CN1806836A - Chinese medicinal composition, its preparation process and quality control method - Google Patents
Chinese medicinal composition, its preparation process and quality control method Download PDFInfo
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- CN1806836A CN1806836A CN 200510200041 CN200510200041A CN1806836A CN 1806836 A CN1806836 A CN 1806836A CN 200510200041 CN200510200041 CN 200510200041 CN 200510200041 A CN200510200041 A CN 200510200041A CN 1806836 A CN1806836 A CN 1806836A
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Abstract
The invention provides a Chinese medicinal composition for treating gynaecologic diseases, which is prepared from cnidium fruit, honeysuckle flower, cape jasmine, cortex pseudolaricis, corktree bark, baikal skullcap root, flavescent sophora root, broom cypress fruit, oriental wormwood, mentha, Chinese mugwort leafmulberry leaf, pubescent angelica root, atractylis ovata and grassleaved sweetflag rhizome. The invention also discloses the process for preparing the medicinal composition and the quality control method.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof, belong to the field of Chinese medicines.
Background technology
Vaginitis is a common gynecological disease.Because vagina communicates with the external world, often bad because of menstrual period or sexual life health, or because of factors such as childbirth and uteroventral operation cause vaginal infection, even can make inflammation attack internal reproductive organ, cause pelvic inflammation.Suffer from diabetes, vitamin B group shortage, ovarian function decline in addition, some allergy or infectious disease person be easy infection more, and the infective pathogen body often is mycete, antibacterial, mycoplasma, chlamydia etc.Except that senile vaginitis, the equal attribute of several vaginitiss spreads disease, and sickness rate is on the rise in recent years.Therefore, it is very necessary to explore a kind of medicine for the treatment of such disease.
Summary of the invention
The purpose of this invention is to provide a kind of preparation treatment women damp-heat vaginal discharge, Chinese medicine composition of using in mycotic, infusorian property and the nonspecific vaginitis medicine and preparation method thereof; The present invention also aims to provide a kind of method of quality control of Chinese medicine composition.
The present invention seeks to be achieved through the following technical solutions:
The inventor has developed a kind of Chinese medicine composition, and the crude drug of said composition makes up by following weight ratio:
50～75 parts of 50～75 parts of Cortex Pseudolariciss of 50～75 portions of Fructus Gardeniaes of 50～75 portions of Flos Loniceraes of Fructus Cnidii
50～75 parts of 50～75 parts of Fructus Kochiae of 100～150 parts of Radix Sophorae Flavescentiss of 50～75 parts of Radix Scutellariaes of Cortex Phellodendri
50～75 parts of 50～75 parts of Radix Angelicae Pubescentiss of 100～150 portions of Folium Artemisiae Argyis of 50～75 portions of Herba Menthaes of Herba Artemisiae Scopariae
100～150 parts of 50～75 parts of Rhizoma Acori Graminei of Rhizoma Atractylodis
Definitely, the weight ratio of these crude drug is:
62.5 parts of 62.5 parts of Cortex Pseudolariciss of 62.5 portions of Fructus Gardeniaes of 62.5 portions of Flos Loniceraes of Fructus Cnidii
62.5 parts of 62.5 parts of Fructus Kochiae of 125 parts of Radix Sophorae Flavescentiss of 62.5 parts of Radix Scutellariaes of Cortex Phellodendri
62.5 parts of 62.5 parts of Radix Angelicae Pubescentiss of 125 portions of Folium Artemisiae Argyis of 62.5 portions of Herba Menthaes of Herba Artemisiae Scopariae
125 parts of 62.5 parts of Rhizoma Acori Graminei of Rhizoma Atractylodis
With above prescription, can make various clinical suitable dosage forms in theory, the inventor is preferably suppository at the characteristics of indication, has studied its preparation technology simultaneously and should be:
Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis add alcohol reflux in will writing out a prescription, and filtrate is condensed into clear paste, and be standby; Get all the other medical materials and decoct with water, collect volatile oil simultaneously, collecting decoction filters, and filtrate is condensed into clear paste, merges spray drying with above-mentioned concentrated extract; With spray powder, volatile oil, add conventional adjuvant and make suppository.
