CN102198062B - Red sage root mask and preparation method thereof - Google Patents
Red sage root mask and preparation method thereof Download PDFInfo
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Abstract
The invention provides a red sage root mask. The red sage root mask is prepared by adding a mask matrix and water into total salvianolic acid utilized as an active ingredient, wherein, the matrix comprises the following components in parts by weight: 4.9-14.7 parts of the total salvianolic acid, 22.4-67.2 parts of a film-forming material, 7.8-23.4 parts of a thickening agent, 4.9-14.7 parts of a skin penetration enhancer, 0.25-0.75 parts of an antioxidant and 1-3 parts of a preservative. The invention further provides a preparation method of the red sage root mask. The red sage root mask is a peel-off mask, wherein, the total salvianolic acid has an effect on promoting body surface microcirculation, thus smoothening the body surface blood circulation, accelerating the blood flow velocity, fully moisturizing and nourishing skin and hair and ensuring the stability of water-soluble components of red sage root. Therefore, the red sage root mask can be widely used in health and skin care.
Description
Technical field
The present invention relates to a kind of Radix Salviae Miltiorrhizae facial film, belong to medical cosmetic field.
Background technology
Radix Salviae Miltiorrhizae (salvia miltiorrhiza bunge) is birth canal ground, a river medical material; Dry root and rhizome for labiate Radix Salviae Miltiorrhizae (salvia miltiorrhiza bunge); Have stasis-dispelling and pain-killing, promoting blood flow to regulate menstruation, the effect of the relieving restlessness of nourishing blood; " Radix Salviae Miltiorrhizae, book carry and can go into percardium removing blood stasis with potent drugs one language, to the greatest extent the Radix Salviae Miltiorrhizae effect in record in " book on Chinese herbal medicine is looked for the truth ".Opinion is so arranged, and it is can tissue regeneration promoting antiabortive, and the regulating menstruation relieving restlessness is reposed and decided will; And all migratory arthralgia, metrorrhagia and leukorrhagia, lump in the abdomen, conjunctival congestion, colic, scabies disease such as swell and ache, always all go by its stasis of blood, remove invariably to see disease; Non-very can be antiabortive with tissue regeneration promoting, repose and decide will also ", be widely used in the treatment cardiovascular disease at present.
Japan scholar Nakao begins one's study the Radix Salviae Miltiorrhizae chemical constituent so far from the thirties in 20th century, and quite ripe to the research of effective ingredient in the red rooted salvia, Radix Salviae Miltiorrhizae mainly contains fat-soluble and water solublity two effective constituents.Wherein fat-soluble effective ingredient is the tanshinone material, mainly contains tanshinone, Tanshinone I, cryptotanshinone, Tanshinone II B, three hydrogen Tanshinone Is; The fat soluble ingredient of red sage root tanshinone compound has antibiotic significantly, antiinflammatory action; Effect shows as protection endotheliocyte, resisting myocardial ischemia, improves effects such as blood flow and metabolism and protecting myocardial cell to cardiovascular system; Tanshinone compound is because of its significant antimicrobial antiphlogistic effect; Be developed as product for resolving poxes widely, like TANSHINONES facial film etc.Water soluble ingredient is mainly phenolic acid, mainly contains salvianolic acid A (claiming danshensu again), salvianolic acid B, salvianolic acid C, rosmarinic acid, rosmarinic acid first vinegar, protocatechualdehyde, Hesperetic acid etc.Wherein salvianolic acid B content in Radix Salviae Miltiorrhizae is the highest, and effect also clearly, is generally believed it is one of main component of Radix Salviae Miltiorrhizae performance curative effect effect.The effect that red sage root water soluble ingredient has strong anti peroxidation of lipid, removes free radical, antioxidation, antiinflammatory, enhancing immunity, microcirculation improvement obstacle; Be widely used in the Chinese medicine preparation; Principal item has Radix Salviae Miltiorrhizae Injection, FUFANG DANSHEN ZHUSHEYE, DANHONG ZHUSHEYE, pellet to return injection, Radix Salviae Miltiorrhizae Radix Astragali injection etc.; Because red sage root water soluble ingredient has than effects such as strong anti-oxidations, self also is easy to oxidized degeneration, and the chance heat stability is also not so good; The cosmetics that with the red sage root water soluble ingredient are raw material at present are less, carry out to help deep excavation Radix Salviae Miltiorrhizae research ten minutes necessity at cosmetic field.
Summary of the invention
Technical scheme of the present invention has provided a kind of Radix Salviae Miltiorrhizae facial film, and it is to be that Radix Salviae Miltiorrhizae total phenolic acids is the facial film that active component is prepared from red sage root water soluble ingredient.Another technical scheme of the present invention has provided the method for preparing of this Radix Salviae Miltiorrhizae facial film.
The invention provides a kind of Radix Salviae Miltiorrhizae facial film; It is to be active component by Radix Salviae Miltiorrhizae total phenolic acids, adds facial film substrate and water and is prepared from, wherein; Described substrate is: filmogen, thickening agent, skin penetration enhancer, antioxidant and antiseptic, and the weight proportion of active component and substrate is:
Radix Salviae Miltiorrhizae total phenolic acids 4.9-14.7 part, filmogen 22.4-67.2 part, thickening agent 7.8-23.4 part, skin penetration enhancer 4.9-14.7 part, antioxidant 0.25-0.75 part, antiseptic 1-3 part.
Wherein, described filmogen is: the mixing of one or more in PVAC polyvinylalcohol, chitosan or the sodium alginate; Described thickening agent is CMC-Na; Described skin penetration enhancer is a kind of in azone, oleic acid, the propylene glycol; Described antioxidant is a water-soluble vitamin c; Described antiseptic is sodium benzoate, ethyl hydroxybenzoate or sodium sorbate.
Further preferably, described filmogen is PVA-1788; Described skin penetration enhancer is an azone; Described antiseptic is a sodium sorbate.
Wherein, the weight proportion of described active component and substrate is:
9.8 parts of Radix Salviae Miltiorrhizae total phenolic acidss, 44.8 parts of PVA, 15.6 parts of CMC-Na, 58.7 parts of glycerol, 97.8 parts of dehydrated alcohol, 0.5 part of Vc, 9.8 parts of azones, 2.0 parts of sodium sorbates.
Wherein, the method for distilling of described Radix Salviae Miltiorrhizae total phenolic acids is:
Get Danshen Root and add water, warm macerating extracts under 65 ℃ of temperature, concentrates; Concentrated solution treats that its absorption is saturated, water flush away water-solubility impurity with HPD722 resin column on the 2ml/min flow velocity dynamic adsorption; With 20% ethanol is that eluant is with 2ml/min flow velocity eluting; Collect eluent, drying gets Radix Salviae Miltiorrhizae total phenolic acids.
