CN102940597A - 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 PDFInfo
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- CN102940597A CN102940597A CN2012105147766A CN201210514776A CN102940597A CN 102940597 A CN102940597 A CN 102940597A CN 2012105147766 A CN2012105147766 A CN 2012105147766A CN 201210514776 A CN201210514776 A CN 201210514776A CN 102940597 A CN102940597 A CN 102940597A
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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
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 (such as BHT, BHA etc.) of synthetic has many side effect, liver, spleen, the lung of human body all there is adverse effect, utilizing the Natural antioxidant to prevent and cure diseases becomes study hotspot.Natural plant antioxidant has that the source is wide, antioxidant activity large, strong and safety is high with the 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 the metal ion by electron transfer, complex catalysis oxidation, associating antioxidation and affect the approach such as gene expression and play a role in vivo.The antioxidant activity that plant extract is found in research often greater than single from composition, demonstration 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 satisfy 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 kind of natural compound plant antioxidant, it is to be made by the plant material of following composition and proportioning:
Herba Lophatheri, the 750-1200 weight portion; Cortex Mori, the 15-40 weight portion; Radix Glycyrrhizae, the 20-50 weight portion; The Herba Artemisiae Scopariae flower, 20～50 weight portions; And Fructus Jujubae, 1～6 weight portion.
Aforesaid natural compound plant antioxidant, 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; The Herba Artemisiae Scopariae flower, 33 weight portions; And Fructus Jujubae, 3 weight portions.
Aforesaid natural compound plant antioxidant, 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; The Herba Artemisiae Scopariae flower, 33 weight portions; And Fructus Jujubae, 1 weight portion.
Aforesaid natural compound plant antioxidant, 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; The Herba Artemisiae Scopariae flower, 50 weight portions; And Fructus Jujubae, 6 weight portions.
A kind of preparation method of natural compound plant antioxidant, the method may further comprise the steps:
A. weight portion takes by weighing Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae as described above, the concentrated component I that obtains after the employing room temperature alcohol leaching;
B. weight portion takes by weighing 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 the natural compound plant antioxidant of acquisition.
Aforesaid preparation method, preferably, the operating process of described steps A is as follows:
A. the Cortex Mori that takes by weighing according to described weight portion, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae add it in 1-3 butanediol and/or dehydrated alcohol of 5～10 times of solid material gross weights, soak under the room temperature 12～36 hours, and I filters to get filtrate;
B. add the sterile purified water of 12～16 times of described solid material gross weights in the filtering residue of above-mentioned filtration step gained, 50～70 ℃ of temperature stirred 0.5～2 hour, and II filters to get filtrate;
C. merging filtrate I and filtrate II obtain mother solution, and be freezing 12～36 hours in-10 ℃～0 ℃;
D. after mother solution recovers room temperature, carry out sucking filtration with 100-200 order filter, 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.
Aforesaid preparation method, preferably, the operating process of described step B is as follows:
A. the raw material Herba Lophatheri is added in the water of 3～8 times of weight, heating and refluxing extraction 2-5 hour, obtain reflux extracting liquid;
B. reflux extracting liquid is filtered, obtain mother solution;
C. mother solution is carried out vacuum concentration, the 30%-60% to the mother solution volume gets concentrated solution;
D. concentrated solution is carried out centrifugalize, remove insoluble matter, collect separating medium;
E. separating medium is carried out the precipitate with ethanol extraction, adding amount of alcohol is the 50%-80% of separating medium cumulative volume, airtight cold preservation 24-48 hour, filter, and obtain the precipitate with ethanol extract;
F. the precipitate with ethanol extract is filtered, remove impurity, obtain target solution;
G. target solution is carried out vacuum concentration, subsequent spray is dry, obtains described component I I.
A kind of natural compound plant antioxidant, it adopts aforesaid method to prepare.
Natural compound plant antioxidant of the present invention has application in the cosmetics of antioxidation and/or white-skinned face function in preparation.