Concrete technology after the parameters optimization is: Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis add 70% alcohol reflux secondary in will writing out a prescription, and each 2 hours, collecting decoction filtered, and filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), and is standby; Get all the other medical materials and decoct with water secondary, each 2 hours, collect volatile oil simultaneously, collecting decoction, filter, filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), merges with above-mentioned concentrated extract, spray drying, spray powder, volatile oil add conventional adjuvant and make suppository.
This suppository can be conveniently used in the treatment of gynaecopathia, and the inventor has tentatively reached goal of the invention.
For the effective quality of control product of the present invention, the inventor has also formulated method of quality control, comprises qualitative identification and assay, below describes respectively.
Qualitative identification comprises in following five kinds one or more:
A. get present composition preparation 5～10g, put in the apparatus,Soxhlet's, add petroleum ether 200ml, refluxed 3 hours, petroleum ether liquid discards, and residue takes out, cold wind dries up, and adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether extraction three times, each 20ml merges ether solution, volatilize, add methanol 1ml and make dissolving, as need testing solution; Other gets the osthole reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetate (30: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
B. get [discriminating] (a) down behind ether extraction surplus water liquid transfer pH2～3 with hydrochloric acid, with ethyl acetate extraction three times, 20ml at every turn, merge ethyl acetate liquid, extract three times, each 20ml with 5% sodium bicarbonate solution, merge alkali liquor, transfer pH2～3, with ethyl acetate extraction three times with hydrochloric acid, each 20ml, merge ethyl acetate liquid, be washed to neutrality, evaporate to dryness, residue adds methanol 5ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography test, draw each 0.5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with the upper solution of butyl acetate-formic acid-water (4: 2: 2), launch, take out, to dry, spray is with 2% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
C. get [discriminating] (b) down behind ethyl acetate extraction surplus water liquid add ammonia and transfer pH9, extract three times with water-saturated n-butanol, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 2～3ml makes dissolving, is added on neutral alumina post (120～160 orders, 5g; Internal diameter 1.5cm), with 50% methanol-eluted fractions, collect eluent 50ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, (2: 3: 4: 0.2) be developing solvent, expansion was taken out with benzene-acetone-ethyl acetate-strong ammonia solution, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
D. get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds 1 of methanol 10ml, hydrochloric acid, shakes up, and supersound process 15 minutes filters, and filtrate is medical material liquid in contrast.Test according to thin layer chromatography, draw [discriminating] (c) each 2 μ l of need testing solution 5 μ l, reference substance and control medicinal material solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-isopropyl alcohol-methanol-water (6: 3: 1.5: 1.5: 0.3) is developing solvent, put in the expansion cylinder of ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
E. get the jasminoidin reference substance in addition, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw [discriminating] (c) a following need testing solution and each 10 μ l of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water (7: 1: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Assay comprises in following three kinds any one or more:
A. the assay of osthole in the Fructus Cnidii
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (70: 30) is a mobile phase, and the detection wavelength is 322nm, and number of theoretical plate is pressed the osthole peak and calculated, and should be not less than 2500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the osthole reference substance, and add neutral alcohol and make dissolving, and dilution, make the solution that contains 20 μ g among every 1ml, in contrast product solution.
The preparation precision of need testing solution is measured this product 5ml, add ammonia 0.25ml, mixing is put and is concentrated near doing in the hot bath, adding the small amount of ethanol dissolving also quantitatively is transferred in the 10ml measuring bottle, supersound process 10 minutes is put to room temperature, adds ethanol dilution to scale, shake up, filter, discard filtrate just, get subsequent filtrate as need testing solution.
Algoscopy precision is respectively measured reference substance solution and each 10～20 μ l of need testing solution, injects chromatograph of liquid, measures peak area, calculates with external standard method, promptly.
This composite preparation per unit amount contains Fructus Cnidii with osthole (C
15H
16O
3) meter, must not be less than 0.3mg.
Above-mentioned unit quantity is meant the finished medicines dosage that contains suitable 10.6g crude drug.
B. the assay of jasminoidin in the Fructus Gardeniae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (11: 89) is a mobile phase, and flow velocity is 1.0ml/min, 30 ℃ of column temperatures.Detect wavelength 238nm.Number of theoretical plate calculates by the jasminoidin peak should be not less than 5000.
The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 35 μ g with mobile phase, shakes up, promptly.