The content that contains salvianolic acid B in the Radix Salviae Miltiorrhizae facial film of the present invention is not less than 1.75mg/g.
The present invention also provides a kind of method for preparing described Radix Salviae Miltiorrhizae facial film, and it comprises the steps:
A, take by weighing the substrate of recipe quantity;
B, get polyvinyl alcohol and add distilled water, swelling is after half an hour, in 95 ℃ of heating in water bath dissolvings;
C, get sodium carboxymethyl cellulose and add distilled water, swelling leaves standstill dissolving after half an hour;
D, the poly-vinyl alcohol solution after will dissolving and carboxymethylcellulose sodium solution mix, and add vitamin C, Radix Salviae Miltiorrhizae total phenolic acids, sodium sorbate successively, stir; Add glycerol, dehydrated alcohol, azone at last, stir, leave standstill, promptly get.
That facial film commonly used mainly comprises is exfoliated, scouring type and powder-type facial film etc., and peel off pack can make skin-tightening, and shrinking pore has the profound pore that cleans, and blood circulation promoting and metabolism are accelerated effects such as drug absorption; It is gentle to clean the profile membrane interaction, be mainly used in rub one's body with a towel, cleaning and skin moistening etc.; The powder-type facial film can not directly use, wipe with before, can according to the state of user skin with can use after hobby selects liquid substance (as: water, astringent, emulsion, fruit juice, astringent etc.) to mix, bother but operation is relative.
Radix Salviae Miltiorrhizae facial film of the present invention is a peel off pack, and Radix Salviae Miltiorrhizae total phenolic acids has the microcirculatory effect of the body surface of promotion, and body surface is freed circulation of the blood, and blood flow is accelerated, and skin and hair are made moist and nutrition fully.Facial film of the present invention has blood circulation promoting and blood stasis dispelling, microcirculation improvement, antioxidation; Effects such as antiinflammatory, it is simple and unadorned to be mainly used in dim complexion, the ecchymosis pigmentation; Skin symptoms such as acne adopt peel off pack can Radix Salviae Miltiorrhizae total phenolic acids component and effect and peel off pack characteristic be combined, and play synergism; And can reach profound effect of cleaning pore, still guarantee the stability of red sage root water soluble ingredient simultaneously, be widely used in the health-care and skin-care aspect.
The specific embodiment
The preparation of embodiment 1 Radix Salviae Miltiorrhizae facial film of the present invention
Get Radix Salviae Miltiorrhizae total phenolic acids (9.8g), PVA (44.8g), CMC-Na (15.6g), glycerol (58.7g);
Dehydrated alcohol (97.8g), Vc (0.5g), azone (9.8g), sodium sorbate (2.0g)
Distilled water (761.0g).
Process 1000g Radix Salviae Miltiorrhizae facial treatment mask.
Method for preparing:
The polyvinyl alcohol that takes by weighing recipe quantity adds 10 times of amount distilled water, and the sodium carboxymethyl cellulose that other takes by weighing recipe quantity adds 20 times of amount distilled water, and swelling makes its dissolving respectively at 95 ℃ of heating in water bath with leaving standstill after half an hour.Poly-vinyl alcohol solution after the dissolving and carboxymethylcellulose sodium solution are mixed, add vitamin C, Radix Salviae Miltiorrhizae total phenolic acids and sodium sorbate successively, stir.Add glycerol, ethanol, azone at last, stir, leave standstill, promptly get.
The preparation of embodiment 2 facial film raw material Radix Salviae Miltiorrhizae total phenolic acidss of the present invention
Instrument: Shimadu LC-20AT type high performance liquid chromatograph (being furnished with the SPD-M20AT detector, LCSolution work station, day island proper Tianjin company); UV, visible light beam split range appearance (day island proper Tianjin); R-201 type Rotary Evaporators (Shanghai Shen Shun Bioisystech Co., Ltd); BP211D electronic balance (German Sartorius company); The DL-360 ultrasonic cleaner; W201 thermostat water bath (Shen, Shanghai is along bio tech ltd), ALPHR1-4LSC freeze drier (CHRIST).
Material: Radix Salviae Miltiorrhizae (originate in Sichuan Zhong Jiang, purchase Chinese crude drug specialized market) in international commerce and trade city; (Chinese pharmaceutical biological product is checked institute, lot number: 111562-200807) to the salvianolic acid B reference substance; NaNO
2(AR); Al (NO
3)
3(AR); NaOH (AR), HPD100 resin (the precious benefactor in Cangzhou department), DA201 resin, HPD722 resin, D101 resin, ethanol (AR).
According to trial test, medical material is beaten powder, it is best to cross a sieve extraction effect, so this experiment is beaten powder with medical material, crosses sieve No. one, subsequent use.
1, method for distilling is preferred
1.1 the design of method for distilling
From salviamiltiorrhizabung, extract Radix Salviae Miltiorrhizae total phenolic acids method for distilling commonly used ultrasonic method, circumfluence method, warm macerating method etc. are arranged; This test is solvent with water; With content of danshinolic acid B, dried cream yield and total phenolic content is evaluation index; Adopt ultrasonic, backflow and warm macerating method to extract the Radix Salviae Miltiorrhizae total phenolic acids extract respectively, investigate relatively three kinds of method for distilling.
Ultrasonic extraction: take by weighing Danshen Root 100g, add 8 times of water gagings, claim to decide weight, supersound extraction 30min filters, and extracts twice, and merging filtrate is subsequent use.
Reflux extraction: take by weighing Danshen Root 100g, add 8 times of water gagings, claim decide weight, reflux, extract, 1.5h is put coldly, claims decide weight again, supplies the weight that subtracts mistake with distilled water, filtration, and extraction twice, merging filtrate, subsequent use.
The warm macerating extraction method: take by weighing Danshen Root 100g, add 8 times of water gagings, claim to decide weight, warm macerating extracts 1.5h (80 ℃), filters, and extracts twice, and merging filtrate is subsequent use.
1.2 the assay method of evaluation index
(1) assay method of content of danshinolic acid B
With reference to " relevant regulations and an appendix VID high effective liquid chromatography for measuring under Radix Salviae Miltiorrhizae item of Chinese pharmacopoeia version in 2010.
1. the selection of chromatographic condition
Chromatographic column: Diamonsil TM (diamond) C
18Post (200 * 4.6mm, 5 μ m); Mobile phase: methanol-acetonitrile-formic acid-water (30: 10: 1: 59); Column temperature: 30 ℃; Flow velocity: 1ml/min; Detect wavelength 286nm.Number of theoretical plate calculates by the salvianolic acid B peak should be not less than 2000.
2. the preparation of reference substance solution
It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and processes the solution that every ml contains 0.147mg, promptly gets.
