CN101606988B - Anti-loss and hair-growing preparation of six ingredients, preparation method and quality testing method thereof - Google Patents
Anti-loss and hair-growing preparation of six ingredients, preparation method and quality testing method thereof Download PDFInfo
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Abstract
The invention discloses an anti-loss and hair-growing preparation of six ingredients, a preparation method and a quality testing method thereof. The preparation is prepared by the following ingredients by weight parts: 25 to 35 parts of rhubarb, 15 to 25 parts of radix sophorae flavescentis, 10 to 20 parts of polygonum multiflorum, 10 to 20 parts of angelica sinensis, 10 to 20 parts of astragalus mongholicus and 3 to 7 parts of mint. The anti-loss and hair-growing preparation of six ingredients has the efficacies of removing dandruff and relieving itching, preventing hair loss and growing hair, and blackening hair and protecting hair. According clinical verification, the total effectiveness of the preparation is 96 percent; and the preparation functions both in prevention and treatment, is safe and non-toxic, and is an ideal pure traditional Chinese medicine for treating seborrheic alopecia. The quality testing method has strong specificity, high precision, good stability and accurate testing result, and can effectively control the quality of the anti-loss and hair-growing preparation of six ingredients, thus ensuring the clinical efficacy thereof.
Description
Technical field:
The present invention relates to a kind of Six-element phalacrosis prevention and hair generation preparation and preparation method thereof and quality determining method, belong to technical field of traditional Chinese medicine pharmacy.
Background technology:
Alopecia is a global problem.There are 8,000 ten thousand people to suffer from alopecia in the U.S.; There are 2,000 ten thousand people in Japan; The European 26% in 20-39 year suffers from alopecia, surpasses 50% more than 40 years old.The situation of China also allows of no optimist: a investigation to 5779 men in 5 cities such as Beijing, Shanghai, Guangzhou, Hangzhou shows: China's male pattern baldness sickness rate reaches 25%.Calculate with 6.72 hundred million male, China male pattern baldness patient has reached about 1.68 hundred million people.And the questionnaire survey of a " doctor advertises for alopecia personage suggestion sincerely " by name also shows, male pattern baldness is " rejuvenation " obviously, and 60% patient just began alopecia before 25 years old, and the ratio of alopecia is unexpectedly up to 83.9% before 30 years old.
The product of treating alopecia and renewable hair in the market emerges in an endless stream, and the shampoo form is arranged, and drug form is also arranged, and also have massage appliance etc., but situation about using according to reality shows that its therapeutic effect is unsatisfactory, and the life cycle that has is long, take effect slowly; The treatment that has is not thorough; The medical expense that has is expensive; The use inconvenience that has etc.For example use more ZHANGGUANG 101 on the market, though effect is better relatively, its expense is somewhat expensive, and need under professional's guidance, use.
For alopecia, still lack comparatively ideal therapy at present.The method that modern medicine is commonly used has the local topical minoxidil, and the solid ferment of intradermal injection cortex class uses contact sensitizing agent such as dinitrochlorobenzene, photochemotherapy, estrogen therapy etc., though these methods have certain curative effect, untoward reaction is in various degree arranged all.The disease that with the alopecia is cardinal symptom in recent years is increasingly extensive.Mostly its etiology and pathogenesis of this type of disease is the hepatic and renal YIN deficiency, blood-deficiency and wind-dry, sending out becomes homeless support due to.
Summary of the invention:
The objective of the invention is to: a kind of Six-element phalacrosis prevention and hair generation preparation and preparation method thereof and quality determining method are provided.The present invention forms so that Six-element natural Chinese medicinal herb prescription is refining, has the effect of removing scurf and relieving itching, phalacrosis prevention and hair generation, black hair hair care, and control takes into account, and safety non-toxic is the ideal pure Chinese medicinal preparation of treatment seborrheic alopecia.
The present invention constitutes like this: a kind of Six-element phalacrosis prevention and hair generation preparation, according to listed as parts by weight, it is processed for 3～7 parts with 25～35 parts of Radix Et Rhizoma Rhei, 15～25 parts of Radix Sophorae Flavescentiss, 10～20 parts of Radix Polygoni Multiflori, 10～20 parts of Radix Angelicae Sinensis, 10～20 parts of the Radixs Astragali, Herba Menthae.
As preferably, according to listed as parts by weight, it is processed for 5 parts with 30 parts of Radix Et Rhizoma Rhei, 20 parts of Radix Sophorae Flavescentiss, 15 parts of Radix Polygoni Multiflori, 15 parts of Radix Angelicae Sinensis, 15 parts of the Radixs Astragali and Herba Menthae.
Described preparation is tincture, gel, ointment or liniment.
The method for preparing of Six-element phalacrosis prevention and hair generation preparation according to the invention is: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder, mixing; According to the percolation under fluid extract and the extractum item, make solvent with 55% ethanol, flood after 24 hours; With the speed of per minute 2～3ml percolation slowly; Collect percolate, activated carbon adsorption, filtration, fill are processed tincture or are added appropriate amount of auxiliary materials and process other preparation.
The method for preparing of Six-element phalacrosis prevention and hair generation gel is: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder, mixing is according to the percolation under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours, with the speed of per minute 2～3ml percolation slowly; Collect percolate, activated carbon adsorption is concentrated into 10～20 weight portions; Add gel substrate 900～990 weight portions, stir, promptly get.