4 pieces of this product are got in the preparation of need testing solution, and 3.0g is got in chopping, and accurate the title decides, place apparatus,Soxhlet's, add petroleum ether (60 ℃～90 ℃) 200ml and refluxed the residue evaporate to dryness 3 hours, put in the tool plug conical flask, the accurate methanol 50ml that adds weighs, it is ultrasonic that (250W 50kHz) handled 30 minutes, put cold, weigh, supply the weight of loss, shake up with methanol, filter, get subsequent filtrate and filter, as need testing solution with microporous filter membrane (0.45 μ m).
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This composite preparation per unit amount contains Fructus Gardeniae with jasminoidin (C
17H
24O
10) meter, must not be less than 0.6mg.
Above-mentioned unit quantity is meant the finished medicines dosage that contains suitable 1.06g crude drug.
C. content of baicalin is measured in the Radix Scutellariae
Chromatographic condition and system suitability test are filler with octadecyl silane; Methanol-0.3% phosphoric acid solution (47: 53) is a mobile phase; 40 ℃ of column temperatures; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the baicalin peak.
It is an amount of that the baicalin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 50 μ g, promptly.
5 pieces of this product are got in the preparation of need testing solution, and chopping takes by weighing 1g, and accurate the title decides, put in the apparatus,Soxhlet's, add petroleum ether (60 ℃～90 ℃) 200ml, refluxed 3 hours, take out filtration paper cylinder, cold wind dries up, and precision adds methanol 50ml, claims to decide weight, (100W 50kHz), was cooled to room temperature to supersound extraction in 30 minutes, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate and filter, promptly with microporous filter membrane (0.45 μ m).
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
This composite preparation per unit amount contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 6.75mg.
Above-mentioned unit quantity is meant the finished medicines dosage that contains suitable 1.06g crude drug.
The specific embodiment
Pharmaceutical preparation of the present invention has heat clearing and damp drying, the function of killing parasites for relieving itching.The inventor cures mainly according to its function, from aspects such as antiinflammatory, anti-vaginitis, trichomonas vaginitises its pharmacodynamics is studied.
1 antiinflammatory action
The influence experiment that this product preparation subcutaneous injection causes the mice capillary permeability to influence and this product preparation xylol of mice ear, the result shows: this product preparation 0.27～1.1g/kg * 4d has obvious inhibitory action to Oleum Tiglii induced mice ear swelling; This product preparation 0.13～0.54g/kg * the equal xylol of 4d subcutaneous injection causes the mice capillary permeability obvious inhibitory action, and BAIAI XIYE 1.0g/kg * 4d also has obvious inhibitory action.
2 pairs of colpitic observation of curative effect of rat experiment
Female rats is made the rat ovary excision with after the 10% urethane lumbar injection 1ml/100g anesthesia, 3 weeks of postoperative 1 time every other day gavage diethylstilbestrol 2mg/kg, when vaginal smear examination confirms to have produced puppet during rutting period, carry out candida albicans infection, the bacterium amount is 8 * 10
5Individual/0.2ml/, once a day, for three days on end, stopped to infect back 4 days, vaginal smear will infect male animal again and be divided into 6 groups at random, 10 every group after confirming to infect successfully, use this product preparation 0.54,0.27,0.138g (crude drug)/kg and 10% BAIAI XIYE respectively, FUYANPING, normal saline flushing vagina, every day 1 time, each 10ml, continuous 7 days, 9 days, turning out cloudy with vaginal smear respectively was the treatment index.
The result shows: this product preparation 0.54g (crude drug)/kg administration was 60%, 80% to vagina fungal infection negative conversion rate in 7 days, 9 days; 10% BAIAI XIYE 10ml (being about 10g (crude drug)/kg) negative conversion rate is respectively 30%, 60%; Positive control drug FUYANPING l0ml negative conversion rate is respectively 20%, 30%.
The inhibitory action of 3 pairs of trichomonas vaginitises
Get 72 in 10 * 15mm test tube, this product preparation is respectively established three parallel group with washing liquid, and 11 every group, numbering 1-11, all the other 6 is matched group.Each pipe adds liver infusion culture fluid 7ml, aseptic calf serum 2ml.This product preparation serves as a beginning concentration with 8mg/ml, BAIAI XIYE 20mg/ml, be made into 11 drug level with two-fold dilution's method respectively, each dosing test group is pressed test tube numbering 1-11 and is added test tube 1ml from high-low drug level respectively, then, every pipe adds infusorian 100 microlitres, put in the incubator 37 ℃ and cultivated 48 hours, measure the minimum worm concentration that presses down of this product preparation and BAIAI XIYE.