3. the preparation of need testing solution
The accurate subsequent filtrate 1ml that draws the Radix Salviae Miltiorrhizae extract for preparing under the Different Extraction Method, adding distil water is settled in the volumetric flask of 25ml, filters with 0.45 μ m microporous filter membrane, promptly gets.
4. the preparation of standard curve
Accurate reference substance solution (0.147mg/ml) 10 μ l, 12 μ l, 14 μ l, 16 μ l, 18 μ l, the 20 μ l of drawing inject chromatograph of liquid, and the record peak area returns peak area value (Y) with sample size (X, μ g), obtains linear equation Y=10
6* X-225177, R
2=0.9999, sample size is good in 1.47 μ g～2.94 μ g internal linear relation.
(2) assay method of Radix Salviae Miltiorrhizae total phenolic acids
1. the preparation of reference substance solution
It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adding distil water is processed the solution that every ml contains 0.167mg, draws 0ml respectively, 0.31ml, and 0.63ml, 1.25ml, 2.5ml, the above-mentioned solution of 4ml adds distilled water and is settled to 5ml.The reference substance solution 2ml that draws each concentration respectively places test tube, adds developer (5ml 0.5%NaNO
2, 0.5ml 10%Al (NO
3)
3, 5ml 1mol/L NaOH solution), subsequent use.
2. the preparation of need testing solution
Adopt Different Extraction Method to extract the 100g Danshen Root, the accurate subsequent filtrate 4ml that draws, adding distil water is settled in the volumetric flask of 250ml, pipettes the above-mentioned solution of 2ml to test tube, adds an amount of developer by the reference substance method for preparing, promptly gets.
3. measure the selection of wavelength
Get the salvianolic acid B reference substance solution and place conical flask, add developer (5ml 0.5%NaNO
2Solution, 0.5ml 10%Al (NO
3)
3Solution, 5ml 1mol/L NaOH solution), shake up, adopt full wavelength scanner, obtaining its maximum absorption wavelength is 499nm.
4. the preparation of standard curve
Get the 1. reference substance solution of a following variable concentrations of 2.4.1.2 respectively, measure its absorbance, obtain Radix Salviae Miltiorrhizae total phenolic acids standard curve Y=4.4432X-0.0226, R
2=0.9981, Radix Salviae Miltiorrhizae total phenolic acids concentration linear relationship between 0.0104mg/ml～0.1336mg/ml is good.
(3) assay method of dried cream yield
Precision is measured each extracting solution 25ml, places the evaporating dish that is dried to constant weight, and water-bath volatilizes; Put in the baking oven 105 ℃ and dry to constant weight, in the dislocation exsiccator, cooling; Weigh, according to formula: dried cream yield (%)=dried cream weight (the g)/medical material amount of taking (g) * 100%, calculate dried cream yield.
2 method for distilling are investigated the result
With salvianolic acid B, Radix Salviae Miltiorrhizae total phenolic acids and dried cream yield is evaluation index, adopts method of weighting scores screening optimum extracting method.Total phenolic acid and the more dried cream yield of content of danshinolic acid B are important in the evaluation index; The weight coefficient of formulating salvianolic acid B, Radix Salviae Miltiorrhizae total phenolic acids, dried cream yield is respectively 0.4,0.4,0.2; Comprehensive grading=40 * (total phenolic content the maximum+40 * (content of danshinolic acid B the maximum in content of danshinolic acid B/three kind of the method)+20 in total phenolic content/three kinds method for distilling * (dried cream yield the maximum in the dried cream yield/three kinds method), the result sees table 1.
Table 1 Different Extraction Method is investigated table as a result
Conclusion: warm macerating extraction method extraction ratio is the highest, and energy savings, so adopt the warm macerating method.
The optimization of 3 warm macerating extraction processes
Investigate the result according to the said extracted method, this paper takes the warm macerating method to extract red sage root water soluble ingredient.According to trial test and literature research, extract and can reach good extraction effect twice, put forward technology and get condition for Radix Salviae Miltiorrhizae total phenolic acids extracts worker's the best: 11 times of solvent consumptions (water), 65 ℃ of temperature extract twice, each 130min.
4 Radix Salviae Miltiorrhizae total phenolic acids purifying process
According to documents and materials research, the purification by macroporous resin technology is adopted in the preparation of Radix Salviae Miltiorrhizae total phenolic acids extract more.Advantages such as macroporous resin has that adsorbance is big, desorbing and regeneration are easy have the effect of pharmaceutically active ingredient in the enrichment, are widely used in the separation and purification of Chinese medicine, in this paper studies, its purification condition have been carried out systematic research.
This test is at first investigated resinous type, from aspect screening and optimizing purifying process conditions such as the investigation of the confirming of blade diameter length ratio, the selection of going up an appearance liquor strength, eluant, eluting solvent consumption, absorption flow velocity, dynamic leakage curves.
4.1 the preparation of sample solution
Take by weighing red rooted salvia 50g, add 11 times of water, extract, extract 2 times in 65 ℃ of water-bath warm macerating; Each 130min supplies water absorption rate 320% when adding water for the first time, and merging filtrate is concentrated into 0.2g/ml (to contain the crude drug amount); Hold over night filters, and filtrating is as sample solution.
4.2 the selection of resin kind and model
The macroporous adsorbent resin kind of using at present both at home and abroad is numerous, and the resin of different model is because the difference of its polarity and functional group, and the absorption property of each constituents is also had evident difference.Therefore to concrete separation and purification purpose, at first need select the macroporous adsorbent resin that suits, treat the high selectivity and the high adsorption of separation component to guarantee macroporous adsorbent resin, thereby satisfy the requirement of separation and purification, improve the efficient of separation and purification.
This experiment is an evaluation index with the adsorbance and the resolution factor of salvianolic acid B; Investigated the effect of macroporous resin resin aspect purification Radix Salviae Miltiorrhizae total phenolic acids composition of four kinds of opposed polarities; To confirm the macroporous adsorbent resin type of purification enrichment Radix Salviae Miltiorrhizae total phenolic acids, each model macroporous adsorbent resin performance is seen table 2.
Each model macroporous adsorbent resin performance of table 2
4.2.1 the investigation of resin static adsorption amount
Take by weighing through pretreated 4 kinds of resin 1g (in dried resin) to 150ml tool plug conical flask; Add sample solution 75ml respectively; Leave standstill 24h (per jolting half an hour in preceding 7 hours once), filter, measure the content of Radix Salviae Miltiorrhizae total phenolic acids in the filtrating; Calculate the static adsorption capacity and the adsorption rate of each dried resin, each model macroporous resin absorption capacity is seen table 3.