Calculate by weight, described gel substrate is made up of for 50～120 parts Acritamer 940 or 9711～4 parts, 2～10 parts of glycerol, 1～3 part of Macrogol 4000,5～40 parts of dehydrated alcohol, 1～5 part of triethanolamine and water.Its method for making is: get Acritamer 940 and add an amount of distilled water and in mortar, grind evenly, drip triethanolamine and regulate and make gel, add Macrogol 4000, glycerol, dehydrated alcohol more successively, grind well and promptly get gel substrate.
The method for preparing of Six-element phalacrosis prevention and hair generation ointment is: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder, mixing is according to the percolation under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours, with the speed of per minute 2～3ml percolation slowly; Collect percolate, activated carbon adsorption is concentrated into 10～20 weight portions; Adding is chilled to ointment base 900～990 weight portions after the room temperature, grinds mixing, promptly gets.
Calculate by weight, described ointment base is made up of for 5～35 parts 1～5 part of sodium carboxymethyl cellulose, 1～3 part of glycerol, 0.01～0.08 part of ethyl hydroxybenzoate and water.Its method for making is: get Carboxymethyl cellulose sodium and place mortar, add glycerol and grind well, add 8～15 parts of entry and make dissolving fully; Add the aqueous solution that is dissolved with ethyl hydroxybenzoate then while grinding, grind evenly, promptly get ointment base.
Calculate by weight, described ointment base also can be made up of for 3～13 parts 10～18 parts of stearic acid, 3～6 parts of glyceryl monostearates, 18～30 parts of Oleum Ricini, 8～17 parts of glycerol, 1～3 part of triethanolamine, 0.08～0.4 part of ethylparaben and water.Its method for making is: get stearic acid, glyceryl monostearate, Oleum Ricini and ethylparaben and melt 50～60 ℃ of heated and stirred; Get oil phase substrate, in addition glycerol, triethanolamine, water are melted 50～60 ℃ of heated and stirred, get aqueous phase substrate; Slowly add oil phase substrate in the aqueous phase substrate; And constantly stir, mixing promptly gets ointment base.
The method for preparing of Six-element phalacrosis prevention and hair generation liniment is: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder, mixing is according to the percolation under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours,, collect percolate with the speed of per minute 2～3ml percolation slowly; Activated carbon adsorption is concentrated into 10～20 weight portions, adds entry or glycerol or ethanol or vegetable oil 900～990 weight portions; Mixing filters, and promptly gets.
The quality determining method of Six-element phalacrosis prevention and hair generation preparation according to the invention comprises to be differentiated and assay, wherein differentiates the thin layer chromatography discriminating that comprises Radix Et Rhizoma Rhei in the preparation and Radix Sophorae Flavescentis; Assay be with in the high effective liquid chromatography for measuring preparation 2,3,5,4 '-content of tetrahydroxystilbene-2-0-β-D-glucoside.
The discrimination method of Radix Et Rhizoma Rhei is to be contrast with Radix Et Rhizoma Rhei control medicinal material and chrysophanic acid reference substance, and with normal hexane: ethyl acetate: formic acid=30: 10: 0.5 is the thin layer chromatography of developing solvent; The discrimination method of Radix Sophorae Flavescentis is to be contrast with the matrine reference substance, and with chloroform: methanol: strong ammonia solution=20: 2.4: 0.8,10 ℃ of lower floor's solution with held are the thin layer chromatography of developing solvent.
2,3,5,4 '-content assaying method of tetrahydroxystilbene-2-0-β-D-glucoside is with 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside reference substance is contrast, with acetonitrile: water=23: 77 is the HPLC of mobile phase.
Described quality determining method comprises:
Differentiate: this preparation 20ml is got in (1), flings to ethanol in the water-bath, adds diethyl ether to extract 2 times, and each 15ml merges ether solution, is concentrated into 1ml as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.2g, and the 10ml jolting that adds diethyl ether was extracted 20 minutes, filters, and filtrating is waved to about 1ml, as control medicinal material solution; Get the chrysophanic acid reference substance again, add diethyl ether and process the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel H lamellae; With normal hexane: ethyl acetate: formic acid=30: 10: 0.5 is developing solvent, launches, and takes out; Dry, put under the 365nm uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; With reference substance chromatograph relevant position on, show a speckle of same color; Put in the ammonia steam smoked after, speckle becomes redness;
(2) get this preparation 20ml, volatilize in the water-bath, add the dissolving of 25ml chloroform and 0.3ml strong ammonia solution, filter, filtrating is waved to 1ml, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With chloroform: methanol: strong ammonia solution=20: 2.4: 0.8,10 ℃ of lower floor's solution with held are developing solvent; Put in the expansion cylinder of ammonia saturated with vapor, launch, take out; Dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay: chromatographic condition and system suitability experiment use 18 alkyl silica gel to be filler; Acetonitrile: water=23: 77 is mobile phase; Column temperature: 40 ℃; The detection wavelength is 320nm; Theoretical cam curve by 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside peak calculates and should be not less than 2000;
The preparation of reference substance solution gets 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside reference substance is an amount of, and accurate the title, decide, and uses 50% dissolve with ethanol, processes the solution that every 1ml contains 0.1mg approximately, shakes up, and promptly gets;
The preparation precision of need testing solution is measured this preparation 5ml, puts in the 50ml measuring bottle, adds 50% ethanol 30ml, close plug, and supersound extraction 10 minutes, taking-up is put and is chilled to room temperature,, shakes up to scale with 50% ethanol dilution, promptly gets;
Accurate each the 10 μ l of above-mentioned three kinds of solution that draw of algoscopy inject chromatograph of liquid, measure, and promptly get;
The every 1ml of this preparation contains 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) must not be less than 0.12mg.