The result shows: it is that 0.5% (1: 40) can make the infusorian death more than 95% that this product preparation minimum presses down worm concentration, better slightly than BAIAI XIYE (MIC is 0.625%).
Further specify technical scheme of the present invention by the following examples.
Embodiment one
[prescription] Fructus Cnidii 50g Flos Lonicerae 50g Fructus Gardeniae 50g Cortex Pseudolaricis 50g
Cortex Phellodendri 50g Radix Scutellariae 100g Radix Sophorae Flavescentis 50g Fructus Kochiae 50g
Herba Artemisiae Scopariae 50g Herba Menthae 100g Folium Artemisiae Argyi 50g Radix Angelicae Pubescentis 50g
Rhizoma Atractylodis 50g Rhizoma Acori Graminei 100g
[method for making] above 14 flavors, decocting boils secondary respectively, each 2 hours, add for the first time 10 times of amounts, add 8 times of amounts for the second time, collect volatile oil simultaneously, collecting decoction, filter, filtrate decompression (65 ℃～70 ℃ ,-0.08Mpa) be condensed into the clear paste that relative density is about 1.32～1.35 (60 ℃), (65 ℃～70 ℃ of drying under reduced pressure,-0.08Mpa), pulverized 140 mesh sieves, standby; With above-mentioned volatile oil, add Arlacel-80 135g, stir evenly, add above-mentioned extract powder again and fully grind well, mixture is joined in the fused 36 type mixed aliphatic esters (60 ℃), adjust total amount to 2700g, mixing, moulding, take out the cooling back, makes 1000 pieces of bolts, promptly.
Embodiment two
[prescription] Fructus Cnidii 62.5g Flos Lonicerae 62.5g Fructus Gardeniae 62.5g Cortex Pseudolaricis 62.5g
Cortex Phellodendri 62.5g Radix Scutellariae 125g Radix Sophorae Flavescentis 62.5g Fructus Kochiae 62.5g
Herba Artemisiae Scopariae 62.5g Herba Menthae 125g Folium Artemisiae Argyi 62.5g Radix Angelicae Pubescentis 62.5g
Rhizoma Atractylodis 62.5g Rhizoma Acori Graminei 125g
[method for making] above 14 flavors are got Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis and are added 70% alcohol reflux secondary, and each 2 hours, collecting decoction filtered, and filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), and is standby; Get all the other medical materials and decoct with water secondary, each 2 hours, collect volatile oil simultaneously, collecting decoction filters, and filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), merges with above-mentioned concentrated extract, spray drying, it is standby that spray powder gets spray powder; With above-mentioned volatile oil, add Arlacel-80 135g, stir evenly, add above-mentioned extract powder again and fully grind well, mixture is joined in the fused 36 type mixed aliphatic esters (60 ℃), adjust total amount to 2700g, mixing, moulding, take out the cooling back, makes 1000 pieces of bolts, promptly.
Embodiment three
[prescription] Fructus Cnidii 75g Flos Lonicerae 75g Fructus Gardeniae 75g Cortex Pseudolaricis 75g
Cortex Phellodendri 75g Radix Scutellariae 150g Radix Sophorae Flavescentis 75g Fructus Kochiae 75g
Herba Artemisiae Scopariae 75g Herba Menthae 150g Folium Artemisiae Argyi 75g Radix Angelicae Pubescentis 75g
Rhizoma Atractylodis 75g Rhizoma Acori Graminei 150g
[method for making] above 14 flavors are got Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis and are added 70% alcohol reflux secondary, and each 2 hours, collecting decoction filtered, and filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), and is standby; Get all the other medical materials and decoct with water secondary, each 2 hours, collect volatile oil simultaneously, collecting decoction filters, and filtrate is condensed into the clear paste of relative density about 1.18 (80 ℃), merges with above-mentioned concentrated extract, spray drying, it is standby that spray powder gets spray powder; With above-mentioned volatile oil, add Arlacel-80 135g, stir evenly, add above-mentioned extract powder again and fully grind well, mixture is joined in the fused 36 type mixed aliphatic esters (60 ℃), adjust total amount to 2700g, mixing, moulding, take out the cooling back, makes 1000 pieces of bolts, promptly.
