CN102940597B - Natural compound botanical antioxidant, as well as preparation method and application thereof in cosmetics - Google Patents

Natural compound botanical antioxidant, as well as preparation method and application thereof in cosmetics Download PDF

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Publication number
CN102940597B
CN102940597B CN201210514776.6A CN201210514776A CN102940597B CN 102940597 B CN102940597 B CN 102940597B CN 201210514776 A CN201210514776 A CN 201210514776A CN 102940597 B CN102940597 B CN 102940597B
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weight portion
weight
natural compound
component
antioxidant
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CN102940597A (en
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万洁
夏泉
温波
李永强
李燕杰
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Yantai Era Health Industry Daily Chemical Co Ltd
NEW AGE HEALTH INDUSTRY(GROUP) CO Ltd
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Yantai Era Health Industry Daily Chemical Co Ltd
NEW AGE HEALTH INDUSTRY(GROUP) CO Ltd
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Abstract

The invention relates to a natural compound botanical antioxidant which comprises the plant raw materials as follows: 750-1200 parts by weight of lophatherum gracile, 15-40 parts by weight of the root bark of white mulberry, 20-50 parts of liquorice, 20-50 parts of artemisia capillaris flower and 1-6 parts by weight of Chinese dates. The invention also provides a preparation method of the natural compound botanical antioxidant, and the application of the natural compound botanical antioxidant in cosmetics for whitening and resisting ageing. According to the invention, the active ingredients of the natural raw materials are effectively extracted and reasonably matched, thus realizing the synergistic effect of different antioxidant active ingredients, and greatly improving the antioxidant activity.

Description

Natural compound plant antioxidant, its preparation method and the application in cosmetics
Technical field
The present invention relates to a kind of compound plant antioxidant.
Background technology
Along with free radical and disease, old and feeble theoretical research deepen continuously, the using value of antioxidant comes into one's own day by day.Because the antioxidant (as BHT, BHA etc.) of synthetic has many side effect, the liver of human body, spleen, lung are all had to adverse effect, utilizing the Natural antioxidant to prevent and cure diseases becomes study hotspot.Natural plant antioxidant has that source is wide, antioxidant activity large, strong and safety is high with body affinity an advantage.Its oxidation-resistant active ingredient is mainly derived from plant polyphenol, flavonoid, active polysaccharide, vitamin, protein and aminoacid etc. [Zheng Deyong etc., plant anti-oxidation and research prospect, Fujian Forestry Inst.'s journal, 2004,24 (1): 88-91].These oxidation-resistant active ingredients are metal ion, the associating antioxidation by electron transfer, complex catalysis oxidation and affect the approach such as gene expression and play a role in vivo.It is single from composition that research finds that the antioxidant activity of plant extract is often greater than, and shows multicomponent antioxidation synergism.They form synergism by approach such as redox cycle system or different mechanism of action complementations.And the antioxidant activity of various plants extract built agent may be higher than single plant extract.Therefore, on research multicomponent antioxidation synergism basis, can pass through the composite of dissimilar antioxidant, develop efficient, safe composite type antioxidant agent, to meet the needs of health product, cosmetics, medical industry development.
Summary of the invention
The object of the present invention is to provide a kind of natural compound plant antioxidant, composite by a certain percentage to the folk prescription extract of phyllostachys nigra (lodd.ex lindl.) munro var.henonis (miff.) spapf et rendle, Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae after, obtain the compound antioxidant that antioxidant activity increases substantially.
For achieving the above object, the present invention includes following technical scheme:
A natural compound plant antioxidant, it is to be made by the plant material of following composition and proportioning:
Herba Lophatheri, 750-1200 weight portion; Cortex Mori, 15-40 weight portion; Radix Glycyrrhizae, 20-50 weight portion; Herba Artemisiae Scopariae flower, 20~50 weight portions; And Fructus Jujubae, 1~6 weight portion.
Natural compound plant antioxidant as above, preferably, it is to be made by the plant material of following composition and proportioning: Herba Lophatheri, 1000 weight portions; Cortex Mori, 25 weight portions; Radix Glycyrrhizae, 34 weight portions; Herba Artemisiae Scopariae flower, 33 weight portions; And Fructus Jujubae, 3 weight portions.
Natural compound plant antioxidant as above, preferably, it is to be made by the plant material of following composition and proportioning: Herba Lophatheri, 1000 weight portions; Cortex Mori, 15 weight portions; Radix Glycyrrhizae, 50 weight portions; Herba Artemisiae Scopariae flower, 33 weight portions; And Fructus Jujubae, 1 weight portion.
Natural compound plant antioxidant as above, preferably, it is to be made by the plant material of following composition and proportioning: Herba Lophatheri, 1000 weight portions; Cortex Mori, 25 weight portions; Radix Glycyrrhizae, 20 weight portions; Herba Artemisiae Scopariae flower, 50 weight portions; And Fructus Jujubae, 6 weight portions.
