CN106309346A - Compound skin external preparation containing brasenia schreberi, preparation method and application thereof - Google Patents

Compound skin external preparation containing brasenia schreberi, preparation method and application thereof Download PDF

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CN106309346A
CN106309346A CN201510364929.7A CN201510364929A CN106309346A CN 106309346 A CN106309346 A CN 106309346A CN 201510364929 A CN201510364929 A CN 201510364929A CN 106309346 A CN106309346 A CN 106309346A
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powder
folium braseniae
braseniae schreberi
radix glycyrrhizae
tremella
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CN106309346B (en
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何正有
屠银芳
姚洁
李维
刘婧
邹昆
蒋用
毕建军
聂敏奎
林明
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Chengdu University
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Chengdu University
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Abstract

The invention discloses a raw material composition of a skin external preparation. The composition includes, by weight, 10-90 parts of brasenia schreberi powder, 10-50 parts of radix glycyrrhizae, and 5-90 parts of white fungus. The invention also discloses a skin external preparation stock solution, which includes, by weight, 10-90 parts of an extract liquid of the brasenia schreberi, 10-50 parts of an extract liquid of the radix glycyrrhizae, and 5-90 parts of an extract liquid of the white fungus. The invention also discloses a method of preparing the skin external preparation stock solution, which includes the steps of: adding the brasenia schreberi powder, radix glycyrrhizae powder and white fungus powder in water, maintaining the temperature for 1-2 h at 60 DEG C and performing extraction for 0.5-2 h, wherein the temperature is not less than 60 DEG C during extraction, and centrifuging the extract to obtain a supernatant and filtering the supernatant, purifying the supernatant through a polyamide column, and concentrating the supernatant. The invention also discloses application of the stock solution in preparation of the skin external preparation. The skin external preparation employs easy-to-obtained raw materials, is low in cost, has quite excellent moisturizing, anti-oxidizing and free radical removal performances, is simple in preparation method and low in production cost, and is free of organic solvent, pigment and tanning.

Description

Compound skin external preparation containing Folium Braseniae Schreberi and preparation method and application
Technical field
The invention belongs to preparation for external application to skin field, be specifically related to a kind of compound skin external preparation raw material containing Folium Braseniae Schreberi, stock solution and its preparation method and application.
Background technology
When evaluating preparation for external application to skin (particularly cosmetic formulations) and being the most excellent, in addition to humidity-preserving type, such as non-oxidizability and removing free radical performance are also the important indicators evaluated.Have the preparation for external application to skin of multiple excellent efficacy concurrently, be the important research content of research worker.
Existing preparation for external application to skin the most all contains a small amount of organic solvent (such as ethanol), although the use of organic solvent facilitates the extraction of effective ingredient in preparation (such as antioxidant and antifree radical agent), but also result in production cost height enterprise and may adversely affect skin.
Owing to a lot of medicinal and edible plants are less to skin damage, medicinal and edible plant is concerned by people as preparation for external application to skin always.But, owing to (1) various medicinal and edible plant is widely different for the active constituent content preparing preparation for external application to skin;(2) medicinal and edible plant composition is more, extracts difficulty bigger;(3) medicinal and edible plant is the most corrupt, and its composition is wayward;Therefore, how to select suitable medicinal and edible plant, stablize its composition and constitute and extract its effective ingredient efficiently and make excellent preparation for external application to skin, become problem demanding prompt solution.
Chinese crude drug is the rarity of the Chinese nation, is applied to preparation for external application to skin, particularly cosmetic formulations, is the pursuit for many years of this area research worker.But, owing to external preparation for skin goods have particular/special requirement, such as humidity-preserving type, non-oxidizability, non-zest etc. and the most deep to the related development of Chinese herbal medicine, cause the bad present situation that the application of Chinese herbal medicine is restricted.
Therefore, medicinal and edible plant and Chinese herbal medicine how is selected to carry out compounding making the research that excellent preparation for external application to skin is a great challenge.