[discriminating]
A. get 5 pieces of this product, chopping accurately takes by weighing 10g, puts in the apparatus,Soxhlet's, add petroleum ether 200ml, refluxed 3 hours, petroleum ether liquid discards, and residue takes out, cold wind dries up, and adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether extraction three times, each 20ml merges ether solution, volatilize, add methanol 1ml and make dissolving, as need testing solution; Other gets the osthole reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetate (30: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
B. get [discriminating] (a) down behind ether extraction surplus water liquid transfer pH2～3 with hydrochloric acid, with ethyl acetate extraction three times, 20ml at every turn, merge ethyl acetate liquid, extract three times, each 20ml with 5% sodium bicarbonate solution, merge alkali liquor, transfer pH2～3, with ethyl acetate extraction three times with hydrochloric acid, each 20ml, merge ethyl acetate liquid, be washed to neutrality, evaporate to dryness, residue adds methanol 5ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography test, draw each 0.5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with the upper solution of butyl acetate-formic acid-water (4: 2: 2), launch, take out, to dry, spray is with 2% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color
C. get [discriminating] (b) down behind ethyl acetate extraction surplus water liquid add ammonia and transfer pH9, extract three times with water-saturated n-butanol, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 2～3ml makes dissolving, is added on neutral alumina post (120～160 orders, 5g; Internal diameter 1.5cm), with 50% methanol-eluted fractions, collect eluent 50ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, (2: 3: 4: 0.2) be developing solvent, expansion was taken out with benzene-acetone-ethyl acetate-strong ammonia solution, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
D. get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds 1 of methanol 10ml, hydrochloric acid, shakes up, and supersound process 15 minutes filters, and filtrate is medical material liquid in contrast.Test according to thin layer chromatography, draw [discriminating] (c) each 2 μ l of need testing solution 5 μ l, reference substance and control medicinal material solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-isopropyl alcohol-methanol-water (6: 3: 1.5: 1.5: 0.3) is developing solvent, put in the expansion cylinder of ammonia saturated with vapor, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
E. get the jasminoidin reference substance in addition, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw [discriminating] (c) a following need testing solution and each 10 μ l of above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water (7: 1: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
[assay]
The assay of jasminoidin in 1 Fructus Gardeniae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (11: 89) is a mobile phase, and flow velocity is 1.0ml/min, 30 ℃ of column temperatures.Detect wavelength 238nm.Number of theoretical plate calculates by the jasminoidin peak should be not less than 5000.
The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 35 He with mobile phase, shakes up, promptly.
4 pieces of this product are got in the preparation of need testing solution, and 3.0g is got in chopping, and accurate the title decides, place apparatus,Soxhlet's, add petroleum ether (60 ℃～90 ℃) 200ml and refluxed the residue evaporate to dryness 3 hours, put in the tool plug conical flask, the accurate methanol 50ml that adds weighs, it is ultrasonic that (250W 50kHz) handled 30 minutes, put cold, weigh, supply the weight of loss, shake up with methanol, filter, get subsequent filtrate and filter, as need testing solution with microporous filter membrane (0.45 μ m).
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every piece of bolt of this product contains Fructus Gardeniae with jasminoidin (C
17H
24O
10) meter, must not be less than 0.75mg.
Every piece of bolt is 2.75g, is equivalent to crude drug 1.06g.
Content of baicalin is measured in 2 Radix Scutellariaes
Chromatographic condition and system suitability test are filler with octadecyl silane; Methanol-0.3% phosphoric acid solution (47: 53) is a mobile phase; 40 ℃ of column temperatures; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the baicalin peak.
It is an amount of that the baicalin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 50 μ g, promptly.
5 pieces of this product are got in the preparation of need testing solution, and chopping takes by weighing 1g, and accurate the title decides, put in the apparatus,Soxhlet's, add petroleum ether (60 ℃～90 ℃) 200ml, refluxed 3 hours, take out filtration paper cylinder, cold wind dries up, and precision adds methanol 50ml, claims to decide weight, (100W 50kHz), was cooled to room temperature to supersound extraction in 30 minutes, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate and filter, promptly with microporous filter membrane (0.45 μ m).