A preparation method for natural compound plant antioxidant, the method comprises the following steps:
A. weight portion takes Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae as described above, the concentrated component I that obtains after employing room temperature alcohol leaching;
B. weight portion takes Herba Lophatheri as described above, successively by water reflux, extract,, precipitate with ethanol extraction and the concentrated component II that obtains;
C. component I and component II are mixed to the natural compound plant antioxidant of acquisition.
Preparation method as above, preferably, the operating process of described steps A is as follows:
A. the Cortex Mori taking according to described weight portion, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae, added in the 1-3 butanediol and/or dehydrated alcohol of 5~10 times of solid material gross weights, soaks 12~36 hours under room temperature, and I filters to get filtrate;
B. in the filtering residue of above-mentioned filtration step gained, add the sterile purified water of 12~16 times of described solid material gross weights, 50~70 ℃ of temperature, stir 0.5~2 hour, and II filters to get filtrate;
C. merging filtrate I and filtrate II obtain mother solution, freezing 12~36 hours in-10 ℃~0 ℃;
D. after mother solution recovers room temperature, with 100-200 order filter, carry out sucking filtration, collect filtrate II I;
E. filtrate II I removes solvent under reduced pressure in 55~65 ℃, to 1/2~1/3 of this filtrate II I original volume, obtains described component I.
Preparation method as above, preferably, the operating process of described step B is as follows:
A. raw material Herba Lophatheri is added in the water of 3~8 times of weight, heating and refluxing extraction 2-5 hour, obtains reflux extracting liquid;
B. reflux extracting liquid is filtered, obtain mother solution;
C. mother solution is carried out to vacuum concentration, the 30%-60% to mother solution volume, obtains concentrated solution;
D. concentrated solution is carried out to centrifugalize, remove insoluble matter, collect separating medium;
E. separating medium is carried out to precipitate with ethanol extraction, adding amount of alcohol is the 50%-80% of separating medium cumulative volume, and airtight cold preservation 24-48 hour filters, and obtains precipitate with ethanol extract;
F. precipitate with ethanol extract is filtered, remove impurity, obtain target solution;
G. target solution is carried out to vacuum concentration, subsequent spray is dry, obtains described component I I.
A natural compound plant antioxidant, it adopts method as above to prepare.
Natural compound plant antioxidant of the present invention has the application in the cosmetics of antioxidation and/or white-skinned face function in preparation.
A facial film with whitening anti-aging function, it is that one-tenth by following proportioning is grouped into:
Emulsifying agent, 1.8-3.5 weight portion; Skin moistening oils and fats, 3.6-44 weight portion; Wetting agent, 2-20 weight portion; Film former, 0.1-1.0 weight portion; Antiseptic, 0.1-1.25 weight portion; Natural compound plant antioxidant of the present invention, 0.1-5.0 weight portion; Deionized water, 45-75 weight portion.
The facial film with whitening anti-aging function as above, preferably, it is that one-tenth by following proportioning is grouped into:
Emulsifying agent, 2-3 weight portion; Skin moistening oils and fats, 15-25 weight portion; Wetting agent, 10-20 weight portion; Film former, 0.2-0.8 weight portion; Antiseptic, 0.1-0.5 weight portion; Natural compound plant antioxidant of the present invention, 0.1-5.0 weight portion; Deionized water, 45-75 weight portion.
A facial film with whitening anti-aging function, it is that one-tenth by following proportioning is grouped into:
A phase: Arlacel-60 polyoxyethylene ether 1.0~2.0 weight portions, sorbitan monostearate, 0.8~1.5 weight portion; Glyceryl stearate and/or PEG-100 stearate, 0.5~3.0 weight portion; Cetearyl alcohol, 0.2~5.0 weight portion; Stearic acid, 0.2~4.0 weight portion; Caprylic/capric triglyceride, 1~10 weight portion; Squalane, 1~10 weight portion; Dormant oils, 1~10 weight portion; Dimethicone, 0.2~5.0 weight portion; Methyl parahydroxybenzoate, 0.02~0.2 weight portion; Propyl p-hydroxybenzoate, 0.02~0.15 weight portion;
B phase: water, 45~75 weight portions; Butanediol, 1~10 weight portion; Glycerol, 1~10 weight portion; Hydroxyethyl-cellulose, 0.1~1.0 weight portion; Allantoin, 0.1~0.3 weight portion; Titanium dioxide, 0.5~5.0 weight portion; Nicotiamide, 0.2~3.0 weight portion;
C phase: De Minshu, 0.01~0.5 weight portion; Fragrant quick relaxing, 0.01~0.3 weight portion; Natural compound plant antioxidant described in claim 1 or 6,0.1~5.0 weight portion;
D phase: dihydroxymethyl dimethyl hydantoin and/or iodo propinyl butyl chloride carbamate, 0.1~0.8 weight portion; Essence, 0.01~0.03 weight portion.