A kind of facial film with whitening anti-aging function, it is that one-tenth by following proportioning is grouped into:
Emulsifying agent, the 1.8-3.5 weight portion; The skin moistening oils and fats, the 3.6-44 weight portion; Wetting agent, the 2-20 weight portion; Film former, the 0.1-1.0 weight portion; Antiseptic, the 0.1-1.25 weight portion; Natural compound plant antioxidant of the present invention, the 0.1-5.0 weight portion; Deionized water, the 45-75 weight portion.
Aforesaid facial film with whitening anti-aging function, preferably, it is that one-tenth by following proportioning is grouped into:
Emulsifying agent, the 2-3 weight portion; The skin moistening oils and fats, the 15-25 weight portion; Wetting agent, the 10-20 weight portion; Film former, the 0.2-0.8 weight portion; Antiseptic, the 0.1-0.5 weight portion; Natural compound plant antioxidant of the present invention, the 0.1-5.0 weight portion; Deionized water, the 45-75 weight portion.
A kind of 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 easypro, 0.01～0.3 weight portion; Claim 1 or 6 described natural compound plant antioxidants, 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.
Aforesaid facial film with whitening anti-aging function, 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 easypro, 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.
Aforesaid facial film with whitening anti-aging function, 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 easypro, 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.
Aforesaid facial film with whitening anti-aging function, 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 easypro, 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 may further comprise the steps:
A. A phase, B are heated to respectively mutually 75～85 ℃ and stirred 10～20 minutes;
B. A is added to the B phase, homogenizing 2～5 minutes, rotating speed are 3000～6000 rev/mins;
C. under stirring mixture is cooled to 60～65 ℃, is heated to subsequently 70～80 ℃, homogenizing 1～2 minute, rotating speed are 1500～3000 rev/mins;
D. the mixture that step c is obtained is cooled to below 50 ℃, slowly adds the C phase, and homogenizing 10～20 seconds, rotating speed are 1000～2000 rev/mins;
E. the mixture that steps d is obtained stirs below the borehole cooling to 45 ℃, adds the D phase, under agitation is cooled to subsequently 35～38 ℃, discharging.
A kind of facial film with whitening anti-aging function, it adopts aforesaid method 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, Herba Lophatheri extract contains flavone compound and the polysaccharide of tool antioxidant activity, Cortex Mori is rich in flavone compound, Radix Glycyrrhizae has licoflavone and Angelica Polysaccharide, and the Herba Artemisiae Scopariae flower is rich in flavone compound, is rich in jujube polysaccharide and VE, VC in the 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.
Simultaneously, 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 and the distribution of pigment in epidermis cell, accelerates the melanin metabolism; Thereby has a white-skinned face function.
Experimental result shows, natural compound plant antioxidant of the present invention is used for cosmetics and has whitening and senile-resistant efficacy.
Description of drawings
Fig. 1 is melanin content situation before and after cleawhite pack () uses;
Fig. 2 is melanin content situation before and after cleawhite pack (two) uses;
Fig. 3 is melanin content situation before and after cleawhite pack (three) uses;
Fig. 4 is the situation of change of skin brightness (L) before and after cleawhite pack () uses;
Fig. 5 is the situation of change of skin brightness (L) before and after cleawhite pack (two) uses;
Fig. 6 is the situation of change of skin brightness (L) before and after cleawhite pack (three) uses.
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 Cortex Mori 25 grams, Herba Artemisiae Scopariae are spent 33 grams, Fructus Jujubae 3 grams and Radix Glycyrrhizae 34 grams, adds 0.3L 1-3 butanediol and 0.7L dehydrated alcohol in raw material, soaks 24 hours under the room temperature;
2) 45 ℃, stirred 2 hours, I filters to get filtrate;
3) add sterile purified water 1.5L in the filtering residue, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II add in the filtering residue, in 45 ℃ of stirrings 2 hours, filter, and obtain mother solution;
5) with mother solution-5 ℃ freezing 24 hours, after filtrate is recovered room temperature, carry out sucking filtration with plate filter, collect filtrate II I;
6) with 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) add the 1.4 antiseptic IS-45 that restrain (two imidazolidinyl urea and iodo propinyl butyl meglumine acid acid ﹠amp among the concentrated solution A; Ni Bojinjiazhi ﹠amp; Propylene glycol is available from American I SP company), mix homogeneously obtains compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) 1kg raw material Folium Bambusae is cleaned be filtered dry after, 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) will go on foot the poly-2 mother liquid obtained vacuum concentration that carry out, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) will go on foot poly-3 concentrated solutions that obtain and carry out centrifugalize, remove insoluble matter, collect separating medium;
5) with separating medium in the step 4, carry out the 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 the spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is carried out spray drying, obtain compound plant antioxidant component II, the weight of component II is 5g.