Summary of the invention
The problem needing solution for the shortcoming of prior art and this area badly, an object of the present invention is to provide a kind of preparation for external application to skin feedstock composition, said composition by weight, including:
Folium Braseniae Schreberi powder 10-90 part
Radix Glycyrrhizae 10-50 part
Tremella 5-90 part;
Described Folium Braseniae Schreberi powder is that fresh Folium Braseniae Schreberi is spray-dried gained after homogenized;
Described preparation for external application to skin includes facial film, essence, emulsion, emulsifiable paste, gel preparation.
Preferably, said composition by weight, including:
Folium Braseniae Schreberi powder 30-60 part
Radix Glycyrrhizae 10-30 part
Tremella 20-60 part.
Preferably, described Folium Braseniae Schreberi powder be fresh Folium Braseniae Schreberi is cleaned after, add the volume pure water less than volume shared by Folium Braseniae Schreberi leaf, utilize refiner to process 30 min under 4000rpm, carry out being spray-dried gained at 60 DEG C.
A kind of preparation for external application to skin stock solution of offer is provided, this stock solution by weight, including:
Folium Braseniae Schreberi extracting solution 10-90 part
Radix Glycyrrhizae extract 10-50 part
Tremella extract 5-90 part;
In described Folium Braseniae Schreberi extracting solution, polyoses content is at least 0.6 mg/ml, and Folium Braseniae Schreberi total polyphenols is at least 1.2 × 10-4mg/ml Without pigment tanning and organic solvent;In described Radix Glycyrrhizae extract, glycyrrhizic acid is at least 2.08 × 10-3mg/ml;In described tremella extract, tremella polysaccharide is at least 2.5 × 10-3mg/ml。
As shown in the embodiment of the present invention, stock solution of the present invention has a most outstanding humidity-preserving type, more outstanding than the performance of keeping humidity of existing outstanding commercial goods and possess the most significant non-oxidizability and remove the ability of free radical.
Tremella polysaccharide and Polysaccharide of Brasenia Schreberi with the use of, the synergism of polysaccharide strengthens its skin-moisturizing, skin effect, provides more nutrition simultaneously, the addition of Tremella so that prepared skin preparation quality is more preferable, and skin affinity strengthens, and viscosity and transparency increase, and moistening effect increases.Radix Glycyrrhizae plays antiinflammatory whitening function, uses with Folium Braseniae Schreberi compatibility, and its antiinflammatory antioxidant activity strengthens, and has the whitening and skin-protecting effect of gentleness concurrently.Radix Glycyrrhizae and Tremella are all warm nature, and sweet in the mouth is nontoxic, and Folium Braseniae Schreberi sweet in the mouth cold in nature is nontoxic, and after three's compatibility, inventory reduces, and skin care effect is strengthened, it is to avoid extract concentrations height affects the quality of product, produces a desired effect simultaneously.
Preferably, this stock solution by weight, including:
Folium Braseniae Schreberi extracting solution 30-60 part
Radix Glycyrrhizae extract 10-30 part
Tremella extract 20-60 part.
Further object is that and provide the method preparing above-mentioned stock solution, the method comprises the steps:
(1) prepared by Folium Braseniae Schreberi powder: carry out being homogenized being spray-dried by fresh Folium Braseniae Schreberi again, obtains Folium Braseniae Schreberi powder, storage;
(2) with water, Radix Glycyrrhizae powder, Tremella powder, step (1) gained Folium Braseniae Schreberi powder are extracted respectively, obtain Radix Glycyrrhizae extract, tremella extract, Folium Braseniae Schreberi extracting solution respectively;Controlling in Folium Braseniae Schreberi extracting solution, polyoses content is at least 0.6 Mg/ml, Folium Braseniae Schreberi total polyphenols is at least 1.2 × 10-4mg/ml Without pigment tanning and organic solvent;Control glycyrrhizic acid in Radix Glycyrrhizae extract and be at least 2.08 × 10-3mg/ml;Control tremella polysaccharide in tremella extract and be at least 2.5 × 10-3mg/ml;By weight, by Folium Braseniae Schreberi extracting solution 10-90 part, Radix Glycyrrhizae extract 10-50 part, the mixing of tremella extract 5-90 part;
Or, by weight, 5-90 part Radix Glycyrrhizae powder, 10-50 part Tremella powder, the Folium Braseniae Schreberi powder of 10-90 part step (1) gained are added to the water as raw material, the volume addition of water is at least 40 times of volume shared by raw material dry weight, at 60 DEG C, it is incubated 1-2 hour, extracts 0.5-2 hour at a temperature of at least 60 DEG C;
(3) by step (2) gains under at least 6000 rpm, centrifugal 10-30 min, take supernatant;
(4) by step (2) and step (3) described method, step (3) gained precipitate is extracted and separates, take supernatant, and merge with step (3) gained supernatant;
(5) step (4) gains are crossed polyamide column, spend centrifugal water eluting;
(6) step (5) effluent is filtered, be concentrated into 20 times of volume shared by raw material dry weight, to obtain final product.