The facial film with whitening anti-aging function as above, preferably, it is that one-tenth by following proportioning is grouped into:
A phase: Arlacel-60 polyoxyethylene ether 1.2 weight portions, sorbitan monostearate, 0.9 weight portion; Glyceryl stearate and/or PEG-100 stearate, 2.8 weight portions; Cetearyl alcohol, 3.5 weight portions; Stearic acid, 1.2 weight portions; Caprylic/capric triglyceride, 1.1 weight portions; Squalane, 6 weight portions; Dormant oils, 2 weight portions; Dimethicone, 1 weight portion; Methyl parahydroxybenzoate, 0.1 weight portion; Propyl p-hydroxybenzoate, 0.05 weight portion;
B phase: water, 67.622 weight portions; Butanediol, 3 weight portions; Glycerol, 8 weight portions; Hydroxyethyl-cellulose, 0.4 weight portion; Allantoin, 0.15 weight portion; Titanium dioxide, 1.2 weight portions; Nicotiamide, 0.2 weight portion;
C phase: De Minshu, 0.15 weight portion; Fragrant quick relaxing, 0.1 weight portion; Natural compound plant antioxidant of the present invention, 0.605 weight portion;
D phase: dihydroxymethyl dimethyl hydantoin and/or iodo propinyl butyl chloride carbamate, 0.16 weight portion; Essence, 0.013 weight portion.
The facial film with whitening anti-aging function as above, preferably, it is that one-tenth by following proportioning is grouped into:
A phase: Arlacel-60 polyoxyethylene ether 1.1 weight portions, sorbitan monostearate, 1.0 weight portions; Glyceryl stearate and/or PEG-100 stearate, 2.5 weight portions; Cetearyl alcohol, 3.0 weight portions; Stearic acid, 1 weight portion; Caprylic/capric triglyceride, 1 weight portion; Squalane, 6 weight portions; Dormant oils, 3 weight portions; Dimethicone, 1 weight portion; Methyl parahydroxybenzoate, 0.1 weight portion; Propyl p-hydroxybenzoate, 0.05 weight portion;
B phase: water, 67.622 weight portions; Butanediol, 3 weight portions; Glycerol, 8 weight portions; Hydroxyethyl-cellulose, 0.4 weight portion; Allantoin, 0.15 weight portion; Titanium dioxide, 1 weight portion; Nicotiamide, 0.2 weight portion;
C phase: De Minshu, 0.15 weight portion; Fragrant quick relaxing, 0.1 weight portion; Natural compound plant antioxidant of the present invention, 0.5 weight portion;
D phase: dihydroxymethyl dimethyl hydantoin and/or iodo propinyl butyl chloride carbamate, 0.16 weight portion; Essence, 0.013 weight portion.
The facial film with whitening anti-aging function as above, preferably, it is that one-tenth by following proportioning is grouped into:
A phase: Arlacel-60 polyoxyethylene ether 1.0 weight portions, sorbitan monostearate, 0.9 weight portion; Glyceryl stearate and/or PEG-100 stearate, 2.8 weight portions; Cetearyl alcohol, 3.2 weight portions; Stearic acid, 1.0 weight portions; Caprylic/capric triglyceride, 1 weight portion; Squalane, 6 weight portions; Dormant oils, 3 weight portions; Dimethicone, 1 weight portion; Methyl parahydroxybenzoate, 0.1 weight portion; Propyl p-hydroxybenzoate, 0.05 weight portion;
B phase: water, 67.622 weight portions; Butanediol, 5 weight portions; Glycerol, 5 weight portions; Hydroxyethyl-cellulose, 0.4 weight portion; Allantoin, 0.15 weight portion; Titanium dioxide, 1 weight portion; Nicotiamide, 0.2 weight portion;
C phase: De Minshu, 0.15 weight portion; Fragrant quick relaxing, 0.1 weight portion; Natural compound plant antioxidant of the present invention, 0.4 weight portion;
D phase: dihydroxymethyl dimethyl hydantoin and iodo propinyl butyl chloride carbamate, 0.16 weight portion; Essence, 0.013 weight portion.
The preparation method of facial film as mentioned above, the method comprises the following steps:
A. A phase, B are heated to respectively mutually to 75~85 ℃ and stir 10~20 minutes;
B. A is added to B phase, homogenizing 2~5 minutes, rotating speed is 3000~6000 revs/min;
C. under stirring, mixture is cooled to 60~65 ℃, is heated to subsequently 70~80 ℃, homogenizing 1~2 minute, rotating speed is 1500~3000 revs/min;
D. mixture step c being obtained is cooled to below 50 ℃, slowly adds C phase, homogenizing 10~20 seconds, and rotating speed is 1000~2000 revs/min;
E. mixture steps d being obtained stirs below borehole cooling to 45 ℃, adds D phase, is under agitation cooled to subsequently 35~38 ℃, discharging.