(3) component I and component II are composite
With component II and purified water, be mixed with aqueous solution with 1: 2 ratio of weight ratio, 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 Cortex Mori 15 grams, Herba Artemisiae Scopariae are spent 33 grams, Fructus Jujubae 1 gram and Radix Glycyrrhizae 50 grams, adds 0.3L 1-3 butanediol and 0.6L dehydrated alcohol in raw material, soaks 24 hours under the room temperature;
2) 45 ℃, stirred 2 hours, I filters to get filtrate;
3) add sterile purified water 1.2L in the filtering residue, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II add in the filtering residue, in 45 ℃ of stirrings 2 hours, carry out coarse filtration, obtain mother solution;
5) with mother solution-5 ℃ freezing 12 hours, after filtrate is recovered room temperature, carry out sucking filtration with plate filter, collect filtrate II I;
6) with 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) add the 2 antiseptic IS-45 that restrain (two imidazolidinyl urea and iodo propinyl butyl meglumine acid acid ﹠amp among the concentrated solution A; Ni Bojinjiazhi ﹠amp; Propylene glycol is available from American I SP company), mix homogeneously obtains compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) 1200kg raw material Folium Bambusae is cleaned be filtered dry after, 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) will go on foot the poly-2 mother liquid obtained vacuum concentration that carry out, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) will go on foot poly-3 concentrated solutions that obtain and carry out centrifugalize, remove insoluble matter, collect separating medium;
5) with separating medium in the step 4, carry out the 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 the spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is carried out spray drying, obtain compound plant antioxidant component II, the weight of component II is 5.2g.
(3) component I and component II are composite
With component II and purified water, be mixed with aqueous solution with 1: 2 ratio of weight ratio, 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 Cortex Mori 25 grams, Herba Artemisiae Scopariae are spent 50 grams, Fructus Jujubae 6 grams and Radix Glycyrrhizae 20 grams, adds 0.4L 1-3 butanediol and 0.7L dehydrated alcohol in raw material, soaks 24 hours under the room temperature;
2) 45 ℃, stirred 2 hours, I filters to get filtrate;
3) add sterile purified water 1.0L in the filtering residue, in 60 ℃ of stirrings 1 hour, II filtered to get filtrate;
4) merging filtrate I and filtrate II add in the filtering residue, in 45 ℃ of stirrings 2 hours, carry out coarse filtration, obtain mother solution;
5) with mother solution-5 ℃ freezing 24 hours, after filtrate is recovered room temperature, carry out sucking filtration with plate filter, collect filtrate II I;
6) with 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) add the 1.2 antiseptic IS-45 that restrain (two imidazolidinyl urea and iodo propinyl butyl meglumine acid acid ﹠amp among the concentrated solution A; Ni Bojinjiazhi ﹠amp; Propylene glycol is available from American I SP company), mix homogeneously obtains compound plant antioxidant component I, this constant product quality.
(2) preparation of component II
1) 750kg raw material Folium Bambusae is cleaned be filtered dry after, 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) will go on foot the poly-2 mother liquid obtained vacuum concentration that carry out, to 50% of mother solution application of sample amount volume, obtain concentrated solution;
4) will go on foot poly-3 concentrated solutions that obtain and carry out centrifugalize, remove insoluble matter, collect separating medium;
5) with separating medium in the step 4, carry out the 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 the spiral wound membrane filtration, remove the macromole impurity such as albumen, obtain target solution;
7) target solution is carried out vacuum concentration, to 20% of target solution volume;
8) step 7 concentrated solution is carried out spray drying, obtain compound plant antioxidant component II, the weight of component II is 3.6 grams.