Each model macroporous resin absorption capacity of table 3
4.2.2 the investigation of resin desorption efficiency
The macroporous adsorbent resin that above-mentioned absorption is saturated, it is colourless that water is washed till water lotion, removes the residual solution of resin surface; Each resin is used 20%, 30%, 50%, 70%, 90% soak with ethanol eluting 2 times respectively successively, each 10mL, soaks 2h, every 1h jolting 1 time at every turn; Collect the eluent of variant concentration of alcohol; Merge, measure the concentration of salvianolic acid B in the eluent, calculate desorption efficiency (%) according to adsorbance.Desorption efficiency=CV/Q, C is the concentration (mg/g) of salvianolic acid B in the filtrating in the formula, and V is the volume (ml) of filtrating, and Q is the adsorbance (mg/g) of resin, sees table 4.
Each model resin resolution factor of table 4
4.2.3 resin preferably reaches the result
Static adsorption amount and resolution factor with salvianolic acid B are evaluation index; Adopt the aggregative weighted point system to investigate; Because of static adsorption amount and resolution factor are important in resin is investigated; So by formula: maximum desorption efficiency * 50 calculates in maximum adsorption rate * 50+ desorption efficiency in comprehensive grading=resin absorption rate/4 kind of resin/4 kinds resin, and the result sees table 5.
Table 5 resin The selection result
Conclusion: resin HPD722 desorption efficiency obviously is superior to other resins, and the static adsorption rate is higher, and comprehensive grading is the highest, so select the HPD722 resin.
The screening of 3 macroporous resin adsorption conditions
3.1 the investigation of blade diameter length ratio
Last appearance column diameter 2cm investigates dress post 8cm respectively, 10cm, the ratio adsorbance of 3 kinds of differing heights HPD722 of 13cm resin.Than adsorbance=(in the sample solution in total phenolic acid amount-raffinate total phenolic acid amount)/resin dry weight.Result such as table 6.
Table 6 blade diameter length ratio is to the influence of resin absorption amount
Conclusion: blade diameter length ratio is 2/13 o'clock, and is more maximum than adsorbance, so adopt blade diameter length ratio 2/13.
3.2 the investigation of last appearance concentration
Take by weighing Danshen Root (crossing sieve No.) 200g, add 11 times of water gagings, extract 2 times each 130min in 65 ℃ of water-baths; Supply water absorption rate 320% when adding water for the first time, merging filtrate is concentrated into 0.2g/ml (to contain the crude drug amount); Leave standstill, filter, thin up becomes concentration to be respectively 0.25g/ml, 0.20g/ml, 3 parts of solution of 0.15g/ml (to contain the crude drug amount); Be the resin of 2/13 HPD722 through blade diameter length ratio, investigate its adsorbance, result such as table 7.
Appearance concentration is to the influence of resin absorption amount on the table 7
Conclusion: when upward appearance concentration was 0.2g/ml (to contain the crude drug amount), adsorbance was maximum.
3.3 the investigation of absorption flow velocity
With the Radix Salviae Miltiorrhizae upper prop liquid of 0.2g/ml (to contain the crude drug amount) respectively with 2ml/min; 3ml/min, the flow velocity of 4ml/min measure the concentration of salvianolic acid B in the effluent through resin column; Calculating is not adsorbed content of danshinolic acid B and is accounted for content of danshinolic acid B ratio in the sample solution, investigates optimum flow rate.The result sees table 8.
The investigation of table 8 absorption flow velocity
Conclusion: when flow velocity was 2ml/min, it was minimum not adsorb content of danshinolic acid B, and not adsorbing content of danshinolic acid B, to account in the sample solution content of danshinolic acid B ratio minimum, so select flow velocity 2ml/min for use.
3.4 the investigation of maximum applied sample amount
With concentration be the Radix Salviae Miltiorrhizae extract of 0.2g/ml (to contain the crude drug amount) with the 2ml/min flow velocity through resin column, every 10ml collects an effluent, measures wherein salvianolic acid B concentration, calculates it and reveals percent.
Radix Salviae Miltiorrhizae total phenolic acids slip (%)=(in the effluent in salvianolic acid B concentration/upper prop liquid salvianolic acid B concentration) * 100%, the result sees table 9.
The maximum applied sample amount of table 9 is investigated the result
Can find out from revealing curve: the 16th part of debris content of danshinolic acid B obviously increases, and salvianolic acid B began to reveal when appearance was described to the 16th part, so confirm that the maximum applied sample amount of Radix Salviae Miltiorrhizae extract is 150ml.
3.5 the selection of eluant
Measuring 7 parts of salvianolic acid B concentration is the medicinal liquid of 0.2g/ml (to contain the crude drug amount), carries out dynamic adsorption through 7 resin columns respectively, earlier with the distillation washing; Remove water-solubility impurity (being mostly saccharide), it is negative to be washed till Molish reaction (chromogenic reaction--the α naphthols strong sulfuric acid response of sugar), uses 10% ethanol more respectively; 20% ethanol, 30% ethanol, 40% ethanol; 50% ethanol, 70% ethanol, each 200ml eluting of 95% ethanol; And press following formula and calculate eluting rate: eluting rate (%)=eluting composition quality/(sample solution composition quality-mistake post effluent composition quality-water elution part composition quality) * 100%, the result sees table 10.
The investigation of table 10 eluant
Conclusion: adopt 20% ethanol elution that salvianolic acid B is had elute effect preferably.
3.6 the investigation of eluant consumption
Measuring 1 part of salvianolic acid B concentration is the medicinal liquid 60ml of 0.2g/ml (to contain the crude drug amount), carries out dynamic adsorption through resin column respectively, earlier with the distillation washing; Remove water-solubility impurity, it is negative to be washed till the molish reaction, uses 20% ethanol with 2ml/min flow velocity eluting more respectively; Every 20min collects once stream part; Measure content of danshinolic acid B in stream part, calculate eluting rate, the result sees table 11.
The investigation of table 11 eluant consumption
Conclusion: when adding the 8th part of eluant, when promptly eluent 20% consumption of ethanol is about 6 times of upper prop liquid, eluting rate is reached more than 90%, elute effect is better.
3.7 confirmatory experiment
The optimal processing parameter of confirming according to above-mentioned experiment makes an experiment, and repeats 3 batches, and calculate purity and yield by following formula: the heavy * 100% of content of danshinolic acid B (g)/dried cream in purity (%)=extract, the result sees table 12.
Table 12 confirmatory experiment result
The result shows that Radix Salviae Miltiorrhizae is behind purification by macroporous resin, and effective ingredient purity significantly improves, and explains that the determined impurity removal process of test is rationally feasible.
4 freeze-dryings prepare Radix Salviae Miltiorrhizae total phenolic acids
To place freezer dryer through the Radix Salviae Miltiorrhizae total phenolic acids extracting solution after extracting purification, lyophilization 36 hours obtains the Radix Salviae Miltiorrhizae total phenolic acids solid extract.