A facial film with whitening anti-aging function, it adopts method as above to prepare.
Beneficial effect of the present invention is, the present invention carries out composite to several plant extracts with antioxidant activity by a certain percentage, wherein, the flavone compound that Herba Lophatheri extract contains tool antioxidant activity and polysaccharide, Cortex Mori is rich in flavone compound, Radix Glycyrrhizae has licoflavone and Angelica Polysaccharide, and Herba Artemisiae Scopariae flower is rich in flavone compound, is rich in jujube polysaccharide and VE, VC in Fructus Jujubae; The present invention effectively extracts and reasonable coordination the active component of these several natural materials, has realized the synergism of different oxidation-resistant active ingredients, has obtained the natural compound plant antioxidant that antioxidant activity significantly improves.
Meanwhile, the activation that Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower extract can restraint of tyrosinase, reduces melanin and generates; Fructus Jujubae extract can improve the distribution in epidermis cell with pigment, accelerates melanin metabolism; Thereby there is white-skinned face function.
Experimental result shows, natural compound plant antioxidant of the present invention has whitening and senile-resistant efficacy for cosmetics.
Accompanying drawing explanation
Fig. 1 is melanin content situation before and after cleawhite pack () is used;
Fig. 2 is melanin content situation before and after cleawhite pack (two) is used;
Fig. 3 is melanin content situation before and after cleawhite pack (three) is used;
Fig. 4 is the situation of change of skin brightness (L) before and after cleawhite pack () is used;
Fig. 5 is the situation of change of skin brightness (L) before and after cleawhite pack (two) is used;
Fig. 6 is the situation of change of skin brightness (L) before and after cleawhite pack (three) is used.
The specific embodiment
The preparation of embodiment 1, compound plant antioxidant (one)
Raw materials used and the adjuvant of the present embodiment and following examples all can obtain by commercially available purchase.
(1) preparation of component I
1) raw material is that 25 grams of Cortex Mori, Herba Artemisiae Scopariae are spent 34 grams, 33 grams, 3 grams, Fructus Jujubae and Radix Glycyrrhizae, in raw material, adds 0.3L 1-3 butanediol and 0.7L dehydrated alcohol, soaks 24 hours under room temperature;
2) 45 ℃, stir 2 hours, I filters to get filtrate;
3) in filtering residue, add sterile purified water 1.5L, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II, add in filtering residue, in 45 ℃ of stirrings 2 hours, filters, and obtains mother solution;
5) by mother solution-5 ℃ freezing 24 hours, after filtrate is recovered room temperature, with plate filter, carry out sucking filtration, collect filtrate II I;
6) by filtrate II I rotary evaporation under 60 ℃ of conditions, concentrate, to be concentrated during to 0.7L (concentrated 3 times), the evaporation of stopping the rotation, obtains concentrated solution A;
7) in concentrated solution A, add antiseptic IS-45 (two imidazolidinyl urea and the iodo propinyl butyl meglumine acid acid & methyl hydroxybenzoate & propylene glycol of 1.4 grams, purchased from American I SP company), mix homogeneously, obtain compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) after 1kg raw material Folium Bambusae is cleaned being filtered dry, add 5L water, heating and refluxing extraction 4 hours, obtains reflux extracting liquid;
2) above-mentioned reflux extracting liquid is filtered by duplex strainer, obtain mother solution;
3) by the poly-2 mother liquid obtained vacuum concentration that carry out of step, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) concentrated solution step poly-3 being obtained carries out centrifugalize, removes insoluble matter, collects separating medium;
5) by separating medium in step 4, carry out precipitate with ethanol extraction, adding amount of alcohol is 70%, and airtight cold preservation 48 hours is filtered, and filtrate recycling ethanol, obtains refined liquid;
6) step 5 refined liquid is passed through to spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out to vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is sprayed and be dried, obtain compound plant antioxidant component II, the weight of component II is 5g.
(3) component I and component II are composite
By component II and purified water, with 1: 2 ratio of weight ratio, be mixed with aqueous solution, mix with 1.5: 48.5 ratios of weight ratio with component I, obtain compound plant antioxidant sample one.