(3) component I and component II are composite
With component II and purified water, be mixed with aqueous solution with 1: 2 ratio of weight ratio, 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 the 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 existed, lone pair electrons were paired, and absorption disappears or weakens, and absorbed the degree that weakens by measuring, and can estimate the activity of free radical scavenger.The DPPH method is to estimate a kind of fast (response time only needs 20min) of natural anti-oxidation activity, easy, flexible feasible method.
(2) experimental apparatus
UV-2000 type ultraviolet/visible spectrophotometer; The KS-150 ultrasonic cleaner; The quick vortex mixer of SK-1; SHZ-D (III) circulating water type vacuum pump; The UV-2550 ultraviolet spectrophotometer; LP-302 type electronic balance; Volumetric flask.
(3) reagent and preparation
(1) reagent
DPPH (hexichol is for the bitterness free acyl radical), the Sigma product.Other reagent are domestic analytical pure.
(2) preparation
(2.1DPPH hexichol is for the bitterness free acyl radical) solution:
Take by weighing 0.1984g DPPH (hexichol is for the bitterness free acyl radical), use anhydrous alcohol solution, standardize solution shakes up in the 50ml volumetric flask, is stored in the refrigerator time spent 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:
Take Herba Artemisiae Scopariae flower 100g, Radix Glycyrrhizae 100g, Cortex Mori 100g, Fructus Jujubae 100g as 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 that embodiment 1 is prepared is mixed with 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 that embodiment 1 is prepared is mixed with the compound antioxidant sample liquid that concentration is 0.2g/L (in solid content).
(4) test method
(1) take dehydrated alcohol as the solvent compound concentration as 2 * 10
-4The DPPH solution of mol/L.
(2) accurately pipette sample liquid 2mL in the 10mL test tube, add 2mL DPPH solution, make cumulative volume remain 4mL, shake up;
(3) pour into behind the static 1h in the optical path 1cm cuvette under the room temperature, under 517nm, measure absorbance, be recorded as the A sample.
(4) add 2mL water in 2mL DPPH solution, 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 80 ℃ and stirred 15 minutes;
B. A is added to the B phase, homogenizing 3 minutes, rotating speed are 6000 rev/mins;
C. under stirring mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 2 minutes, rotating speed are 2000 rev/mins;
D. be cooled to below 50 ℃, slowly add the C phase, homogenizing 15 seconds, rotating speed are 1500 rev/mins;
E. stir below the borehole cooling to 45 ℃, add the D phase, under agitation be cooled to subsequently 35 ℃, discharging gets 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 85 ℃ and stirred 15 minutes;
B. A is added to the B phase, homogenizing 3 minutes, rotating speed are 6000 rev/mins;
C. under stirring mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 1 minute, rotating speed are 2000 rev/mins;
D. be cooled to below 50 ℃, slowly add the C phase, homogenizing 15 seconds, rotating speed are 1500 rev/mins;
E. stir below the borehole cooling to 45 ℃, add the D phase, under agitation be cooled to subsequently 35 ℃, discharging gets 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 80 ℃ and stirred 15 minutes;
B. A is added to the B phase, homogenizing 3 minutes, rotating speed are 6000 rev/mins;
C. under stirring mixture is cooled to 60 ℃, is heated to subsequently 75 ℃, homogenizing 1 minute, rotating speed are 2000 rev/mins;
D. be cooled to below 50 ℃, slowly add the C phase, homogenizing 10 seconds, rotating speed are 2000 rev/mins;
E. stir below the borehole cooling to 45 ℃, add the D phase, under agitation be cooled to subsequently 35 ℃, discharging gets 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), and test subject makes the variation of skin color before and after apply some make up (and cosmetic industry composition), thereby determines 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 the sample code name)
(3) experiment crowd and testing time
The experimenter amounts to 6 people.Concrete sex composition and age structure are determined at random.If there are during this time 2 people untoward reaction to occur, then stop test; The result does not find untoward reaction.
Testing time: 2 hours.