The domestic research to Folium Braseniae Schreberi is concentrated mainly on Polysaccharide of Brasenia Schreberi semifinished product extraction process, and extracting method is complex, and is prone to extract the impurity such as pigment tannin, and polysaccharide viscosity is big, it is difficult to purification, thus affects product quality.The colloid of Folium Braseniae Schreberi attachment easily comes off after plucking a period of time, due to more containing moisture, the most rotten, and traditional furnace drying method is time-consumingly long and causes Folium Braseniae Schreberi leaf variable color serious, and lyophilization efficiency is low and cost is high.Fresh tender leaf colloid is best in quality, the highest with Folium Braseniae Schreberi yield in summer again, and how to be preserved and not destroy its colloid by the Folium Braseniae Schreberi of a large amount of for summer high-qualitys is problem demanding prompt solution.
The extraction ratio to Polysaccharide of Brasenia Schreberi of the present invention at least can reach 0.6 mg/ml, and does not use organic solvent, does not also contain the foreign material such as pigment tanning, and not only production cost is low, it is often more important that be particularly suitable as preparing the raw material of preparation for external application to skin.
Preferably, in step (1), described Folium Braseniae Schreberi powder be fresh Folium Braseniae Schreberi is cleaned after, add the volume pure water less than volume shared by Folium Braseniae Schreberi leaf, utilize refiner to process 30 min under 4000rpm, carry out being spray-dried gained at 60 DEG C;In step (5), the packing volume of polyamide column is extracting solution 3-4 times, and flow velocity is 1.0 ml/min, the deionization washing post of 1 times of column volume, collects effluent;In step (6), filter method is successively with 200 mesh gauzes, filter paper, 5 μm membrane filtrations;Method for concentration includes rotary evaporation, ultrafiltration, dialysis.
In step 1, fresh Folium Braseniae Schreberi contains large quantity of moisture (about 97%), and external colloid enriches (965g volume is 1000ml), adds a small amount of pure water, when addition is amassed more than monoploid, is unfavorable for homogenate and spray drying.Blade can be crushed by homogenate 4000rpm, 30min, and degree of grinding is moderate.60 DEG C are dried and will not destroy its composition, and drying efficiency liquid is ideal.
In step 2, Folium Braseniae Schreberi and Tremella ratio are the most, and Radix Glycyrrhizae ratio controls below 30%, and Radix Glycyrrhizae is too much, affects extracting solution color and luster.Owing to Folium Braseniae Schreberi and Tremella water absorption are big, polysaccharide water absorption and swelling formation viscous solution, therefore 40 times of volumes and above extraction, less than this volume extracting solution thickness, it is unfavorable for effective ingredient dissolution and subsequent treatment.Extracting front warm water soaking so that dry powder water absorption and swelling, the especially dissolution of Folium Braseniae Schreberi powder and Tremella powder, beneficially polysaccharide, then homogenate is extracted.
Parameter of noncentricity, extracting solution viscosity is high, and blade could be separated by 6000rpm with clear liquid, need 6000rpm and more than, 10min can reach desired separated effect.
The adsorbable wherein tannin of polyamide, and adsorption effect is better than macroporous resin and zwitterion resin, is investigated by adsorbance, amount of filler: when loading volume is 3:1, reaching preferable adsorption effect, flow velocity 1.0 ml/min, under this flow velocity, can fully adsorb, higher than this flow velocity, detanning matter is insufficient, tannin test positive, and sample fluid viscosity is high, it is extremely difficult to high flow rate.