The traditional Chinese medical science thinks that alopecia often by youth's people, contains in the heat in blood, and multiple irritated by mind, seven emotions are unsuccessful, and strongly fragrant fire-transformation of a specified duration accumulates in burning hot, intense heat bringing about wind syndrome, " pneumatic leaf falls ", hair is alopecia therefore.So teenager is suffered from primary disease, is mostly due to the interior-heat that its treatment also should be with clearing away heat and cooling blood, the agent of the hair growth promoting of dispeling the wind.Can't absurd clothes tonic.Otherwise benefit is hot more more, and Re Zefa falls more more.The spirit emotion changes is one of major reason of primary disease, and Chinese and western medicine is consistent on this aspect.As long as keep the stable of emotion in daily life as far as possible, competent sleep can prevent the alopecia that causes because of direct stimulation, overfatigue at least.The traditional Chinese medical science early has understanding to alopecia, and blood stored in the liver, hair is the sign of blood condition are arranged, kidney governing bones, its flourish reason with suffer from a deficiency of the kidney, blood deficiency is relevant.In recent years and the blood stasis theory is arranged, thus the treatment of bald generally method with the kidney invigorating, to nourish blood, invigorate blood circulation be main.Deficiency of spleen-QI type, deficiency of the liver and kindey type, stagnation of liver-QI blood stasis type, QIXUELIANGXU type are roughly had the inclination by its traditional Chinese medical science branch.Side's opinions such as the patient can dialectically be enriched blood to nourish blood by the doctor, nourishing the liver and kidney, invigorating the spleen and benefiting QI, yin nourishing removing heat from blood, depressed liver-energy dispersing and QI regulating, astringent or styptic treatment for spontaneous sweating collateral dredging are controlled.
Six-element phalacrosis prevention and hair generation preparation of the present invention is processed by Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali, Herba Menthae.In the side, Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis drive hot dampness big bitter Great Cold, and bacterio static itching-relieving pushes away and swings the poison heresy, and the merit of blood circulation promoting and blood stasis dispelling is arranged; Radix Polygoni Multiflori replenishing YIN and blood, Radix Angelicae Sinensis is invigorated blood circulation; The sweet temperature of the Radix Astragali, the diuretic blood stasis dispelling, QI invigorating, the Tuoli toxin expelling, the assistant Radix Polygoni Multiflori, Radix Angelicae Sinensis, profit blood is dry, the merit of activating blood circulation and unblocking obstruction; Be aided with the Herba Menthae dispelling wind and heat pathogens, refresh oneself's article, pore a surname loose, and fate blood follows, to reduce fat secretion.All medicines share, and blood circulation promoting and blood stasis dispelling dispels the wind, and will nourish blood, bacterio static itching-relieving, and moist hair resides in wherein.Thereby said preparation has nourshing blood and promoting blood circulation, the function of the hair growth promoting of dispeling the wind, and qi-blood disharmony, dryness-transformation is given birth to wind and the dandruff that causes increases, the pruritus symptom has certain mitigation.
Six-element phalacrosis prevention and hair generation tincture is brownish red to a peony clear liquid, has special odor; Wherein contain a kind of polymer substance that can efficiently suppress sebum secretion, this material can make undue active sebaceous gland atrophy, removes the various mycins in the scalp hair follicle, prevents seborrheic alopecia rapidly; Can also activate hair follicle for hair growth provides essential nutrient substance, promote scalp blood circulation and hair replacement.A large amount of clinical practices show: used this tincture treatment seborrheic alopecia 3～5 days, and can obviously produce scalp and become dry the curative effect that alopecia alleviates gradually; Used about 20～30 days, and just can suppress alopecia fully, and a large amount of New Development germinatings are arranged; Used 3～4 months, the patient that hair follicle is not downright bad fully as yet, the symptom of alopecia, poliosis will be recovered largely and improved.
The external of this preparation is wiped and to be put the alopecia position on the skin, and with the principle of transdermal administration, the degree of depth is infiltrated cortex, and blood circulation promoting promotes hair regeneration, and is peculiar to seborrheic alopecia, physiologic alopecia, young and middle-aged early whitening of hair effect.To alopecia areata, alopecia totalis, alopecia universalis, poliosis, teen-ager leukotrichia, dandruff too much, scalp itch also has peculiar effect.
Five step therapies of Six-element phalacrosis prevention and hair generation tincture: reduce the epidermis oils and fats, improve subcutaneous blood fortune; Directly lax vascular smooth muscle, the expansion blood capillary promotes subcutaneous microcirculation, improves the hair growth environment; Rely on distinctive polymer substance, strengthen the oxygen content of hair follicle cell, activate the regeneration capacity of hair follicle cell, promote the melanic generation of hair follicle; Utilize the several amino acids and the trace element that are contained, directly nutrition is provided, impel hair follicle to transform to trophophase by rest period to hair follicle; Grow New Development, the poliosis blackening.