(4) experiment condition and experimental technique
Experiment condition: temperature (℃): 20+1; Humidity (%): 50+10.
Experimental technique:
1. select successively cycle labeling of experimenter's left hand and right hand forearm: the tested zone of sample sets and blank zone;
2. the technical staff uses dermal melanin and haemachrome Mexameter MX18 and skin Lab color difference meter test probe to measure the experimenter through the experiment position that clear water was washed, and averages, and is designated as blank value.
3. test the position the experimenter and smear sample, use successively three facial film.
4. the experimenter is after using facial film 15min, with the facial film flush away, after the experimenter sits quietly 15min, uses dermal melanin and haemachrome Mexameter MX18 and skin Lab color difference meter test probe experiments of measuring position 3 times by the technical staff with clear water, averages.
The numerical value that statistics records is analyzed its dermal melanin content and skin brightness Changing Pattern.
(5) interpretation of result
1. melanin content mutation analysis
Fig. 1-3 is sample sets melanin content situation before and after cleawhite pack ()～(three) use.After using cleawhite pack, melanin content obviously reduces, and interpret sample has the preferably ability of check melanin, namely 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.The result was shown in Fig. 4-6 before and after cleawhite pack ()～(three) used, after sample is used at tested position, 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 composition and proportioning:
Herba Lophatheri, the 750-1200 weight portion; Cortex Mori, the 15-40 weight portion; Radix Glycyrrhizae, the 20-50 weight portion; The Herba Artemisiae Scopariae flower, 20～50 weight portions; And Fructus Jujubae, 1～6 weight portion.
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; The Herba Artemisiae Scopariae flower, 33 weight portions; And Fructus Jujubae, 3 weight portions.
3. the preparation method of a natural compound plant antioxidant is characterized in that, the method may further comprise the steps:
A. take by weighing Cortex Mori, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae according to the weight portion described in claim 1 or 2, the concentrated component I that obtains after the employing room temperature alcohol leaching;
B. take by weighing Herba Lophatheri according to the weight portion described in claim 1 or 2, successively by water reflux, extract,, precipitate with ethanol extraction and the concentrated component II that obtains;
C. component I and component II are mixed 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. the Cortex Mori that takes by weighing according to described weight portion, Radix Glycyrrhizae, Herba Artemisiae Scopariae flower and Fructus Jujubae add it in 1-3 butanediol and/or dehydrated alcohol of 5～10 times of solid material gross weights, soak under the room temperature 12～36 hours, and I filters to get filtrate;
B. add the sterile purified water of 12～16 times of described solid material gross weights in the filtering residue of above-mentioned filtration step gained, 50～70 ℃ of temperature stirred 0.5～2 hour, and II filters to get filtrate;
C. merging filtrate I and filtrate II obtain mother solution, and be freezing 12～36 hours in-10 ℃～0 ℃;
D. after mother solution recovers room temperature, carry out sucking filtration with 100-200 order filter, 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.
5. preparation method as claimed in claim 3 is characterized in that, the operating process of described step B is as follows:
A. the raw material Herba Lophatheri is added in the water of 3～8 times of weight, heating and refluxing extraction 2-5 hour, obtain reflux extracting liquid;
B. reflux extracting liquid is filtered, obtain mother solution;
C. mother solution is carried out vacuum concentration, the 30%-60% to the mother solution volume gets concentrated solution;
D. concentrated solution is carried out centrifugalize, remove insoluble matter, collect separating medium;
E. separating medium is carried out the precipitate with ethanol extraction, adding amount of alcohol is the 50%-80% of separating medium cumulative volume, airtight cold preservation 24-48 hour, filter, and obtain the precipitate with ethanol extract;
F. the precipitate with ethanol extract is filtered, remove impurity, obtain target solution;
G. target solution is carried out vacuum concentration, subsequent spray is dry, obtains described component I I.
6. a natural compound plant antioxidant is characterized in that, it adopts, and each described method prepares among the claim 3-5.
7. natural compound plant antioxidant claimed in claim 6 has application in the cosmetics of antioxidation and/or white-skinned face function in preparation.