Effluent is concentrated into 20 times of volumes, viscosity and effective ingredient moderate concentration.
Preferably, in step (2), by weight, Radix Glycyrrhizae powder is 10-30 part, and Tremella powder is 20-60 part, and Folium Braseniae Schreberi powder is 30-60 part.
Further object is that offer utilizes stock solution of the present invention in the application preparing on preparation for external application to skin.Preparation for external application to skin includes facial film, essence, emulsion, emulsifiable paste, gel preparation.
It should be appreciated that owing to the present invention has the most outstanding function, the present invention is applicable to all to be needed moisturizing or anti-oxidation function or removes the preparation for external application to skin of free radical, does not limit to cited by the present invention.
Described facial film includes 20-50% stock solution, 0.05-5% hyaluronic acid, 0.5-5% Jojoba oil by mass percentage;Described emulsion includes 20-50% stock solution, 0.05-5% hyaluronic acid, 0.5-5% Jojoba oil, 1-10% lecithin by mass percentage;Described essence includes 20-50% stock solution, 0.05-5% hyaluronic acid by mass percentage.
Beneficial effects of the present invention:
1, raw material be easy to get, cheap;
2, there is the most outstanding performance of keeping humidity, antioxygenic property and removing free radical performance;
3, preparation technology is simple, without expensive device, low production cost;
4, do not contain organic solvent, pigment tanning, health is not constituted any injury.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of Folium Braseniae Schreberi extracting solution;
Fig. 2 is the performance of keeping humidity design sketch of the present invention;
Fig. 3 is the antioxygenic property design sketch of the present invention.
Detailed description of the invention
The foregoing of the present invention is described in further detail by detailed description of the invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to Examples below.
Embodiment 1
1. the preparation of Folium Braseniae Schreberi powder: choose fresh Folium Braseniae Schreberi 1000g, clear water is clean, and volume is 1000ml, equal pulp grinder 4000rpm, 30min, 60 DEG C of spray drying, obtains Folium Braseniae Schreberi powder, standby.
2 stock solution extracting method:
A Folium Braseniae Schreberi powder 10g, Radix Glycyrrhizae powder 10g, Tremella powder 10g add pure water 1200ml, and 60 DEG C are incubated swelling 1 hour, and homogenate extracts 2 hours.
B is centrifuged (6000rpm, 10min), collects supernatant, and precipitation is extracted again, merges supernatant.
C supernatant crosses polyamide column, deionized water eluting.
D effluent filters, and uses 200 mesh filtered through gauze, then filter paper, 5 micron membrane filter filter, and are concentrated by ultrafiltration to 20 times of dry sample bulking values 600ml, to obtain final product.The stock solution prepared is clear viscous solution, slightly opalescence, and viscosity is high.
Embodiment 2
1. the preparation of Folium Braseniae Schreberi powder: choose fresh Folium Braseniae Schreberi 1000g, clear water is clean, and volume is 1000ml, equal pulp grinder 4000rpm, 30min, 60 DEG C of spray drying, obtains Folium Braseniae Schreberi powder, standby.
2 stock solution extracting method:
A Folium Braseniae Schreberi powder 15g, Radix Glycyrrhizae powder 5g, Tremella powder 10g add pure water 1200ml, and 60 DEG C are incubated swelling 1 hour, and homogenate extracts 2 hours.
B is centrifuged (6000rpm, 10min), collects supernatant, and precipitation is extracted again, merges supernatant.
C supernatant crosses polyamide column, deionized water eluting.
D effluent filters, and uses 200 mesh filtered through gauze, then filter paper, 5 micron membrane filter filter, and are concentrated by ultrafiltration to 20 times of dry sample bulking values 600ml, to obtain final product.The stock solution prepared is clear viscous solution, slightly opalescence, and viscosity is high.