In order to verify the effect of Six-element phalacrosis prevention and hair generation preparation of the present invention; The applicant is that example has been carried out clinical experimental study with Six-element phalacrosis prevention and hair generation tincture; " Six-element phalacrosis prevention and hair generation tincture " externally-used embrocation of application of pure Chinese medicine preparation has been obtained significantly anti-alopecia and effects such as hair growth promoting, removing scurf and relieving itching, and contrasts with patient that simple use hair growth promoting tincture (Beijing Tongrentang Technology Development Co.ltd. Pharmaceutical Factory) is treated; The former effect is satisfied, the existing summary as follows:
1, clinical data
Hair loss patient is totally 126 examples, is divided into two groups at random, and two groups at the age, do not have significant difference on alopecia scope and the course of disease length.The treatment group is with Six-element phalacrosis prevention and hair generation tincture treatment totally 68 examples, wherein male 36 examples, women 30 examples, age 17-65 year, course of disease 0.7-13; Matched group is totally 56 examples, wherein male 32 examples, women 28 examples, age 16.5-67 year, course of disease 1.5-10.Two groups of patients belong to moist seborrheic alopecia 70 examples, dryness seborrheic alopecia 54 examples.The alopecia of forehead symmetry is many than center, the crown.Skin lesion place scalp is greasy shinny, and a large amount of dandruffs are arranged, and is the broken little bran skin shape of canescence, or dry scalp lacks gloss, conscious pruritus.
1.1 Therapeutic Method treatment group patient external Six-element phalacrosis prevention and hair generation tincture is coated with the affected part gently with medicinal liquid, tunks 5-10 minute with finger gently at the coating place at last, every day 1-2 time, 30d is 1 course of treatment, treats 4 courses of treatment continuously.Matched group patient external hair tincture (Beijing Tongrentang Technology Development Co.ltd. Pharmaceutical Factory) dips in medicine with absorbent cotton and wipes affected part, 3 times/d.Reach treatment before all patient treatments and followed up a case by regular visits to the record result in back 4 months, evaluate curative effect after the drug withdrawal.
1.2 observation index seborrheic alopecia patient observes the forward and backward alopecia degree of treatment, scalp itch, squama, sebum and every square centimeter of newborn number of hairs.The fine hair on birds or animals galley proof is sent out whether chap, black, hard, long etc.Whether alopecia areata patient observes the forward and backward topical manifestations of medication, smooth like the alopecia district, has or not fine hair on birds or animals hair, terminal hair, and fine hair on birds or animals hair, terminal hair account for alopecia district ratio etc.Further consultation in every month 1 time.
1.3 curative effect determinate standard recovery from illness: the alopecia district recovers normal, no scratchiness; Produce effects: alopecia obviously reduces or recovers normal, and dandruff, pruritus disappear, and the affected part has obvious New Development growth or former fine hair on birds or animals galley proof to send out chap, black, hard, long, and outward appearance is obviously improved; Effectively: alopecia, dandruff reduce, and pruritus alleviates, and there is the New Development growth in the affected part, and outward appearance makes moderate progress; Invalid: alopecia, dandruff slightly reduce or no change, and pruritus is slightly light or the same, no New Development growth, and outward appearance is improved not obvious.
1.4 all The data X of statistical method
2Check judges that with P not statistically significant is arranged.
2, result
Two groups of patients of two groups of therapeutic effect (seeing table 1), 4 all cure rates relatively have statistical significance (X
2=10.7324, P＜0.01), treatment group total effective rate is 57.35%, matched group is that 33.93%, two group of curative effect is through X
2Check, difference has statistical significance (X
2=6.7683, P＜0.01).
Table 1 liang group patient clinical efficacy comparison (example, %)
| Group | The example number | Recovery from illness | Produce effects | Effectively | Invalid | Effective percentage (%) |
| The treatment group | 68 | 19 | 20 | 21 | 8 | 57.35 |
| Matched group | 56 | 3 | 16 | 22 | 15 | 33.93 |
Annotate: P＜0.05.
3, discuss
The initial effect of Six-element phalacrosis prevention and hair generation tincture shows as hair strengthening, promptly stops alopecia or alopecia and reduces, and occurs hair growth promoting, long hair subsequently, promptly bears the fine hair on birds or animals galley proof earlier and sends out, and gradually becomes terminal hair again, or the fine hair on birds or animals galley proof is sent out blackening gradually, thick, hard, long.This medicine too much all has therapeutical effect in various degree to scalp itch, dandruff, sebum except that hair strengthening, hair regrowth are arranged, pruritus is disappeared or alleviate, and dandruff disappears or reduces.This medicine can make the too much sebum of head reduce, and makes the few and dry person of part head sebum become soft and moist.Do not find obvious adverse reaction in this test.
Six-element phalacrosis prevention and hair generation tincture is a pure Chinese medicinal preparation, the merit that has nourshing blood and promoting blood circulation, dispels the wind and think of a way.Qi-blood disharmony, dryness-transformation is given birth to wind and the dandruff that causes increases, and the pruritus symptom has certain mitigation, cooperates suitable massage affected part to strengthen the hair follicle microcirculation, improves trichotrophy, and promotion hair growth and drug absorption have better hair growing effect.
In order to ensure the science of quality determining method of the present invention, effectively and reasonably, the applicant has also carried out relevant experimental study to it:
There is not the assay project in the quality inspection standard { Guizhou Province Department of Public Health file [No. the 476th, Qianweiyaozhi (93)] } of former phalacrosis prevention and hair generation spirit [No. the 29th, the accurate word of medicine (1993) L defended in the Guizhou Province], and not clear and definite recipe quantity and detailed method for making.The Radix Polygoni Multiflori that contains in the Six-element phalacrosis prevention and hair generation preparation prescription of the present invention is principal agent in the side, and for controlling product quality better, the applicant has carried out methodological study to its assay.