The preparation (two) of embodiment 2 compound plant antioxidants
(1) preparation of component I
1) raw material is that 15 grams of Cortex Mori, Herba Artemisiae Scopariae are spent 50 grams, 33 grams, 1 gram, Fructus Jujubae and Radix Glycyrrhizae, in raw material, adds 0.3L 1-3 butanediol and 0.6L dehydrated alcohol, soaks 24 hours under room temperature;
2) 45 ℃, stir 2 hours, I filters to get filtrate;
3) in filtering residue, add sterile purified water 1.2L, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II, add in filtering residue, in 45 ℃ of stirrings 2 hours, carries out coarse filtration, obtains mother solution;
5) by mother solution-5 ℃ freezing 12 hours, after filtrate is recovered room temperature, with plate filter, carry out sucking filtration, collect filtrate II I;
6) by filtrate II I rotary evaporation under 60 ℃ of conditions, concentrate, to be concentrated during to 1.0L (concentrated 2 times), the evaporation of stopping the rotation, obtains concentrated solution A;
7) in concentrated solution A, add antiseptic IS-45 (two imidazolidinyl urea and the iodo propinyl butyl meglumine acid acid & methyl hydroxybenzoate & propylene glycol of 2 grams, purchased from American I SP company), mix homogeneously, obtain compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) after 1200kg raw material Folium Bambusae is cleaned being filtered dry, add 5L water, heating and refluxing extraction 4 hours, obtains reflux extracting liquid;
2) above-mentioned reflux extracting liquid is filtered by duplex strainer, obtain mother solution;
3) by the poly-2 mother liquid obtained vacuum concentration that carry out of step, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) concentrated solution step poly-3 being obtained carries out centrifugalize, removes insoluble matter, collects separating medium;
5) by separating medium in step 4, carry out precipitate with ethanol extraction, adding amount of alcohol is 70%, and airtight cold preservation 48 hours is filtered, and filtrate recycling ethanol, obtains refined liquid;
6) step 5 refined liquid is passed through to spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out to vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is sprayed and be dried, obtain compound plant antioxidant component II, the weight of component II is 5.2g.
(3) component I and component II are composite
By component II and purified water, with 1: 2 ratio of weight ratio, be mixed with aqueous solution, mix with 1.5: 48.5 ratios of weight ratio with component I, obtain compound plant antioxidant sample two.
The preparation (three) of embodiment 3 compound plant antioxidants
(1) preparation of component I
1) raw material is that 25 grams of Cortex Mori, Herba Artemisiae Scopariae are spent 20 grams, 50 grams, 6 grams, Fructus Jujubae and Radix Glycyrrhizae, in raw material, adds 0.4L 1-3 butanediol and 0.7L dehydrated alcohol, soaks 24 hours under room temperature;
2) 45 ℃, stir 2 hours, I filters to get filtrate;
3) in filtering residue, add sterile purified water 1.0L, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II, add in filtering residue, in 45 ℃ of stirrings 2 hours, carries out coarse filtration, obtains mother solution;
5) by mother solution-5 ℃ freezing 24 hours, after filtrate is recovered room temperature, with plate filter, carry out sucking filtration, collect filtrate II I;
6) by filtrate II I rotary evaporation under 60 ℃ of conditions, concentrate, to be concentrated during to 0.6L (concentrated 3 times), the evaporation of stopping the rotation, obtains concentrated solution A;
7) in concentrated solution A, add antiseptic IS-45 (two imidazolidinyl urea and the iodo propinyl butyl meglumine acid acid & methyl hydroxybenzoate & propylene glycol of 1.2 grams, purchased from American I SP company), mix homogeneously, obtain compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) after 750kg raw material Folium Bambusae is cleaned being filtered dry, add 5L water, heating and refluxing extraction 4 hours, obtains reflux extracting liquid;
2) above-mentioned reflux extracting liquid is filtered by duplex strainer, obtain mother solution;
3) by the poly-2 mother liquid obtained vacuum concentration that carry out of step, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) concentrated solution step poly-3 being obtained carries out centrifugalize, removes insoluble matter, collects separating medium;
5) by separating medium in step 4, carry out precipitate with ethanol extraction, adding amount of alcohol is 70%, and airtight cold preservation 48 hours is filtered, and filtrate recycling ethanol, obtains refined liquid;
6) step 5 refined liquid is passed through to spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out to vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is sprayed and be dried, obtain compound plant antioxidant component II, the weight of component II is 3.6 grams.
(3) component I and component II are composite
By component II and purified water, with 1: 2 ratio of weight ratio, be mixed with aqueous solution, mix with 1.0: 49 ratios of weight ratio with component I, obtain compound plant antioxidant sample three.
Embodiment 4DPPH antioxidation testing experiment
(1) experimental principle
DPPH (hexichol is for bitterness free acyl radical) analytic process is widely used in the research of hydroxyl radical scavenger character.DPPH is a kind of stable free radical in organic solvent, and its lone pair electrons have strong absorption (aobvious darkviolet) near 517nm.When organic scavenger exists, lone pair electrons are paired, and absorb and disappear or weaken, and absorb the degree weakening by mensuration, can evaluate the activity of free radical scavenger.DPPH method is to evaluate a kind of (response time only needs 20min) fast of natural anti-oxidation activity, easy, flexible feasible method.