Embodiment 3
1. the preparation of Folium Braseniae Schreberi powder: choose fresh Folium Braseniae Schreberi 1000g, clear water is clean, and volume is 1000ml, equal pulp grinder 4000rpm, 30min, 60 DEG C of spray drying, obtains Folium Braseniae Schreberi powder, standby.
2 stock solution extracting method:
A Folium Braseniae Schreberi powder 20g, Radix Glycyrrhizae powder 10g, Tremella powder 10g add pure water 1600ml, and 60 DEG C are incubated swelling 1 hour, and homogenate extracts 2 hours.
B is centrifuged (6000rpm, 10min), collects supernatant, and precipitation is extracted again, merges supernatant.
C supernatant crosses polyamide column, deionized water eluting.
D effluent filters, and uses 200 mesh filtered through gauze, then filter paper, 5 micron membrane filter filter, and are concentrated by ultrafiltration to 20 times of dry sample bulking values 800ml, to obtain final product.The stock solution prepared is clear viscous solution, slightly opalescence, and viscosity is high.
Embodiment 5
Except Folium Braseniae Schreberi powder used be 90g, Radix Glycyrrhizae powder be 50g and in addition to Tremella powder is 90g, remaining is consistent with embodiment.
Embodiment 6
Except Folium Braseniae Schreberi powder used be 10g, Radix Glycyrrhizae powder be 10g and in addition to Tremella powder is 5 g, remaining is consistent with embodiment.
Embodiment 7
Moisturizing essence makes.
Formula such as table 1.
Table 1
Embodiment 8
Moisturizing emulsion makes.
Formula such as table 2.
Table 2
Embodiment 9
Gel-type making face mask.
Formula such as table 3.
Table 3
Embodiment 10
Folium Braseniae Schreberi powder adds pure water, 20 times of dry weight volumes, heating extraction 2 hours;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Radix Glycyrrhizae powder adds pure water, 20 times of dry weight volumes, heating extraction 2 hours;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Tremella powder adds pure water, 20 times of dry weight volumes, heating extraction 2 hours;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
By Folium Braseniae Schreberi extracting solution 90 parts, Radix Glycyrrhizae extract 50 parts, tremella extract 90 parts mixing.
Embodiment 11
Folium Braseniae Schreberi powder adds pure water, 20 times of dry weight volumes, heating extraction 0.5 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Radix Glycyrrhizae powder adds pure water, 20 times of dry weight volumes, heating extraction 0.5 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Tremella powder adds pure water, 20 times of dry weight volumes, heating extraction 0.5 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
By Folium Braseniae Schreberi extracting solution 10 parts, Radix Glycyrrhizae extract 10 parts, tremella extract 5 parts mixing.
Embodiment 12
Folium Braseniae Schreberi powder adds pure water, 20 times of dry weight volumes, heating extraction 1 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Radix Glycyrrhizae powder adds pure water, 20 times of dry weight volumes, heating extraction 1 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
Tremella powder adds pure water, 20 times of dry weight volumes, heating extraction 1 hour;Centrifugal (6000rpm and more than, 10min), collects supernatant, and precipitation is extracted again, merges supernatant;Supernatant liquid filtering, is concentrated into 20 times of dry sample bulking values, obtains Folium Braseniae Schreberi gel extraction liquid.
By Folium Braseniae Schreberi extracting solution 50 parts, Radix Glycyrrhizae extract 40 parts, tremella extract 20 parts mixing.
Experimental example 1
Folium Braseniae Schreberi extracting solution component analysis (infrared analysis)
500-4000cm-1 infrared scan analysis after embodiment 10-12 gained Folium Braseniae Schreberi extracting solution is processed further, result shows and is mainly composed of polysaccharide: 3432cm-1(O-H), 2919cm-1(C-H), 1627cm-1(-C=O), 1423cm-1 (-C O), 1045cm-1 (C-OH), as shown in Figure of description 1.
Experimental example 2
Embodiment 1-3 gained stock solution is carried out humidity-preserving type mensuration.Stock solution moistening effect of the present invention is best.Hyaluronic acid 0.1% has a certain viscosity, therefore the retentiveness essence lotion minimum compared with viscosity is good, but after 24 hours, Lancome essence lotion moisturizing rate is 12%.