In sum, the optimum extraction process of Radix Salviae Miltiorrhizae total phenolic acids of the present invention is: extract 65 ℃ of temperature, extract twice, each 130min adds 11 times of water gagings.The macroporous resin optimum optimizing condition is: blade diameter length ratio 2/13, last appearance concentration 0.2g/ml (to contain the crude drug amount), absorption flow velocity 2ml/min, maximum applied sample amount 150ml, 6 times of amount 20% ethanol elutions.More than the experimental condition of absorption and parsing all at room temperature carries out.At last purifying process is verified that the result shows that under optimum process condition, the purity of Radix Salviae Miltiorrhizae total phenolic acids improves greatly, impurity content reduces greatly.
Embodiment 3 Radix Salviae Miltiorrhizae facial film mesostroma screening tests of the present invention
The selection of 1 filmogen
1. the selection of filmogen type
Through the document inquiry, in the facial film preparation, polyvinyl alcohol (PVA), chitosan, sodium alginate are used more extensive.Wherein, polyvinyl alcohol is a kind of water-soluble high-molecular compound, and film property, flexibility and hygroscopicity are all good, is one of filmogen of extensive use the most, according to the trial test checking, optimizes polyvinyl alcohol as filmogen simultaneously.
2. the selection of filmogen model
The model that PVA is commonly used has PVA-0588, PVA-1788, PVA-1799 adopts the PVA (comprising powder and granule) of different model to make an experiment in the test, respectively with PVA in 85% alcoholic solution after the alcoholysis 2 times, each 24 hours, filter, dry.Air dried PVA is an amount of after taking by weighing alcoholysis, adds an amount of distilled water immersion after half an hour, and heating makes its dissolving.Investigate its dissolution time, stickiness, filming performance, pliability, uniformity, hands is twisted with the fingers comfort level etc., and the result sees table 13.
The investigation of table 13 different model PVA
Conclusion: the PVA-1788 dissolution time is shorter, is prone to dissolving, and stickiness, film property, pliability, uniformity, that hands is twisted with the fingers comfort level is all better, so this experiment employing PVA-1788 is as filmogen.
3. the investigation of filmogen concentration
The PVA-1788 granule that takes by weighing the alcoholysis after drying respectively is an amount of, is dissolved in the 100ml distilled water, is made into the PVA solution of variable concentrations, investigates its film property, stickiness, and after adding the thickness behind the 5%CMC-Na, see table 14.
The investigation of table 14 variable concentrations PVA
Conclusion: the 10%PVA filming performance is good, and stickiness is moderate, so select for use it as film forming concentration.
The selection of 2 thickening agents
According to literature survey research, be used with PVA, best results person is CMC-Na.CMC-Na is nontoxic, non-stimulated, is the adjuvant that medicine, cosmetic industry are used always.Prove that through trial test CMC-Na can reach uniform thickening effect as thickening agent, so this research adopts it as thickening agent.
Accurate to claim decide CMC-Na an amount of, adds in the 100ml water, leave standstill treat its abundant swelling half an hour after, put heating in water bath, until dissolving fully, be made into the CMC-Na solution of 3%, 5%, 8% concentration, its stickiness and smear ductility and see table 15.
The investigation of table 15CMC-Na concentration
Conclusion: the CMC-Na stickiness of 5% concentration is with to smear ductility all better, so this test employing 5% concentration.
3 punctate opacity of the cornea design-effect surface method optimizations prescription main matrix
In conjunction with the consumption commonly used of main matrix in trial test and the facial film, can screen the use amount ranges that obtains main matrix, so punctate opacity of the cornea design-effect surface method is mainly only adopted in this part experimental study.
3.1 punctate opacity of the cornea design factor and level
Show that according to document and trial test research the principal element that influences membrane presentation quality and film-formation result is PVA
1788With the addition (C) of amount ratio (A), glycerol consumption (B) and the dehydrated alcohol of CMC-Na, so these 3 factors of this EXPERIMENTAL DESIGN high spot reviews, each factor has designed horizontal extent according to trial test, like table 16.
Table 16 influence factor and level
3.2 test method
Take by weighing additives by the punctate opacity of the cornea EXPERIMENTAL DESIGN, press Radix Salviae Miltiorrhizae facial treatment mask preparation technology preparation, make the Radix Salviae Miltiorrhizae facial treatment mask.Test is an index with film formation time and film ocular estimate, and film formation time is for getting 2g substrate, coats equably on the skin of the inboard 3cm * 3cm of human arm and forms the time that can take off thin film, and the film ocular estimate comprises film forming integrity degree, uniformity, demoulding property etc.Result of the test adopts following method evaluation: OD (overall score)=4 * Di (film formation time)+6 * Di (ocular estimate); Wherein film formation time is more little good more in the scope greater than 25min; Acceptable maximum is 45min; Because film formation time is all greater than 25min, film formation time adopts normalization method to handle: Di=(Ymax-Yi)/(Ymax-Ymin); Film ocular estimate score value is the bigger the better, so adopt normalization method to handle: Di=(Yi-Ymin)/(Ymax-Ymin).Test arrangement harmony in the exterior result such as table 17, wherein 15～20
#Equal value representation for the result of each index of repeated trials.
Table 17 punctate opacity of the cornea EXPERIMENTAL DESIGN and result
3.3 model match
Utilize Design expert 7.0 softwares, TOP SCORES (OD) is carried out multiple linear regression and binomial match to amount ratio (A), glycerol consumption (B) and the alcoholic acid addition (C) of CMC-Na respectively, the result is following.
Multiple linear regression fitting result: OD=+1.93245+2.99302 * A+0.054436 * B
-7.88307 * 10
-3* C (P=0.0096, r=0.7951), though can be through the t check, degree of fitting is lower.
(P=0.0028 r=0.9362), can check through t, but degree of fitting is not high enough for nonlinear multivariable fitting result: OD=+17.83295+2.39902 * A-3.57156 * B-0.80538 * C+0.73800 * AB-0.24750 * AC+0.19750 * BC.
Binomial fitting result: OD=+11.66233+6.88699 * A-2.10070 * B-0.77761 * C+0.73800 * AB-0.24750 * AC+0.19750 * BC-1.92342 * A
2-0.13371 * B
2-9.92063 * 10
-4* C
2(P=0.0238, r=0.9618), degree of fitting is higher, but the higher C of P value is removed in P＞0.01
2, obtain fit equation:
OD=+11.98777+6.80970 * A-2.14119 * B-0.80538 * C+0.73800 * AB-0.24750 * AC+0.19750 * BC-1.89030 * A
2-0.13003 * B
2(P=0.0071, r=0.9618), can check through t, and degree of fitting be good P＜0.01, and predictability is good.