(2) experimental apparatus
UV-2000 type ultraviolet/visible spectrophotometer; KS-150 ultrasonic cleaner; The quick vortex mixer of SK-1; SHZ-D (III) circulating water type vacuum pump; UV-2550 ultraviolet spectrophotometer; LP-302 type electronic balance; Volumetric flask.
(3) reagent and preparation
(1) reagent
DPPH (hexichol is for bitterness free acyl radical), Sigma product.Other reagent are domestic analytical pure.
(2) preparation
2.1DPPH (hexichol is for bitterness free acyl radical) solution:
Take 0.1984g DPPH (hexichol is for bitterness free acyl radical), with anhydrous alcohol solution, standardize solution, in 50ml volumetric flask, shakes up, and is stored in refrigerator used time stepwise dilution as storing solution.
2.2 Herba Artemisiae Scopariae flower sample liquid, Radix Glycyrrhizae sample liquid, Cortex Mori sample liquid, Fructus Jujubae sample liquid:
The Herba Artemisiae Scopariae of take flower 100g, Radix Glycyrrhizae 100g, Cortex Mori 100g, Fructus Jujubae 100g are raw material, use the preparation method identical with embodiment 1 component I to prepare respectively Herba Artemisiae Scopariae flower, Radix Glycyrrhizae, Cortex Mori, Fructus Jujubae extracting solution.
2.3 phyllostachys nigra (lodd.ex lindl.) munro var.henonis (miff.) spapf et rendle sample liquid:
Take water as solvent, the component II of embodiment 1 preparation is mixed with to the phyllostachys nigra (lodd.ex lindl.) munro var.henonis (miff.) spapf et rendle sample liquid that concentration is 0.05g/L.
2.4 compound antioxidant sample liquid:
Take water as solvent, the sample one of embodiment 1 preparation is mixed with to the compound antioxidant sample liquid that concentration is 0.2g/L (in solid content).
(4) test method
(1) take dehydrated alcohol as solvent compound concentration be 2 * 10 -4the DPPH solution of mol/L.
(2) accurately pipette sample liquid 2mL in 10mL test tube, add 2mL DPPH solution, make cumulative volume remain 4mL, shake up;
(3) under room temperature, after static 1h, pour in optical path 1cm cuvette, under 517nm, measure absorbance, be recorded as A sample.
(4) in 2mL DPPH solution, add 2mL water, measure its absorbance, this value record is that A is blank, according to the DPPH clearance rate of following formula calculation sample.
Clearance rate (%)=[(A blank-A sample)/A is blank] * 100%
(5) result and evaluation
The preparation of embodiment 5 cleawhite pack
(1) composition of cleawhite pack and proportioning are as shown in table 1:
Table 1
(2) preparation process:
A. A phase, B are heated to respectively mutually to 80 ℃ and stir 15 minutes;
B. A is added to B phase, homogenizing 3 minutes, rotating speed is 6000 revs/min;
C. under stirring, mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 2 minutes, rotating speed is 2000 revs/min;
D. be cooled to below 50 ℃, slowly add C phase, homogenizing 15 seconds, rotating speed is 1500 revs/min;
E. stir below borehole cooling to 45 ℃, add D phase, be under agitation cooled to subsequently 35 ℃, discharging obtains cleawhite pack ().
Embodiment 6 cleawhite pack (two)
(1) composition of cleawhite pack and proportioning are as shown in table 2:
Table 2
(2) preparation process:
A. A phase, B are heated to respectively mutually to 85 ℃ and stir 15 minutes;
B. A is added to B phase, homogenizing 3 minutes, rotating speed is 6000 revs/min;
C. under stirring, mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 1 minute, rotating speed is 2000 revs/min;
D. be cooled to below 50 ℃, slowly add C phase, homogenizing 15 seconds, rotating speed is 1500 revs/min;
E. stir below borehole cooling to 45 ℃, add D phase, be under agitation cooled to subsequently 35 ℃, discharging obtains cleawhite pack (two).
Embodiment 7 cleawhite pack (three)
(1) composition of cleawhite pack and proportioning are as shown in table 3:
Table 3
(2) preparation process:
A. A phase, B are heated to respectively mutually to 80 ℃ and stir 15 minutes;
B. A is added to B phase, homogenizing 3 minutes, rotating speed is 6000 revs/min;
C. under stirring, mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 1 minute, rotating speed is 2000 revs/min;
D. be cooled to below 50 ℃, slowly add C phase, homogenizing 10 seconds, rotating speed is 2000 revs/min;
E. stir below borehole cooling to 45 ℃, add D phase, be under agitation cooled to subsequently 35 ℃, discharging obtains cleawhite pack (three).