Moisturizing rate calculates, and under RH60% constant humidity, for the practical situation of more preferable simulated skin, selects appropriately sized glass plate to stick 3M micro-porous permeable adhesive tape (1 × 2cm), amount of samples about 0.05g/cm2.Aqueous solution is coated in and posts on 3M adhesive tape, weigh after putting constant humidity exsiccator certain time into, calculate moisturizing rate.
Calculate: moisturizing rate %=(1-(M1-M2)/m) × 100
Moisture weight after M2 mono-placement
M1 mono-places front moisture weight
M mono-coating weight
Experimental example 3
Embodiment 1-3 gained stock solution is carried out non-oxidizability test.Pyrogallol autoxidation in the basic conditions, constantly discharges O2-, O2-Can promote again autoxidation further, after mouse thymus cells 30s, intermedium accumulated concentrations is linear with the time, and the general linear time can maintain 4min, can try to achieve oxidation rate to characterize O2-Understand ability.Clearance rate=(in formula: A0 is the blank absorbency not adding drug solns;Ai is the absorbance of solution after dosing;Aj is the absorbance of sample solution self, and during 9min, pyrogallol oxidation system color products has reached stable, therefore free radical scavenging effect calculates with light absorption value during 9min.)
4 antioxidation experiment packet sample-adding table (n=3) of table
Table 4
Being added by pyrogallol 0.5ml in reaction system, cuvette is poured in shaking immediately into, manual time-keeping simultaneously.Full wavelength scanner 30s, the uv absorption figure of 60s, 90s, 120s, 180s, 320nm goes out absorbance to be increased in time and increases.320nm is selected to go out to measure absorbance.
Group 1 mensuration system autoxidation speed is 0.0036(y=0.0036x+0.2587;R2=0.9910);Group 2 mensuration sample-adding rear oxidation speed 0.0013 (y=0.0013x+0.2318;R2=0.9832);Group 3 is blank;Group 4 mensuration sample self absorbance.Measurement result such as Fig. 3, after stock solution of the present invention (i.e. compound fluid) adds, oxidation rate is decreased obviously, and has stronger Scavenging ability, and free radical scavenging activity is 49.01%.
Experimental example 4
Different Extraction Method gained extracting solution antioxidant activity is evaluated
The antioxidant activity of alkali extracting solution is slightly below Aqueous extracts, mainly containing more impurity in alkali extract, have impact on its antioxidant activity, and color is brown, it is impossible to for cosmetics;Ethanol extract has preferable antioxidant activity equally, but pigment etc. are more, and color is relatively deep, and without moisture retention effect.The oxidation rate of Aqueous extracts is 0.0013(y=0.0013x+0.2183, R2=0.9915), the oxidation rate of alkali extract is 0.0018(y=0.0018x+0.2703, R2=0.9816), alcohol extract oxidation rate is 0.0011(y=0.0011x+0.2874, R2=0.9682).
Experimental example 5
Organic free radical scavenging capacity detects.DPPH existsOrganic solventIn be a kind of stable free radical, its alcoholic solution is purple, and needs low-temperature dark to store, and has a single electronics, thus can accept an electronics orHydrion, under wavelength is 517nm, there is absorption maximum.HaveFree radical scavengerIn the presence of, the single electron of DPPH is captured and makes its lighter, in maximumLight absorbsLight absorption value at wavelength declines, and decline degree inLinear relationship,AbsorbanceThe reduction of level shows the increase of non-oxidizability, thus with the oxidation resistance of evaluation test sample.This oxidation resistance suppression ratio represents, suppression ratio is the biggest, and non-oxidizability is the strongest.
Experiment material: DPPH reagent, extracting solution sample.
Experimental technique:
DPPH preparation of reagents: DPPH (0.2mM) 0.0079g, 50% ethanol SDS 1.5% dissolves, and is settled to 100ml, now with the current.Experimental group: DPPH 2ml, extracting solution 1ml, retarder thinner 2ml, blank group: DPPH 2ml, water 1ml, retarder thinner 2ml, sample sets: extracting solution 1ml, retarder thinner 4ml.