3.4 effect surface is drawn
According to fit equation, draw effect surface figure and the circle of equal altitudes of index OD with factors vary.Optimize PVA1788:CMC-Na (1.4～2), glycerol consumption (5%～8%) is good; Optimize PVA1788:CMC-Na (1.4～2), dehydrated alcohol consumption (8%～14%) is good; Optimize glycerol consumption (3%～6%), dehydrated alcohol consumption (8%～11%) or glycerol consumption (6%～8%), dehydrated alcohol consumption (17%～20%) is good.Above-mentioned scope is overlapping; The optimum range of predicting each factor is PVA1788:CMC-Na (1.4～2), glycerol consumption (5.5%～6%), dehydrated alcohol consumption (8%～11%); In conjunction with practical operation and preparation purpose; The final PVA1788:CMC-Na=1.5 that selects, the glycerol consumption is 6%, the dehydrated alcohol consumption is 10% conduct prescription consumption.
Press PVA
1788: CMC-Na=1.5, glycerol consumption are 6%, and the dehydrated alcohol consumption is that 10% composition prepares 3 lot sample article, carries out demonstration test, and checking is the result coincide, and predictability is good.See table 18.
3.5 optimize the prescription checking
Table 18 demonstration test (n=3)
*Be deviation=(predictive value-measured value)/predictive value * 100%
Confirming of 4 drug contents
Press PVA
1788: CMC-Na=1.5, glycerol consumption are 6%, and the dehydrated alcohol consumption is that 10% ratio is prepared 5 parts of blank substrate, adds the Radix Salviae Miltiorrhizae total phenolic acids solids (water-soluble extract of red sage root) of 0.5%, 1%, 2%, 3% different proportion respectively, and observe phenomena is seen table 19.
Table 19 adds dose and investigates
* centrifugal rotational speed is 12000r/min, 10min
Conclusion: 0.5%, 1% adds dose all can reach the effect that keeps facial film stability, but 0.5% to add dose too little, so employing 1% adds dose.
The investigation of 5 other adjuvants
In the investigation of other adjuvants, to calculate for ease, this EXPERIMENTAL DESIGN is reference with the total amount of the main matrix (comprising PVA, CMC-Na, dehydrated alcohol and glycerol) in the prescription, measuring with this is the amount that basic calculation adds other adjuvant.
5.1 the investigation of skin penetration enhancer
Medicine is brought into play curative effect through the absorption of skin or mucosa, often adds penetration enhancer to promote the absorption of effective ingredient, and Percutaneous absorption enhancer commonly used has azone, oleic acid, propylene glycol etc.Wherein azone, nonirritant nontoxic because of it, characteristic that transdermal enhancing effect is strong are the most commonly used, and color and luster became milky after this test added azone, and is more even, and do not have bubble, so consider that the employing azone is as the skin penetration enhancer.Investigate and add the various dose azone: 0.1%, 0.5%, 1%, 2%, 3%.Oil droplet appearance material surface appears in the sample that adds 2%, 3% azone, and unstable, azone is 1%～3% as the penetration enhancer common dose, so adopt 1% azone as the skin penetration enhancer.
5.2 the investigation of antioxidant
The Radix Salviae Miltiorrhizae total phenolic acids composition is prone to oxidation deterioration, so need to add antioxidant.Support one's family usually as antioxidant, water-soluble vitamin c is adopted in this test, can reach good antioxidant effect.Investigate vitamin C (Vc) addition: 0.01%, 0.05%, 0.1%, 0.2%.Observe phenomena is seen table 20.
Table 20Vc addition is investigated
Conclusion: after adding 0.05%Vc, the color sample no change, and not thinning, antioxidant effect is better.
5.3 choice of preservatives
Ethanol content is lower than 20% in the Radix Salviae Miltiorrhizae facial treatment mask, does not have antiseptic effect, so in the Radix Salviae Miltiorrhizae facial treatment mask, often add antiseptic to suppress antibacterial and fungus growth.Sodium benzoate, ethyl hydroxybenzoate, sodium sorbate are the most frequently used antiseptic, but this sample contains tween, and tween is prone to influence antiseptic effect with ethyl hydroxybenzoate generation complexation, and sodium sorbate strengthens under the tween effect, so adopt sodium sorbate as antiseptic.Antiseptic effect behind the sodium sorbate of investigation adding 0.1%, 0.2%, 0.3% various dose.Sample was placed after 1 month, and going mouldy appears in the sample that adds 0.1% sodium sorbate, and going mouldy all appears in the sodium sorbate that adds 0.2% and 0.3% dosage, so employing 0.2% consumption.
5.4 final preparation prescription
Radix Salviae Miltiorrhizae total phenolic acids (9.8g), PVA (44.8g), CMC-Na (15.6g), glycerol (58.7g);
Dehydrated alcohol (97.8g), Vc (0.5g), azone (9.8g), sodium sorbate (2.0g)
Distilled water (761.0g).
Process 1000g Radix Salviae Miltiorrhizae facial treatment mask.
Embodiment 4 Radix Salviae Miltiorrhizae facial treatment mask release in vitro degree are investigated
1 release in vitro degree evaluation methodology
The external release situation of Franz diffusion cell method research medicine is adopted in this test, is divided into two parts: supply chamber and receiving chamber, effectively diffusion area is 3.14cm
2, the reception tank volume is 14ml.In receiving chamber, add electromagnetic agitation (long 0.9cm
2, wide 0.4cm
2) and the 14ml normal saline, and in time discharge bubble, the 25mm CAM is fixed between the diffuser casing receiving chamber; Place on the constant temperature blender with magnetic force of 35 ℃～37 ℃ of bath temperatures, 300rpm; Behind 40min, take a sample, measure salvianolic acid B concentration, unit of account area transit dose with the HPLC method.
Chromatographic column: Diamonsil TM (diamond) C
18Post (200*4.6mm, 5 μ m); Mobile phase: methanol-acetonitrile-phosphoric acid-water (30: 10: 1: 59); Flow velocity 1.0ml/min; Detect wavelength: 286nm, 30 ℃ of column temperatures; Theoretical cam curve is calculated by the salvianolic acid B peak should be not less than 2000.
The preparation of 2 standard curves
It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and processes the solution that every 1ml contains 0.146mg, promptly gets the salvianolic acid B reference substance solution.By above-mentioned chromatographic condition, difference auto injection 3 μ l, 5 μ l, 7 μ l; 9 μ l, 11 μ l, the record peak area is an abscissa with salvianolic acid B sample size X (μ g); Peak area Y (A) is a vertical coordinate, the line linearity recurrence of going forward side by side of mapping, and obtaining regression equation is y=370875x-197690, R
2=0.9999, the result shows that the sample size of salvianolic acid B is good in 0.146 μ g～1.606 μ g scope internal linear relation.
The test of 3 precision
The accurate 10 μ l salvianolic acid B reference substance solution of drawing, continuous sample introduction 6 times, the record peak area, the result sees table 21.
Table 21 precision is investigated the result
Conclusion: RSD＜2%, it is good to show that sample introduction and chromatograph detect precision.