8. the facial film with whitening anti-aging function is characterized in that, it is that one-tenth by following proportioning is grouped into:
Emulsifying agent, the 1.8-3.5 weight portion; The skin moistening oils and fats, the 3.6-44 weight portion; Wetting agent, the 2-20 weight portion; Film former, the 0.1-1.0 weight portion; Antiseptic, the 0.1-1.25 weight portion; Claim 1 or 6 described natural compound plant antioxidants, the 0.1-5.0 weight portion; Deionized water, the 45-75 weight portion.
9. the facial film with whitening anti-aging function is characterized in that, 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 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 easypro, 0.01～0.3 weight portion; Claim 1 or 6 described natural compound plant antioxidants, 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 the described facial film of claim 9 is characterized in that, the method may further comprise the steps:
A. A phase, B are heated to respectively mutually 75～85 ℃ and stirred 10～20 minutes;
B. A is added to the B phase, homogenizing 2～5 minutes, rotating speed are 3000～6000 rev/mins;
C. under stirring mixture is cooled to 60～65 ℃, is heated to subsequently 70～80 ℃, homogenizing 1～2 minute, rotating speed are 1500～3000 rev/mins;
D. the mixture that step c is obtained is cooled to below 50 ℃, slowly adds the C phase, and homogenizing 10～20 seconds, rotating speed are 1000～2000 rev/mins;
E. the mixture that steps d is obtained stirs below the borehole cooling to 45 ℃, adds the D phase, under agitation is cooled to subsequently 35～38 ℃, discharging.
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| CN104510637A (en) * | 2013-09-26 | 2015-04-15 | 青岛锦涟鑫商贸有限公司 | Chinese herbal medicine spot removing mask |
| CN104510636A (en) * | 2013-09-26 | 2015-04-15 | 青岛锦涟鑫商贸有限公司 | Traditional Chinese medicine whitening mask |
| CN105434233A (en) * | 2015-12-08 | 2016-03-30 | 广州市花安堂生物科技有限公司 | Keratin repair essence and preparation method thereof |
| CN107468566A (en) * | 2017-08-16 | 2017-12-15 | 佛山实瑞先导材料研究院（普通合伙） | A kind of antioxidant and its application |
| 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 |
| 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 |
| CN111012702A (en) * | 2018-10-10 | 2020-04-17 | 株式会社利奥化学韩国 | Cosmetic composition containing herba Artemisiae Scopariae extract obtained by Heat-tin extraction method and low temperature aging as effective component |
| CN111419747A (en) * | 2020-04-18 | 2020-07-17 | 北温草生物科技(上海)有限公司 | Chinese herbal medicine composition for whitening and brightening skin |
| CN113018228A (en) * | 2021-01-28 | 2021-06-25 | 泉后(广州)生物科技研究院有限公司 | Anti-aging composition, cream and preparation method thereof |
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| CN104510637A (en) * | 2013-09-26 | 2015-04-15 | 青岛锦涟鑫商贸有限公司 | Chinese herbal medicine spot removing mask |
| CN104510636A (en) * | 2013-09-26 | 2015-04-15 | 青岛锦涟鑫商贸有限公司 | Traditional Chinese medicine whitening mask |
| CN105434233A (en) * | 2015-12-08 | 2016-03-30 | 广州市花安堂生物科技有限公司 | Keratin repair essence and preparation method thereof |
| CN107468566A (en) * | 2017-08-16 | 2017-12-15 | 佛山实瑞先导材料研究院（普通合伙） | A kind of antioxidant and its application |
| 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 |
| 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 |
| CN111012702A (en) * | 2018-10-10 | 2020-04-17 | 株式会社利奥化学韩国 | Cosmetic composition containing herba Artemisiae Scopariae extract obtained by Heat-tin extraction method and low temperature aging as effective component |
| CN111419747A (en) * | 2020-04-18 | 2020-07-17 | 北温草生物科技(上海)有限公司 | Chinese herbal medicine composition for whitening and brightening skin |
| CN113018228A (en) * | 2021-01-28 | 2021-06-25 | 泉后(广州)生物科技研究院有限公司 | Anti-aging composition, cream and preparation method thereof |
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