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
This product contains Radix Scutellariae with baicalin (C for every piece
21H
18O
11) meter, must not be less than 6.75mg.
Every piece of bolt is 2.75g, is equivalent to crude drug 1.06g.
Claims (8)
1. Chinese medicine composition is characterized in that this Chinese medicine composition is to be made by the crude drug of following weight ratio:
50～75 parts of 50～75 parts of Cortex Pseudolariciss of 50～75 portions of Fructus Gardeniaes of 50～75 portions of Flos Loniceraes of Fructus Cnidii
50～75 parts of 50～75 parts of Fructus Kochiae of 100～150 parts of Radix Sophorae Flavescentiss of 50～75 parts of Radix Scutellariaes of Cortex Phellodendri
50～75 parts of 50～75 parts of Radix Angelicae Pubescentiss of 100～150 portions of Folium Artemisiae Argyis of 50～75 portions of Herba Menthaes of Herba Artemisiae Scopariae
100～150 parts of 50～75 parts of Rhizoma Acori Graminei of Rhizoma Atractylodis
2. Chinese medicine composition as claimed in claim 1 is characterized in that the weight ratio of each crude drug is:
62.5 parts of 62.5 parts of Cortex Pseudolariciss of 62.5 portions of Fructus Gardeniaes of 62.5 portions of Flos Loniceraes of Fructus Cnidii
62.5 parts of 62.5 parts of Fructus Kochiae of 125 parts of Radix Sophorae Flavescentiss of 62.5 parts of Radix Scutellariaes of Cortex Phellodendri
62.5 parts of 62.5 parts of Radix Angelicae Pubescentiss of 125 portions of Folium Artemisiae Argyis of 62.5 portions of Herba Menthaes of Herba Artemisiae Scopariae
125 parts of 62.5 parts of Rhizoma Acori Graminei of Rhizoma Atractylodis
3. Chinese medicine composition as claimed in claim 1 or 2 is characterized in that said composition can be prepared into suppository.
4. the preparation method of the described Chinese medicine composition of claim 3 is characterized in that this method comprises the steps:
Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis add alcohol reflux in will writing out a prescription, and filtrate is condensed into clear paste, and be standby; Get all the other medical materials and decoct with water, collect volatile oil simultaneously, collecting decoction filters, and filtrate is condensed into clear paste, merges spray drying with above-mentioned concentrated extract; With spray powder, volatile oil, add conventional adjuvant and make suppository.
5. the preparation method of Chinese medicine composition as claimed in claim 4 is characterized in that this method comprises the steps:
Fructus Cnidii, Fructus Gardeniae, Cortex Phellodendri, Radix Scutellariae, Radix Sophorae Flavescentis add 70% alcohol reflux secondary in will writing out a prescription, and each 2 hours, collecting decoction filtered, and the clear paste of relative density 1.15～1.20 was standby when filtrate was condensed into 80 ℃; Get all the other medical materials and decoct with water secondary, each 2 hours, collect volatile oil simultaneously, collecting decoction filters the clear paste of relative density about 1.15～1.20 when filtrate is condensed into 80 ℃, merge with above-mentioned concentrated extract, spray drying adds conventional adjuvant with spray powder, volatile oil and makes suppository.