Radix Polygoni Multiflori in the prescription is a main component, with reference to " 2005 editions Radix Polygoni Multiflori medical materials of Chinese pharmacopoeia are detected as and are divided into 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9), select Radix Polygoni Multiflori contained 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) content is index, in the preparation of the present invention 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) the high performance liquid chromatogram content assaying method carried out the research of projects such as precision, stability, repeatability, the recovery test range of linearity, set up effective content assaying method, with control product quality.
1, instrument and reagent
Instrument: Tianjin, island prominence LC-10Atvp high performance liquid chromatograph
Chromatographic column: Hypersil-ODS C
18(4.6 * 150mm)
HS10260D ultrasonic washing unit (260W, 40KHZ, the permanent Orco skill in Tianjin Development Co., Ltd)
The AUW120D electronic balance (100,000/, day island proper Tianjin company)
Reagent: 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 100080-200306)
Six-element phalacrosis prevention and hair generation tincture sample and Radix Polygoni Multiflori negative sample;
Generally use acetonitrile to be analytical pure, mobile phase uses acetonitrile to be chromatographically pure, and water is ultra-pure water, and other reagent is analytical pure.
2, the selection of condition determination
The preparation of need testing solution: accurate absorption tincture 5ml of the present invention, put in the 50ml measuring bottle, add 50% ethanol 30ml, close plug, supersound extraction 10min, taking-up is put and is chilled to room temperature,, shakes up to scale with 50% ethanol dilution, promptly gets.
3, chromatographic condition confirms
With reference to related data 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) method under the assay item, 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) at the 320nm place big absworption peak is arranged, so select wavelength 320nm as measuring wavelength.
In addition mobile phase is studied, with acetonitrile-water (23: 77) for mobile phase makes an experiment, to 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) separating effect, theoretical cam curve be all relatively good.Obtain flow speed control simultaneously when 1.0ml/min, retention time, separating degree are all desirable, and negative sample is noiseless.
So final definite chromatographic condition is: the detection wavelength is 320nm; Mobile phase is acetonitrile-water (23: 77); Flow velocity is 1.0ml/min.
4, the investigation of linear relationship
Precision takes by weighing 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) reference substance 25.92mg, put in the 25ml volumetric flask, add 50% dissolve with methanol solution, be settled to scale (concentration is 1.0368mg/ml).Accurate respectively 1ml, 1ml, 1ml, 3ml, the 5ml of drawing; Respectively place 50ml, 25ml, 10ml, 10ml, 10ml volumetric flask, add 50% methanol, shake up to scale; Be mixed with variable concentrations solution; Accurate each the 10 μ l of above-mentioned 5 parts of reference substance solution that draw according to the chromatographic condition sample introduction, measure peak area.With reference substance concentration is abscissa, and the peak area integrated value is a vertical coordinate drawing standard curve, with peak area sample concentration (μ g/ml) is carried out linear regression and calculates.Getting equation of linear regression is: 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9): y=0.0000771X-1.52572058, r=0.9999, by table can know 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) good in 20.736 μ g/ml～518.4 μ g/ml scope internal linear relation.The result sees table 2:
Table 22,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) linear relationship
5, precision test
Get 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) reference substance solution (103.68 μ g/ml) 10 μ l, repeat sample introduction 5 times, measure peak area, 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) average peak area be 1362173; RSD (%) is 0.62%.The result sees table 3:
Table 32,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) precision test
6, the investigation of sample extraction time
Accurate 4 parts of the tincture 5ml of the present invention that draw put in the 50ml measuring bottle, add 50% ethanol 30ml; Close plug, supersound process 5 minutes, 10 minutes, 15 minutes, 20 minutes, taking-up is put and is chilled to room temperature; To scale, shake up accurate respectively above-mentioned test sample liquid and the reference substance 10 μ l injection chromatograph of liquid drawn with 50% ethanol dilution; Measure, promptly get.The result is following:
The investigation of table 4 ultrasonic time
| Ultrasonic time (minute) | 5 | 10 | 15 | 20 |
| Content (mg/ml) | 0.1432 | 0.1416 | 0.1395 | 0.1407 |
Can know that by the result extraction time influences not quite the assay result, so the selective extraction time is 10min.
7, stability test
Get tincture 5ml of the present invention, prepare test liquid by the method for preparing of test liquid under the assay item, respectively at 0,2,4,6,8 hour sample introduction, measure 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) peak area, 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) average peak area is 187961, RSD is 0.487%, explains that test liquid is good at 8 hours internal stabilities.The result sees table 5.
Table 52,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) stability test
8, replica test
By the content assaying method that the present invention drafts, get 5 parts in same lot number sample, precision is measured 5ml, operates by the method under need testing solution preparation and the mensuration item, measures result such as table 6 in accordance with the law:
Table 62,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) replica test
9, recovery test
Precision is measured 5 parts of the tinctures of the present invention of known content, every part of 3ml, accurate respectively add a certain amount of 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) reference substance solution 1ml (concentration 1.0368mg/ml), handle according to the need testing solution method for preparing, promptly get 5 duplicate samples solution.Measure according to the method under the assay item, calculate recovery rate, the result sees table 7.