Experimental group measures and adds free radical scavenging effect after stock solution of the present invention, and blank group measures DPPH self absorbance under equal conditions, and sample sets measures sample self absorbance.Measuring the time dependent absorbance A of solution, every 60s value 1 time, when absorbance is basically unchanged, extracting solution is complete with radical reaction, absorbance when record is stablized.After experiment shows to react 1 hour, basicly stable.
Clearance rate=(in formula: A0 is the blank absorbency of non-dosing DPPH solution;After Ai is dosing, the absorbance of DPPH solution;Aj is the absorbance of sample solution self.)
Table 5 organic free radical clearance rate (n=3)
Folium Braseniae Schreberi extracting solution: 20g, 40 times of volumes extract, and are concentrated into 20 times after purification, measure.
Radix Glycyrrhizae extract: 20g, same method processes and obtains.
Compound extract: Folium Braseniae Schreberi 10g, Radix Glycyrrhizae 10g, same method processes and obtains.

Claims (10)

1. a preparation for external application to skin feedstock composition, it is characterised in that described compositions by weight, including:
Folium Braseniae Schreberi powder 10-90 part
Radix Glycyrrhizae 10-50 part
Tremella 5-90 part;
Described Folium Braseniae Schreberi powder is that fresh Folium Braseniae Schreberi is spray-dried gained after homogenized;
Described preparation for external application to skin includes facial film, essence, emulsion, emulsifiable paste, gel preparation.
Compositions the most according to claim 1, it is characterised in that described compositions by weight, including:
Folium Braseniae Schreberi powder 30-60 part
Radix Glycyrrhizae 10-30 part
Tremella 20-60 part;
Described Folium Braseniae Schreberi powder is that fresh Folium Braseniae Schreberi is spray-dried gained after homogenized;
Described preparation for external application to skin includes facial film, essence, emulsion, emulsifiable paste, gel preparation.
Compositions the most according to claim 1 and 2, it is characterized in that, described Folium Braseniae Schreberi powder be fresh Folium Braseniae Schreberi is cleaned after, add the volume pure water less than volume shared by Folium Braseniae Schreberi leaf, utilize refiner to process 30 min under 4000rpm, carry out being spray-dried gained at 60 DEG C.
4. a preparation for external application to skin stock solution, it is characterised in that described stock solution by weight, including:
Folium Braseniae Schreberi extracting solution 10-90 part
Radix Glycyrrhizae extract 10-50 part
Tremella extract 5-90 part;
In described Folium Braseniae Schreberi extracting solution, polyoses content is at least 0.6 mg/ml, and Folium Braseniae Schreberi total polyphenols is at least 1.2 × 10-4mg/ml Without pigment tanning and organic solvent;In described Radix Glycyrrhizae extract, glycyrrhizic acid is at least 2.08 × 10-3mg/ml;In described tremella extract, tremella polysaccharide is at least 2.5 × 10-3mg/ml。
Stock solution the most according to claim 4, it is characterised in that described stock solution by weight, including:
Folium Braseniae Schreberi extracting solution 30-60 part
Radix Glycyrrhizae extract 10-30 part
Tremella extract 20-60 part;
In described Folium Braseniae Schreberi extracting solution, polyoses content is at least 0.6 mg/ml, and Folium Braseniae Schreberi total polyphenols is at least 1.2 × 10-4mg/ml Without pigment tanning and organic solvent;In described Radix Glycyrrhizae extract, glycyrrhizic acid is at least 2.08 × 10-3mg/ml;In described tremella extract, tremella polysaccharide is at least 2.5 × 10-3mg/ml。
6. the preparation method of stock solution as described in claim 4 or 5, it is characterised in that described method comprises the steps:
(1) prepared by Folium Braseniae Schreberi powder: carry out being homogenized being spray-dried by fresh Folium Braseniae Schreberi again, obtains Folium Braseniae Schreberi powder, storage;