6. the method for quality control of the described Chinese medicine composition of claim 3 is characterized in that this method comprises one or more in the following qualitative identification:
A. get present composition preparation 5～10g, put in the apparatus,Soxhlet's, add petroleum ether 200ml, refluxed 3 hours, petroleum ether liquid discards, and residue takes out, cold wind dries up, and adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether extraction three times, each 20ml merges ether solution, volatilize, add methanol 1ml and make dissolving, as need testing solution; Other gets the osthole reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetates of 30: 1, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
B. get under the above-mentioned a item behind ether extraction surplus water liquid and transfer pH2～3 with hydrochloric acid, with ethyl acetate extraction three times, each 20ml, merge ethyl acetate liquid, extract three times, each 20ml with 5% sodium bicarbonate solution, merge alkali liquor, transfer pH2～3, with ethyl acetate extraction three times with hydrochloric acid, each 20ml, merge ethyl acetate liquid, be washed to neutrality, evaporate to dryness, residue adds methanol 5ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 0.5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with the upper solution of butyl acetate-formic acid of 4: 2: 2-water, launch, take out, to dry, spray is with 2% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
C. getting under the above-mentioned a item behind ethyl acetate extraction surplus water liquid adds ammonia and transfers pH9, extract three times with water-saturated n-butanol, each 20ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 2～3ml makes dissolving, is added on the neutral alumina post, with 50% methanol-eluted fractions, collect eluent 50ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with 2: 3: 4: benzene-acetone of 0.2-ethyl acetate-strong ammonia solution was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
D. get the berberine hydrochloride reference substance, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Other gets Cortex Phellodendri control medicinal material 0.1g, adds 1 of methanol 10ml, hydrochloric acid, shakes up, and supersound process 15 minutes filters, and filtrate is medical material liquid in contrast; Test according to thin layer chromatography, draw each 2 μ l of need testing solution 5 μ l, reference substance and control medicinal material solution under the above-mentioned c item, put respectively on same silica gel g thin-layer plate, with 6: 3: 1.5: benzene-ethyl acetate of 1.5: 0.3-isopropyl alcohol-methanol-water was developing solvent, put in the expansion cylinder of ammonia saturated with vapor, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
E. get the jasminoidin reference substance in addition, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution and each 10 μ l of above-mentioned reference substance solution under the above-mentioned c item, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid of 7: 1: 2-water is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ dry by the fire to the speckle colour developing clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
7. the method for quality control of Chinese medicine composition as claimed in claim 6, what it is characterized in that this method also comprises following quantitative approach:
A. the assay of osthole in the Fructus Cnidii
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 70: 30 methanol-water is a mobile phase, and the detection wavelength is 322nm, and number of theoretical plate is pressed the osthole peak and calculated, and should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing the osthole reference substance, and add neutral alcohol and make dissolving, and dilution, make the solution that contains 20 μ g among every 1ml, in contrast product solution;
The preparation precision of need testing solution is measured this product 5ml, add ammonia 0.25ml, mixing is put and is concentrated near doing in the hot bath, adding the small amount of ethanol dissolving also quantitatively is transferred in the 10ml measuring bottle, supersound process 10 minutes is put to room temperature, adds ethanol dilution to scale, shake up, filter, discard filtrate just, get subsequent filtrate as need testing solution;
Algoscopy precision is respectively measured reference substance solution and each 10～20 μ l of need testing solution, injects chromatograph of liquid, measures peak area, calculates with external standard method, promptly.
B. the assay of jasminoidin in the Fructus Gardeniae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 11: 89 acetonitrile-water is a mobile phase, and flow velocity is 1.0ml/min, and 30 ℃ of column temperatures detect wavelength 238nm, and number of theoretical plate calculates by the jasminoidin peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing the jasminoidin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 35 μ g with mobile phase, shakes up, promptly.
4 pieces of this product are got in the preparation of need testing solution, and 3.0g is got in chopping, the accurate title, decide, and places apparatus,Soxhlet's, adds petroleum ether 200ml and refluxed 3 hours, the residue evaporate to dryness is put in the tool plug conical flask, the accurate methanol 50ml that adds, weigh, supersound process 30 minutes is put cold, weigh, supply the weight of loss, shake up with methanol, filter, get subsequent filtrate and filter, as need testing solution with 0.45 μ m microporous filter membrane.
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
C. content of baicalin is measured in the Radix Scutellariae
Chromatographic condition and system suitability test are filler with octadecyl silane; 47: 53 methanol-0.3% phosphoric acid solution is a mobile phase; 40 ℃ of column temperatures; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the baicalin peak;
It is an amount of that the baicalin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 50 μ g, promptly;
5 pieces of this product are got in the preparation of need testing solution, and chopping takes by weighing 1g, and accurate the title decides, put in the apparatus,Soxhlet's, add petroleum ether 200ml, refluxed 3 hours, take out filtration paper cylinder, cold wind dries up, and precision adds methanol 50ml, claim to decide weight, supersound extraction 30 minutes is cooled to room temperature, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
8. Chinese medicine composition as claimed in claim 1 or 2 is in preparation treatment women damp-heat vaginal discharge, the application in mycotic, infusorian property and the nonspecific vaginitis medicine.
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