The test of table 7 average recovery
Test shows: average recovery rate is 101.2%, RSD=1.6%, and this method has the response rate preferably.
Experimental summary: through in the Six-element phalacrosis prevention and hair generation tincture 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) assay experiment, show: good in 20.736 μ g/ml～518.4 μ g/ml scope internal linear relation, precision empirical average peak area is 1362173, and RSD (%) is 0.62%; The stability test average peak area is 187961, and RSD is 0.487%, explains that test liquid is good at 8 hours internal stabilities; The replica test average content is 0.1432, and RSD is 0.23%; Average recovery test average recovery rate is 100.186%, RSD=0.7197%.Therefore, this content assaying method is feasible.
Compared with prior art, Six-element phalacrosis prevention and hair generation preparation provided by the present invention has the effect of removing scurf and relieving itching, phalacrosis prevention and hair generation, black hair hair care, and its total effective rate of clinical verification reaches 96%; And control takes into account, and safety non-toxic is the ideal pure Chinese medicinal preparation of treatment seborrheic alopecia; Said quality determining method specificity is strong, and precision is high, good stability, and measurement result is accurate, can effectively control the quality of Six-element phalacrosis prevention and hair generation preparation, thereby guarantees its clinical efficacy.
The specific embodiment:
Below be embodiment:
Embodiments of the invention 1: the preparation of Six-element phalacrosis prevention and hair generation tincture:
Radix Et Rhizoma Rhei 30g, Radix Sophorae Flavescentis 20g, Radix Polygoni Multiflori 15g, Radix Angelicae Sinensis 15g, Radix Astragali 15g, Herba Menthae 5g
Get above Six-element, be ground into coarse powder, mixing is according to the percolation (pharmacopeia appendix I O) under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours, with the speed of per minute 2～3ml percolation slowly; Collect percolate 1000ml, activated carbon adsorption filters; Fill, packing promptly gets Six-element phalacrosis prevention and hair generation tincture.Its method for using is divided into washout method and two kinds of outer rubbing methods.Washout method: get this preparation 20ml after the hair washing, add warm water 100ml dilution back and directly drench, and pat gently after 2～3 minutes and dry, no longer flushing in the scalp and the portion of sending out; 2～3 days once.Outer rubbing method: the affected part with local scrub, is embrocated with medicinal liquid with hot towel then gently by elder generation, kowtows gently at the coating place with finger at last and hits 5～10 minutes, every day 1～2 time.During the treatment, diet cigarette, wine and pungent thing.The ethanol allergy sufferers is forbidden.
Embodiments of the invention 2: the preparation of Six-element phalacrosis prevention and hair generation gel:
Get Radix Et Rhizoma Rhei 25g, Radix Sophorae Flavescentis 15g, Radix Polygoni Multiflori 10g, Radix Angelicae Sinensis 10g, Radix Astragali 10g and Herba Menthae 3g, be ground into coarse powder, mixing; According to the percolation under fluid extract and the extractum item, make solvent with 55% ethanol, flood after 24 hours; With the speed of per minute 2～3ml percolation slowly, collect percolate, activated carbon adsorption; Be concentrated into 10g, add gel substrate and (form by Acritamer 940 20g, glycerol 60g, Macrogol 4000 20g, dehydrated alcohol 220g, triethanolamine 30g and water 800g; Get Acritamer 940 and add an amount of distilled water and in mortar, grind evenly, drip triethanolamine and regulate and make gel, add Macrogol 4000, glycerol, dehydrated alcohol more successively, grind well promptly get) 940g, stir, promptly get Six-element phalacrosis prevention and hair generation gel.10～30g is got in the said preparation external at every turn, embrocates in scalp and root of hair portion, and 2～3 days once.
Embodiments of the invention 3: the preparation of Six-element phalacrosis prevention and hair generation ointment:
Get Radix Et Rhizoma Rhei 35g, Radix Sophorae Flavescentis 25g, Radix Polygoni Multiflori 20g, Radix Angelicae Sinensis 20g, Radix Astragali 20g and Herba Menthae 7g, be ground into coarse powder, mixing; According to the percolation under fluid extract and the extractum item, make solvent with 55% ethanol, flood after 24 hours; With the speed of per minute 2～3ml percolation slowly, collect percolate, activated carbon adsorption; Be concentrated into 20g, the ointment base that adding is chilled to after the room temperature (is made up of sodium carboxymethyl cellulose 150g, glycerol 100g, ethyl hydroxybenzoate 2.5g and water 1000g; Get Carboxymethyl cellulose sodium and place mortar, add glycerol and grind well, add entry 800ml and make dissolving fully, add the aqueous solution that is dissolved with ethyl hydroxybenzoate then while grinding, grind evenly, promptly get) 950g, grind mixing, promptly get Six-element phalacrosis prevention and hair generation ointment.10～30g is got in the said preparation external at every turn, embrocates in scalp and root of hair portion, and 2～3 days once.