4 study on the stability
Draw the sample in the diffusion cell reception tank, after filtering with 0.45 μ m microporous filter membrane, respectively at 0h, 1h, 2h, 4h, 6h, sample introduction is measured behind the 8h, record salvianolic acid B peak area, the result sees table 22.
Table 22 study on the stability table
Conclusion: RSD＜3% shows that sample is stable in 8h.
5 average recoveries are investigated
Get 6 parts of the about 0.5g of Radix Salviae Miltiorrhizae facial treatment mask (content of danshinolic acid B 0.189%) of known content, accurately claim surely, the accurate respectively salvianolic acid B reference substance 6ml that adds 0.146mg/ml adds 75% methanol to 25ml, extracts in ultrasonic 30 minutes, filters, and surveys its content of danshinolic acid B.Result such as table 23.
Table 23 application of sample reclaims measures table (n=6) as a result
Conclusion: average recovery between 95%～105%, average recovery rate 98.8%, the RSD value is 1.35%, meets the requirement of assay.
6 release in vitro degree results
Parallel preparation three duplicate samples are measured the concentration in the diffusion cell behind the 40min, calculate unit are salvianolic acid B transit dose behind the 40min, try to achieve meansigma methods, and the result sees table 24.
Table 24 release in vitro degree is investigated the result
7 brief summaries
The present invention at first adopts single factor method to filter out main filmogen kind, filmogen concentration, thickening agent, filters out to adopt 10%PVA-1788 and 5%CMC-Na, and film-formation result is best, and film suppleness, demoulding property are good; Adopting punctate opacity of the cornea design-effect surface method then is the addition (C) of amount ratio (A), glycerol consumption (B) and the dehydrated alcohol of evaluation index screening main matrix adjuvant PVA1788 and CMC-Na with film presentation quality and film-formation result, and optimize optimal parameter: PVA1788:CMC-Na=1.5, glycerol are 6%; Ethanol is 10%, filter out the prescription main matrix after, investigate through single factor and to filter out other additives; Confirmed preparation prescription: Radix Salviae Miltiorrhizae total phenolic acids (9.8g), PVA (44.8g), CMC-Na (15.6g); Glycerol (58.7g), dehydrated alcohol (97.8g), Vc (0.5g); Azone (9.8g), sodium sorbate (2.0g), distilled water (761.0g); At last this facial film is carried out the evaluation of release in vitro degree, the release in vitro degree is good.
The quality control of embodiment 5 facial films of the present invention
The Radix Salviae Miltiorrhizae facial treatment mask is processed by the salviamiltiorrhizabung water solubility extract; Have effects such as strong microcirculation improvement obstacle, anti peroxidation of lipid, removing free radical, antioxidation, antiinflammatory, enhancing immunity; Salvianolic acid B is one of its main effective ingredient; In conjunction with literature research, select the index components of salvianolic acid B as this quality of control.
1 chromatographic condition
Chromatographic column: Diamonsil TM (diamond) C
18Post (200*4.6mm, 5 μ m); Mobile phase: methanol-acetonitrile-phosphoric acid-water (30: 10: 1: 59); Flow velocity 1.0ml/min; Detect wavelength: 286nm, 30 ℃ of column temperatures; Theoretical cam curve is calculated by the salvianolic acid B peak should be not less than 2000.
The preparation of 2 reference substance solution
It is an amount of to get the salvianolic acid B reference substance, and accurate the title decides, and adds 75% methanol and processes the solution that every 1ml contains 0.146mg, promptly gets the salvianolic acid B reference substance solution.
The preparation of 3 need testing solutions
Sample thief 1g, the accurate title, decide, and adds 75% methanol solution and be settled to 25ml, and supersound process 30 minutes filters, and filters with 0.45 μ m microporous filter membrane, promptly gets.
4 specificities are investigated
Get the not sample 1g of pastille, the accurate title, decide, and adds 75% methanol solution and be settled to 25ml, and supersound process 30 minutes filters, and filters sample introduction with 0.45 μ m microporous filter membrane.The result shows, and is negative noiseless.
The preparation of 5 standard curves
By above-mentioned chromatographic condition, difference auto injection 3 μ l, 5 μ l, 7 μ l; 9 μ l, 11 μ l, the record peak area is an abscissa with salvianolic acid B sample size X (μ g); Peak area Y (A) is a vertical coordinate, the line linearity recurrence of going forward side by side of mapping, and obtaining regression equation is y=370875x-197690, R
2=0.9999, the result shows that the sample size of salvianolic acid B is good in 0.146 μ g～1.606 μ g scope internal linear relation.
The test of 6 precision
The accurate 10 μ l salvianolic acid B reference substance solution of drawing, continuous sample introduction 6 times, the record peak area, the result sees table 25.
Table 25 precision is investigated the result
Conclusion: RSD＜2%, it is good to show that sample introduction and chromatograph detect precision.
7 study on the stability
With the sample after the filtration of 0.45 μ m microporous filter membrane, respectively at 0h, 1h, 2h, 4h, 6h, sample introduction is measured behind the 8h, record salvianolic acid B peak area, the result sees table 26.
Table 26 study on the stability table
8 average recoveries are investigated
Get 6 parts of the about 0.5g of Radix Salviae Miltiorrhizae facial treatment mask (content of danshinolic acid B 0.189%) of known content, accurate claim fixed, the accurate respectively salvianolic acid B reference substance solution 6ml that adds 0.146mg/ml; Add 75% methanol to 25ml; Supersound process was extracted in 30 minutes, filtered, and surveyed its content of danshinolic acid B.The result sees table 27.
Table 27 application of sample reclaims measures table (n=6) as a result
Conclusion: average recovery between 95%～105%, average recovery rate 98.8%, the RSD value is 1.35%, meets the requirement of assay.
9 sample determinations
Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing measure according to above-mentioned chromatographic condition, measure the result and see table 28.
Table 28 ten lot sample article assays are table as a result
Conclusion: the salvianolic acid B average content is 2.18mg/g, takes all factors into consideration various factors, and tentative these article content of danshinolic acid B is not less than about 80% of average content, promptly is not less than 1.75mg/g.
The preliminarily stabilised Journal of Sex Research of the Radix Salviae Miltiorrhizae facial treatment mask of embodiment 6 facial films of the present invention
With reference to " two appendix XIXC of Chinese pharmacopoeia version in 2010 medicine stability test guideline is carried out the investigation of preliminarily stabilised property to three lot sample article 100801,100802,100803.
1 test apparatus, material
Instrument: PH analyzer, Shimadu LC-20AT type high performance liquid chromatograph (being furnished with the SPD-M20AT detector, LC Solution work station, day island proper Tianjin company); The Germany Sartorius BP211D of company electronic balance; The DL-360 ultrasonic cleaner; Refrigerator, climatic chamber.
Material: 3 batches of laboratory amplification quantity production samples; The salvianolic acid B reference substance.
