system, what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its gross weight is 10.00g.
Embodiment 6
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing polyoxyethylene castor oil 3.6g, almond oil 0.4g, vitamin E oil 0.07g, essence 0.02g, put into beaker, under 20 ℃ of room temperature conditions, manually stir with its abundant mix homogeneously, then to wherein slowly adding distilled water, manually stir on adding distil water limit, limit, the system viscosity is less during beginning, and along with the increase of the distillation water yield, it is sticky that system can become, this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, unexpected when thinning when system, what produced this moment promptly is O/W type nano-emulsion, the baicalin of 0.06g is directly added, stirring is until whole dissolvings, and what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its weight is 9.07g.
Embodiment 7
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing polyoxyethylene hydrogenated Oleum Ricini 4.5g, olive oil 0.5g, vitamin E oil 0.054g, essence 0.016g, put into beaker, under 24 ℃ of room temperature conditions, manually stir with its abundant mix homogeneously, then to wherein slowly adding distilled water, manually stir on adding distil water limit, limit, the system viscosity is less during beginning, and along with the increase of the distillation water yield, it is sticky that system can become, this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, unexpected when thinning when system, what produced this moment promptly is O/W type nano-emulsion, the baicalin of 0.10g is directly added, stirring is until whole dissolvings, and what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its weight is 10.23g.
Embodiment 8
With determining optimal proportion according to 9: 1~1: 9 rule drafting pseudo-ternary phase diagram by calculating HLB value selected oil and surfactant, cosurfactant.Accurately take by weighing polyoxyethylene castor oil 3.6g, Adeps Serpentis 0.4g, vitamin E oil 0.07g, essence 0.02g, put into beaker, under 25 ℃ of room temperature conditions, manually stir with its abundant mix homogeneously, then to wherein slowly adding distilled water, manually stir on adding distil water limit, limit, the system viscosity is less during beginning, and along with the increase of the distillation water yield, it is sticky that system can become, this moment, liquid crystal state or water-in-oil type nanoemulsion may appear in system, continue to drip and constantly stir, unexpected when thinning when system, what produced this moment promptly is O/W type nano-emulsion, the baicalin of 0.06g is directly added, stirring is until whole dissolvings, and what produced this moment promptly is water white transparency oil-in-water baicalin nano-milk cosmetics, claims that its weight is 9.07g.

Claims (2)

1, a kind of nanometer baicalin emulsion cosmetics, it is characterized in that, by mass percent be: 15.80%~43.99% surfactant, 5.10%~6.90% oil, 0.10 ‰~10.00 ‰ baicalin, 0.16%~0.22% essence, surplus are that distilled water is formed, and total component is 100%;
Described surfactant is any or several mixture in lauric acid polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, castor oil hydrogenated polyoxyethylene ether, tween 80 and the Arlacel-80;
Described oil is any or several mixture in isopropyl myristate, isopropyl palmitate, iso-octyl palmitate, Jojoba oil, white mineral oil, liquid paraffin, vitamin E oil, olive oil, Adeps Serpentis, the almond oil.
2, nanometer baicalin emulsion cosmetics according to claim 1 is characterized in that: the particle diameter of described nanometer baicalin emulsion cosmetics is 10nm~100nm.
CN200610104589A 2006-09-18 2006-09-18 Baicalin nanometer emulsion cosmetics Expired - Fee Related CN100577140C (en)

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