Embodiments of the invention 4: the preparation of Six-element phalacrosis prevention and hair generation ointment:
Get Radix Et Rhizoma Rhei 25g, Radix Sophorae Flavescentis 25g, Radix Polygoni Multiflori 10g, Radix Angelicae Sinensis 20g, Radix Astragali 10g and Herba Menthae 7g, be ground into coarse powder, mixing; According to the percolation under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours, with the speed of per minute 2～3ml percolation slowly; Collect percolate; Activated carbon adsorption is concentrated into 15g, and the ointment base that adding is chilled to after the room temperature (is made up of stearic acid 14 weight portions, glyceryl monostearate 4 weight portions, Oleum Ricini 24 weight portions, glycerol 12 weight portions, triethanolamine 2 weight portions, ethylparaben 0.24 weight portion and water 8 weight portions; Get stearic acid, glyceryl monostearate, Oleum Ricini and ethylparaben and melt, get oil phase substrate, in addition glycerol, triethanolamine, water are melted 50～60 ℃ of heated and stirred 50～60 ℃ of heated and stirred; Get aqueous phase substrate, oil phase substrate is slowly added in the aqueous phase substrate, and constantly stir; Mixing; Promptly get) 920g, grind mixing, promptly get Six-element phalacrosis prevention and hair generation ointment.
Embodiments of the invention 5: the preparation of Six-element phalacrosis prevention and hair generation liniment:
Get Radix Et Rhizoma Rhei 35g, Radix Sophorae Flavescentis 15g, Radix Polygoni Multiflori 20g, Radix Angelicae Sinensis 10g, Radix Astragali 20g and Herba Menthae 3g, be ground into coarse powder, mixing is according to the percolation under fluid extract and the extractum item; Make solvent with 55% ethanol, flood after 24 hours,, collect percolate with the speed of per minute 2～3ml percolation slowly; Activated carbon adsorption is concentrated into 18g, adds entry or glycerol or ethanol or vegetable oil 980g; Mixing filters, and promptly gets Six-element phalacrosis prevention and hair generation liniment.10～30g is got in the said preparation external at every turn, embrocates in scalp and root of hair portion, and 2～3 days once.
Embodiments of the invention 6: the quality determining method of Six-element phalacrosis prevention and hair generation preparation comprises following project:
Differentiate: this preparation 20ml is got in (1), flings to ethanol in the water-bath, adds diethyl ether to extract 2 times, and each 15ml merges ether solution, is concentrated into 1ml as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.2g, and the 10ml jolting that adds diethyl ether was extracted 20 minutes, filters, and filtrating is waved to about 1ml, as control medicinal material solution; Get the chrysophanic acid reference substance again, add diethyl ether and process the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel H lamellae; With normal hexane: ethyl acetate: formic acid=30: 10: 0.5 is developing solvent, launches, and takes out; Dry, put under the 365nm uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; With reference substance chromatograph relevant position on, show a speckle of same color; Put in the ammonia steam smoked after, speckle becomes redness.
(2) get this preparation 20ml, volatilize in the water-bath, add the dissolving of 25ml chloroform and 0.3ml strong ammonia solution, filter, filtrating is waved to 1ml, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With chloroform: methanol: strong ammonia solution=20: 2.4: 0.8,10 ℃ of lower floor's solution with held are developing solvent; Put in the expansion cylinder of ammonia saturated with vapor, launch, take out; Dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color.
Assay: chromatographic condition and system suitability experiment use 18 alkyl silica gel to be filler; Acetonitrile: water=23: 77 is mobile phase; Column temperature: 40 ℃; The detection wavelength is 320nm; Theoretical cam curve by 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside peak calculates and should be not less than 2000.
The preparation of reference substance solution gets 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside reference substance is an amount of, and accurate the title, decide, and uses 50% dissolve with ethanol, processes the solution that every 1ml contains 0.1mg approximately, shakes up, and promptly gets.
The preparation precision of need testing solution is measured this preparation 5ml, puts in the 50ml measuring bottle, adds 50% ethanol 30ml, close plug, and supersound extraction 10 minutes, taking-up is put and is chilled to room temperature,, shakes up to scale with 50% ethanol dilution, promptly gets.
Accurate each the 10 μ l of above-mentioned three kinds of solution that draw of algoscopy inject chromatograph of liquid, measure, and promptly get.
The every 1ml of this preparation contains 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside (C
20H
22O
9) must not be less than 0.12mg.
Claims (9)
1. Six-element phalacrosis prevention and hair generation preparation, it is characterized in that: according to listed as parts by weight, it is processed for 3～7 parts with 25～35 parts of Radix Et Rhizoma Rhei, 15～25 parts of Radix Sophorae Flavescentiss, 10～20 parts of Radix Polygoni Multiflori, 10～20 parts of Radix Angelicae Sinensis, 10～20 parts of the Radixs Astragali, Herba Menthae.
2. according to the described Six-element phalacrosis prevention and hair generation of claim 1 preparation, it is characterized in that: according to listed as parts by weight, it is processed for 5 parts with 30 parts of Radix Et Rhizoma Rhei, 20 parts of Radix Sophorae Flavescentiss, 15 parts of Radix Polygoni Multiflori, 15 parts of Radix Angelicae Sinensis, 15 parts of the Radixs Astragali and Herba Menthae.
3. according to claim 1 or 2 described Six-element phalacrosis prevention and hair generation preparations, it is characterized in that: described preparation is tincture, gel, ointment or liniment.
4. like the method for preparing of each said Six-element phalacrosis prevention and hair generation preparation among the claim 1-3, it is characterized in that: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder; Mixing according to the percolation under fluid extract and the extractum item, is made solvent with 55% ethanol; Flood after 24 hours,, collect percolate with the speed of per minute 2～3ml percolation slowly; Activated carbon adsorption, filtration, fill are processed tincture or are added appropriate amount of auxiliary materials and process gel, ointment or liniment.