(2) with water, Radix Glycyrrhizae powder, Tremella powder, step (1) gained Folium Braseniae Schreberi powder are extracted respectively, obtain Radix Glycyrrhizae extract, tremella extract, Folium Braseniae Schreberi extracting solution respectively;Controlling in Folium Braseniae Schreberi extracting solution, polyoses content is at least 0.6 mg/ml, and Folium Braseniae Schreberi total polyphenols is at least 1.2 × 10-4mg/ml Without pigment tanning and organic solvent;Control glycyrrhizic acid in Radix Glycyrrhizae extract and be at least 2.08 × 10-3mg/ml;Control tremella polysaccharide in tremella extract and be at least 2.5 × 10-3mg/ml;By weight, by Folium Braseniae Schreberi extracting solution 10-90 part, Radix Glycyrrhizae extract 10-50 part, the mixing of tremella extract 5-90 part;
Or, by weight, 5-90 part Radix Glycyrrhizae powder, 10-50 part Tremella powder, the Folium Braseniae Schreberi powder of 10-90 part step (1) gained are added to the water as raw material, the volume addition of water is at least 40 times of volume shared by raw material dry weight, at 60 DEG C, it is incubated 1-2 hour, extracts 0.5-2 hour at a temperature of at least 60 DEG C;
(3) by step (2) gains under at least 6000 rpm, centrifugal 10-30 min, take supernatant;
(4) by step (2) and step (3) described method, step (3) gained precipitate is extracted and separates, take supernatant, and merge with step (3) gained supernatant;
(5) step (4) gains are crossed polyamide column, spend centrifugal water eluting;
(6) step (5) effluent is filtered, be concentrated into 20 times of volume shared by raw material dry weight, to obtain final product.
Method the most according to claim 6, it is characterised in that in step (1), described Folium Braseniae Schreberi powder be by fresh Folium Braseniae Schreberi clean after, add volume and be less than the pure water of volume shared by Folium Braseniae Schreberi leaf, utilize refiner to process 30 min under 4000rpm, carry out being spray-dried gained at 60 DEG C;In step (5), the packing volume of polyamide column is extracting solution 3-4 times, and flow velocity is 1.0 ml/min, the deionization washing post of 1 times of column volume, collects effluent;In step (6), filter method is successively with 200 mesh gauzes, filter paper, 5 μm membrane filtrations;Method for concentration includes rotary evaporation, ultrafiltration, dialysis.
Method the most according to claim 6, it is characterised in that in step (2), by weight, Radix Glycyrrhizae powder is 10-30 part, and Tremella powder is 20-60 part, and Folium Braseniae Schreberi powder is 30-60 part.
9. stock solution described in claim 4 or 5 is in the application prepared on preparation for external application to skin, it is characterised in that described preparation for external application to skin includes facial film, essence, emulsion, emulsifiable paste, gel preparation.
Application the most according to claim 9, it is characterised in that described facial film includes 20-50% stock solution, 0.05-5% hyaluronic acid, 0.5-5% Jojoba oil by mass percentage;Described emulsion includes 20-50% stock solution, 0.05-5% hyaluronic acid, 0.5-5% Jojoba oil, 1-10% lecithin by mass percentage;Described essence includes 20-50% stock solution, 0.05-5% hyaluronic acid by mass percentage.
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CN108014045A (en) * 2017-12-25 2018-05-11 广东芭薇生物科技股份有限公司 A kind of man's skin care compositions and its application
CN110613647A (en) * 2019-10-12 2019-12-27 中南民族大学 Water shield mask liquid and preparation method thereof

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CN104161715A (en) * 2014-06-26 2014-11-26 吴雪琴 Preparing method and product of whitening skincare lotion

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CN102579290A (en) * 2011-01-07 2012-07-18 李庆华 Extraction method for gelatin in water shield
CN104161715A (en) * 2014-06-26 2014-11-26 吴雪琴 Preparing method and product of whitening skincare lotion

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108014045A (en) * 2017-12-25 2018-05-11 广东芭薇生物科技股份有限公司 A kind of man's skin care compositions and its application
CN110613647A (en) * 2019-10-12 2019-12-27 中南民族大学 Water shield mask liquid and preparation method thereof
CN110613647B (en) * 2019-10-12 2022-08-30 中南民族大学 Water shield mask liquid and preparation method thereof

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