Embodiment 6 white-skinned face function evaluation test and evaluation of result
(1) experimental principle
Human experimentation, forms test population by experiment crowd (25-45 year, women), the test subject variation of skin color before and after (and cosmetic industry composition) that makes to apply some make up, thus determine the white-skinned face function of cosmetics (or functional component).
(2) experimental apparatus and sample
Experimental apparatus: MPA9 Multi-functional skin tester (dermal melanin and haemachrome Mexameter MX18 and skin Lab color difference meter test probe, German CK electronics corporation produces).
Given the test agent: cleawhite pack (), cleawhite pack (two), cleawhite pack (three).
(hereinafter to be referred as sample code name)
(3) experiment crowd and testing time
Experimenter amounts to 6 people.Concrete sex composition and age structure are determined at random.If there are during this time 2 people to occur untoward reaction, stop test; Result is not found untoward reaction.
Testing time: 2 hours.
(4) experiment condition and experimental technique
Experiment condition: temperature (℃): 20+1; Humidity (%): 50+10.
Experimental technique:
1. select experimenter's left hand and right hand forearm cycle labeling successively: the tested region of sample sets and blank region;
2. technical staff uses dermal melanin and haemachrome Mexameter MX18 and skin Lab color difference meter test probe to measure the experiment position that experimenter washed through clear water, averages, and is designated as blank value.
3. experimenter, test position and smear sample, use successively three facial film.
4. experimenter, after using facial film 15min, washes away facial film with clear water, until experimenter, sits quietly after 15min, by technical staff, uses dermal melanin and haemachrome Mexameter MX18 and skin Lab color difference meter test probe experiments of measuring position 3 times, averages.
The numerical value that statistics records, analyzes its dermal melanin content and skin brightness Changing Pattern.
(5) interpretation of result
1. melanin content mutation analysis
Fig. 1-3 are sample sets melanin content situation before and after cleawhite pack ()~(three) use.Use after cleawhite pack, melanin content obviously reduces, and interpret sample has the ability of good check melanin, has certain white-skinned face function.
2. skin brightness (L) changes
L characterizes skin brightness, and its value is larger, and color is deflection white more.Before and after cleawhite pack ()~(three) use, result as Figure 4-Figure 6, tested position is used after sample, sample sets L-value of skin when not using sample has the trend of certain increase, and interpret sample has the ability that increases definitely skin brightness.

Claims (10)

1. a natural compound plant antioxidant, is characterized in that, it is to be made by the plant material of following weight portion:
Herba Lophatheri, 750-1200 weight portion; Cortex Mori, 15-40 weight portion; Radix Glycyrrhizae, 20-50 weight portion; Herba Artemisiae Scopariae flower, 20~50 weight portions and Fructus Jujubae, 1~6 weight portion;
Its preparation method comprises the following steps:
A. according to above-mentioned weight portion, take Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae, the concentrated component I that obtains after employing room temperature alcohol leaching;
B. according to above-mentioned weight portion, take Herba Lophatheri, successively by water reflux, extract,, precipitate with ethanol extraction and the concentrated component I I that obtains;
C. component I and component I I are mixed to the natural compound plant antioxidant of acquisition.
2. natural compound plant antioxidant as claimed in claim 1, is characterized in that, it is to be made by the plant material of following composition and proportioning:
Herba Lophatheri, 1000 weight portions; Cortex Mori, 25 weight portions; Radix Glycyrrhizae, 34 weight portions; Herba Artemisiae Scopariae flower, 33 weight portions and Fructus Jujubae, 3 weight portions.
3. a preparation method for natural compound plant antioxidant, is characterized in that, the method comprises the following steps:
A. according to the weight portion described in claim 1 or 2, take Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae, the concentrated component I that obtains after employing room temperature alcohol leaching;
B. according to the weight portion described in claim 1 or 2, take Herba Lophatheri, successively by water reflux, extract,, precipitate with ethanol extraction and the concentrated component I I that obtains;
C. component I and component I I are mixed to the natural compound plant antioxidant of acquisition.
4. preparation method as claimed in claim 3, is characterized in that, the operating process of described steps A is as follows:
A. according to described weight portion, take Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae, added in the 1,3 butylene glycol and/or dehydrated alcohol of 5~10 times of above-mentioned four kinds of raw material gross weights, soak 12~36 hours under room temperature, I filters to get filtrate;
B. the sterile purified water that adds 12~16 times of described above-mentioned four kinds of raw material gross weights in the filtering residue of above-mentioned filtration step gained, 50~70 ℃ of temperature, stir 0.5~2 hour, and II filters to get filtrate;
C. merging filtrate I and filtrate II obtain mother solution, freezing 12~36 hours in-10 ℃~0 ℃;
D. after mother solution recovers room temperature, with 100-200 order filter, carry out sucking filtration, collect to obtain filtrate II I;
E. filtrate II I removes solvent under reduced pressure in 55~65 ℃, to 1/2~1/3 of this filtrate II I original volume, obtains described component I.