5. according to the method for preparing of the said Six-element phalacrosis prevention and hair generation of claim 4 preparation, it is characterized in that: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder, mixing; According to the percolation under fluid extract and the extractum item, make solvent with 55% ethanol, flood after 24 hours, with the speed of per minute 2～3ml percolation slowly; Collect percolate, activated carbon adsorption is concentrated into 10～20 weight portions; Add gel substrate 900～990 weight portions, stir, promptly get gel.
6. according to the method for preparing of the said Six-element phalacrosis prevention and hair generation of claim 4 preparation, it is characterized in that: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder; Mixing according to the percolation under fluid extract and the extractum item, is made solvent with 55% ethanol; Flood after 24 hours,, collect percolate with the speed of per minute 2～3ml percolation slowly; Activated carbon adsorption is concentrated into 10～20 weight portions, and adding is chilled to ointment base 900～990 weight portions after the room temperature; Grind mixing, promptly get ointment.
7. according to the method for preparing of the said Six-element phalacrosis prevention and hair generation of claim 4 preparation, it is characterized in that: get Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Polygoni Multiflori, Radix Angelicae Sinensis, the Radix Astragali and Herba Menthae, be ground into coarse powder; Mixing according to the percolation under fluid extract and the extractum item, is made solvent with 55% ethanol; Flood after 24 hours,, collect percolate with the speed of per minute 2～3ml percolation slowly; Activated carbon adsorption is concentrated into 10～20 weight portions, adds entry or glycerol or ethanol or vegetable oil 900～990 weight portions; Mixing filters, and promptly gets liniment.
8. like the quality determining method of the said Six-element phalacrosis prevention and hair generation of claim 1-3 preparation; It is characterized in that: said quality determining method comprises to be differentiated and assay; Wherein differentiate the thin layer chromatography discriminating that comprises Radix Et Rhizoma Rhei in the preparation and Radix Sophorae Flavescentis; The discrimination method of Radix Et Rhizoma Rhei is to be contrast with Radix Et Rhizoma Rhei control medicinal material and chrysophanic acid reference substance; With n-hexane: ethyl acetate: formic acid=30: 10: 0.5 is the thin layer chromatography of developing solvent, and the discrimination method of Radix Sophorae Flavescentis is to be contrast with the matrine reference substance, and with chloroform: methanol: strong ammonia solution=20: 2.4: 0.8,10 ℃ of lower floor's solution with held are the thin layer chromatography of developing solvent; Assay is with in the high effective liquid chromatography for measuring preparation 2,3,5; The content of 4 ˊ-tetrahydroxystilbene-2-0-β-D-glucoside, 2,3; 5,4 '-content assaying method of tetrahydroxystilbene-2-0-β-D-glucoside is with 2,3; 5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside reference substance is contrast, with acetonitrile: water=23: 77 is the HPLC of mobile phase.
9. according to the quality determining method of the said Six-element phalacrosis prevention and hair generation of claim 8 preparation, it is characterized in that: described quality determining method comprises:
Differentiate: this preparation 20ml is got in (1), flings to ethanol in the water-bath, adds diethyl ether to extract 2 times, and each 15ml merges ether solution, is concentrated into 1ml as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.2g, and the 10ml jolting that adds diethyl ether was extracted 20 minutes, filters, and filtrating is waved to 1ml, as control medicinal material solution; Get the chrysophanic acid reference substance again, add diethyl ether and process the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel H lamellae; With n-hexane: ethyl acetate: formic acid=30: 10: 0.5 is developing solvent, launches, and takes out; Dry, put under the 365nm uviol lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; With reference substance chromatograph relevant position on, show a speckle of same color; Put in the ammonia steam smoked after, speckle becomes redness;
(2) get this preparation 20ml, volatilize in the water-bath, add the dissolving of 25ml chloroform and 0.3ml strong ammonia solution, filter, filtrating is waved to 1ml, as need testing solution; Other gets the matrine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, as reference substance solution; According to the test of Chinese Pharmacopoeia appendix VI B thin layer chromatography, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With chloroform: methanol: strong ammonia solution=20: 2.4: 0.8,10 ℃ of lower floor's solution with held are developing solvent; Put in the expansion cylinder of ammonia saturated with vapor, launch, take out; Dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
Assay: chromatographic condition and system suitability experiment use 18 alkyl silica gel to be filler; Acetonitrile: water=23: 77 is mobile phase; Column temperature: 40 ℃; The detection wavelength is 320nm; Theoretical cam curve by 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside peak calculates and should be not less than 2000;
The preparation of reference substance solution gets 2,3,5,4 '-tetrahydroxystilbene-2-0-β-D-glucoside reference substance is an amount of, and accurate the title, decide, and uses 50% dissolve with ethanol, processes the solution that every 1ml contains 0.1mg, shakes up, and promptly gets;
The preparation precision of need testing solution is measured this preparation 5ml, puts in the 50ml measuring bottle, adds 50% ethanol 30ml, close plug, and supersound extraction 10 minutes, taking-up is put and is chilled to room temperature,, shakes up to scale with 50% ethanol dilution, promptly gets;
Accurate each the 10 μ l of above-mentioned three kinds of solution that draw of algoscopy inject chromatograph of liquid, measure, and promptly get;
The every 1ml of this preparation contains 2,3,5,4 ˊ-tetrahydroxystilbene-2-0-β-D-glucoside C
20H
22O
9Must not be less than 0.12mg.
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