2 investigation project and methods
According to Radix Salviae Miltiorrhizae facial treatment mask dosage form is liniment; To the more responsive characteristics of temperature; With reference to " related request under 2010 editions two appendix XI XC of the Chinese pharmacopoeia item; The Radix Salviae Miltiorrhizae facial treatment mask has been carried out the inspection of projects such as appearance character, lamination, assay, film property, microorganism, and the result sees table 29,30.
3 long term tests are investigated
With reference to " related request under two appendix XI of Chinese pharmacopoeia version in 2010 XC item carries out long-term stable experiment to the Radix Salviae Miltiorrhizae facial treatment mask and investigates.
Three batches of Radix Salviae Miltiorrhizae facial treatment mask samples getting plastic bottle packing place 6 ℃ ± 2 ℃ of temperature respectively, humidity 60% ± 10% time, regularly 0,1,2, March sampling and measuring, the result sees table 29.
The ambient stable property investigation result of table 29 three lot sample article
4 accelerated tests are investigated
Get three batches of Radix Salviae Miltiorrhizae facial treatment mask samples of plastic bottle packing, respectively at 25 ℃ ± 2 ℃, humidity 60% ± 10% held, regularly 0,1,2, March sampling and measuring, the result sees table 30.
The accelerated stability test result of table 30 three lot sample article
Conclusion: Radix Salviae Miltiorrhizae facial treatment mask sample, is placed after 3 months under humidity 60% ± 10% condition at 25 ℃ ± 2 ℃, and sample is stable at aspects such as outward appearance, lamination, content, film property, meets the requirements.
5 brief summaries
Through investigating 3 months the long term test and the preliminarily stabilised property of accelerated test discussion Radix Salviae Miltiorrhizae facial treatment mask; The result shows check results and initial phase ratio such as appearance character, lamination, related substance and content, the film property of facial film; No significant change, limit test of microbe is qualified.
And the inventor is through carrying out the test of test of acute skin irritation property and eye irritation to rabbit, the result shows skin and the equal nonirritant of eyes.
In sum, Radix Salviae Miltiorrhizae facial film of the present invention is a peel off pack, and is safe in utilization, stable, can be widely used in health-care and skin-care.
Claims (2)
1. Radix Salviae Miltiorrhizae facial film; It is characterized in that: it is to be active component by Radix Salviae Miltiorrhizae total phenolic acids, adds facial film substrate and water and is prepared from, wherein; Described substrate is: filmogen, thickening agent, skin penetration enhancer, antioxidant and antiseptic, and the weight proportion of active component and substrate is:
Radix Salviae Miltiorrhizae total phenolic acids 4.9-14.7 part, filmogen 22.4-67.2 part, thickening agent 7.8-23.4 part, skin penetration enhancer 4.9-14.7 part, antioxidant 0.25-0.75 part, antiseptic 1-3 part;
Wherein, described filmogen is: the mixing of one or more in PVAC polyvinylalcohol, chitosan or the sodium alginate; Described thickening agent is CMC-Na; Described skin penetration enhancer is a kind of in azone, oleic acid, the propylene glycol; Described antioxidant is a water-soluble vitamin c; Described antiseptic is sodium benzoate, ethyl hydroxybenzoate or sodium sorbate;
The method for distilling of described Radix Salviae Miltiorrhizae total phenolic acids is:
Get Danshen Root and add water, warm macerating extracts under 65 ℃ of temperature, concentrates; Concentrated solution treats that its absorption is saturated, water flush away water-solubility impurity with HPD722 resin column on the 2ml/min flow velocity dynamic adsorption; With 20% ethanol is that eluant is with 2ml/min flow velocity eluting; Collect eluent, drying gets Radix Salviae Miltiorrhizae total phenolic acids.
2. Radix Salviae Miltiorrhizae facial film according to claim 1 is characterized in that: described filmogen is PVA-1788; Described skin penetration enhancer is an azone; Described antiseptic is a sodium sorbate.
3. Radix Salviae Miltiorrhizae facial film, it is characterized in that: the weight proportion of described active component and substrate is:
9.8 parts of Radix Salviae Miltiorrhizae total phenolic acidss, 44.8 parts of PVA, 15.6 parts of CMC-Na, 58.7 parts of glycerol, 97.8 parts of dehydrated alcohol, 0.5 part of Vc, 9.8 parts of azones, 2.0 parts of sodium sorbates;
The method for distilling of described Radix Salviae Miltiorrhizae total phenolic acids is:
Get Danshen Root and add water, warm macerating extracts under 65 ℃ of temperature, concentrates; Concentrated solution treats that its absorption is saturated, water flush away water-solubility impurity with HPD722 resin column on the 2ml/min flow velocity dynamic adsorption; With 20% ethanol is that eluant is with 2ml/min flow velocity eluting; Collect eluent, drying gets Radix Salviae Miltiorrhizae total phenolic acids.
4, according to any described Radix Salviae Miltiorrhizae facial film of claim 1-3, it is characterized in that: the content that contains salvianolic acid B in the Radix Salviae Miltiorrhizae facial film is not less than 1.75mg/g.
5, a kind of method for preparing the described Radix Salviae Miltiorrhizae facial film of claim 3, it comprises the steps:
A, take by weighing the substrate of recipe quantity;
B, get polyvinyl alcohol and add distilled water, swelling is after half an hour, in 95 ℃ of heating in water bath dissolvings;
C, get sodium carboxymethyl cellulose and add distilled water, swelling leaves standstill dissolving after half an hour;
D, the poly-vinyl alcohol solution after will dissolving and carboxymethylcellulose sodium solution mix, and add vitamin C, Radix Salviae Miltiorrhizae total phenolic acids, sodium sorbate successively, stir; Add glycerol, dehydrated alcohol, azone at last, stir, leave standstill, promptly get.
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| CN101756817A (en) * | 2008-12-22 | 2010-06-30 | 天津天阜康生物技术发展有限公司 | Traditional Chinese medicine whitening mask |
| CN101843572A (en) * | 2010-06-11 | 2010-09-29 | 成佩秀 | Skin-care anti-wrinkle face mask |
| CN101919793A (en) * | 2009-06-15 | 2010-12-22 | 李小兵 | Chinese herbal medicine mask capable of removing acne and whitening |
-
2011
- 2011-05-26 CN CN201110139220A patent/CN102198062B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101756817A (en) * | 2008-12-22 | 2010-06-30 | 天津天阜康生物技术发展有限公司 | Traditional Chinese medicine whitening mask |
| CN101919793A (en) * | 2009-06-15 | 2010-12-22 | 李小兵 | Chinese herbal medicine mask capable of removing acne and whitening |
| CN101843572A (en) * | 2010-06-11 | 2010-09-29 | 成佩秀 | Skin-care anti-wrinkle face mask |
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