5. preparation method as claimed in claim 3, is characterized in that, the operating process of described step B is as follows:
A. raw material Herba Lophatheri is added in the water of 3~8 times of weight, heating and refluxing extraction 2-5 hour, obtains reflux extracting liquid;
B. reflux extracting liquid is filtered, obtain mother solution;
C. mother solution is carried out to vacuum concentration, the 30%-60% to mother solution volume, obtains concentrated solution;
D. concentrated solution is carried out to centrifugalize, remove insoluble matter, collect separating medium;
E. separating medium is carried out to precipitate with ethanol extraction, adding amount of alcohol is the 50%-80% of separating medium cumulative volume, and airtight cold preservation 24-48 hour filters, and obtains precipitate with ethanol extract;
F. precipitate with ethanol extract is filtered, remove impurity, obtain target solution;
G. target solution is carried out to vacuum concentration, subsequent spray is dry, obtains described component I I.
6. a natural compound plant antioxidant, is characterized in that, it is to adopt the method described in claim 4 or 5 to prepare.
7. the natural compound plant antioxidant described in claim 1,2 or 6 has the application in the cosmetics of antioxidation and/or white-skinned face function in preparation.
8. a facial film with whitening anti-aging function, is characterized in that, it is that one-tenth by following weight portion is grouped into:
Emulsifying agent, 1.8-3.5 weight portion; Skin moistening oils and fats, 3.6-44 weight portion; Wetting agent, 2-20 weight portion; Film former, 0.1-1.0 weight portion; Antiseptic, 0.1-1.25 weight portion; Natural compound plant antioxidant described in claim 1,2 or 6,0.1-5.0 weight portion; Deionized water, 45-75 weight portion.
9. a facial film with whitening anti-aging function, is characterized in that, it is that one-tenth by following weight portion is grouped into:
A phase: Arlacel-60 polyoxyethylene ether 1.0~2.0 weight portions, sorbitan monostearate, 0.8~1.5 weight portion; Glyceryl stearate and PEG-100 stearate, 0.5~3.0 weight portion; Cetearyl alcohol, 0.2~5.0 weight portion; Stearic acid, 0.2~4.0 weight portion; Caprylic/capric triglyceride, 1~10 weight portion; Squalane, 1~10 weight portion; Dormant oils, 1~10 weight portion; Dimethicone, 0.2~5.0 weight portion; Methyl parahydroxybenzoate, 0.02~0.2 weight portion; Propyl p-hydroxybenzoate, 0.02~0.15 weight portion;
B phase: water, 45~75 weight portions; Butanediol, 1~10 weight portion; Glycerol, 1~10 weight portion; Hydroxyethyl-cellulose, 0.1~1.0 weight portion; Allantoin, 0.1~0.3 weight portion; Titanium dioxide, 0.5~5.0 weight portion; Nicotiamide, 0.2~3.0 weight portion;
C phase: De Minshu, 0.01~0.5 weight portion; Fragrant quick relaxing, 0.01~0.3 weight portion; Natural compound plant antioxidant described in claim 1,2 or 6,0.1~5.0 weight portion;
D phase: dihydroxymethyl dimethyl hydantoin and/or iodo propinyl butyl chloride carbamate, 0.1~0.8 weight portion; Essence, 0.01~0.03 weight portion.
10. the preparation method of facial film as claimed in claim 9, is characterized in that, the method comprises the following steps:
A. A phase, B are heated to respectively mutually to 75~85 ℃ and stir 10~20 minutes;
B. A is added to B phase, homogenizing 2~5 minutes, rotating speed is 3000~6000 revs/min;
C. under stirring, mixture is cooled to 60~65 ℃, is heated to subsequently 70~80 ℃, homogenizing 1~2 minute, rotating speed is 1500~3000 revs/min;
D. mixture step c being obtained is cooled to below 50 ℃, slowly adds C phase, homogenizing 10~20 seconds, and rotating speed is 1000~2000 revs/min;
E. mixture steps d being obtained stirs below borehole cooling to 45 ℃, adds D phase, is under agitation cooled to subsequently 35~38 ℃, discharging.
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CN105434233B (en) * 2015-12-08 2017-03-22 广州市花安堂生物科技有限公司 Keratin repair essence
CN107569413A (en) * 2017-08-16 2018-01-12 佛山实瑞先导材料研究院(普通合伙) A kind of antioxidant and its application
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CN108066189A (en) * 2017-12-19 2018-05-25 北京明弘科贸有限责任公司 There is the anti-ageing ganoderma lucidum skin care compositions for dispelling yellow and its application
CN108553396A (en) * 2018-05-28 2018-09-21 四川农业大学 A kind of anti-ageing natural compound facial mask of safe whitening and preparation method thereof
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