CN1806827A - 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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Abstract
The invention discloses a Chinese medicinal composition prepared from corktree bark, rhubarb horsetails, root of red rooted saliva, frankincense, myrrh, alkanna tinctoria, clam shell and borneol by a predetermined weight ratio. The composition can be used for treating colpitis mycotica or trichomonal vaginitis. The invention discloses the method for preparing the Chinese medicinal composition and its quality control method.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, belong to the field of Chinese medicines.
Background technology
Vaginitis is the inflammation of connective tissue under vaginal mucosa and the mucosa, is the common disease of gynecological's outpatient service.Vaginitis changes with the character of leucorrhea clinically and the pudendum infections is itched, and causalgia is main clinical characters, and common vaginitis has bacterial vaginitis, trichomonal vaginitis, colpitis mycotica, senile vaginitis.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.Suffer from diabetes, vitamin B group shortage, ovarian function decline in addition, some allergy or infectious disease person be easy infection more, the infective pathogen body often is mycete, antibacterial, mycoplasma, chlamydia etc., except that senile vaginitis, trichomonal vaginitis, colpitis mycotica sickness rate in recent years are on the rise.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 and treat Chinese medicine composition of using in damp heat downward flowing type colpitis mycotica or the trichomonal vaginitis medicine and preparation method thereof a kind of the preparation; 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:
At first be that prescription is formed, comprise following bulk drugs:
80～100 parts of 350～450 parts of Olibanums of 350～450 parts of Radix Salviae Miltiorrhizaes of 350～450 parts of Radix Et Rhizoma Rhei of Cortex Phellodendri
15～25 parts of 150～250 parts of Borneolum Syntheticums of 350～450 portions of Concha Meretricis Seu Cyclinaes of 80～100 portions of Radix Arnebiae (Radix Lithospermi)s of Myrrha
Further after the research, determine that its best group becomes:
90 parts of Cortex Phellodendri 400 parts of Radix Et Rhizoma Rhei, 400 parts of Olibanums of 400 parts of Radix Salviae Miltiorrhizaes (system)
20 parts of 200 parts of Borneolum Syntheticums of 400 portions of Concha Meretricis Seu Cyclinaes of 90 portions of Radix Arnebiae (Radix Lithospermi)s of Myrrha (processed)
Should write out a prescription, invention is thought can make clinical required various dosage forms, is preferably suppository.Be directed to this, the inventor has carried out technical study again.In order to make suppository, must earlier former prescription be extracted refiningly, its process is as follows:
Get Concha Meretricis Seu Cyclinae powder and be broken into fine powder, standby; Cortex Phellodendri, Radix Et Rhizoma Rhei be with 70% alcohol reflux three times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, filter, merging filtrate is evaporated to relative density and is 1.12～1.15 (50 ℃), and is standby.Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae ethanol warm macerating (40～45 ℃) three times, 3 days for the first time, second and third time each 2 days filtered, and merging filtrate is evaporated to relative density and is 1.12～1.15 (40 ℃), and is standby.Olibanum, Myrrha distillating extracting oil, aqueous solution filters, and medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, being evaporated to relative density is the thick paste of 1.30～1.35 (50 ℃), add above-mentioned fine powder, mixing, oven drying at low temperature is pulverized, powder gets dry extract, add the volatile oil and the Borneolum Syntheticum of beta-schardinger dextrin-inclusion, mixing obtains pharmaceutical intermediate.
Further research, find also can realize with following process conditions:
Get Concha Meretricis Seu Cyclinae powder and be broken into fine powder, standby; Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae be with 70% alcohol reflux secondary, and each 2 hours, filter, merging filtrate is evaporated to relative density and is 1.12～1.15 (50 ℃), and is standby.Olibanum, Myrrha distillating extracting oil, aqueous solution filters, and medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, being evaporated to relative density is the thick paste of 1.30～1.35 (50 ℃), add above-mentioned fine powder, mixing, oven drying at low temperature is pulverized, powder gets dry extract, add the volatile oil and the Borneolum Syntheticum of beta-schardinger dextrin-inclusion, mixing obtains pharmaceutical intermediate.
In order to last any intermediate, be equipped with suitable adjuvant, just can be pressed into suppository.
In order effectively to control the quality of product of the present invention, the inventor has also formulated method of quality control, comprises qualitative identification and assay two parts, discusses respectively below.
Qualitative identification has partly comprised following several:
A. get present composition preparation 5～10g, the 20ml that adds methylene chloride makes dissolving, adds ethanol 10ml, stir evenly, add methanol 300ml, jolting 20 minutes, freezing 1 hour, filter the filtrate evaporate to dryness, residue adds 20ml hot water makes dissolving, with ether extraction three times, and each 20ml, merge ether solution, with 1% sodium hydroxide extraction three times, 20ml at every turn, merge alkali liquor, standby; Surplus ether solution volatilizes, and adds methanol 5ml and makes dissolving, as need testing solution; Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetate (19: 1), launch, take out, dry, with the corresponding position of reference substance chromatograph on, the speckle of apparent same color.
B. get the alkali liquor under the above-mentioned a item, add hydrochloric acid and transfer pH4～5, with ether extraction three times, each 20ml merges ether solution, volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution; Other gets the Shikonin reference substance, adds ethanol and makes the solution that every 1ml contains 0.1mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (60 ℃～90 ℃)-ethyl acetate-formic acid (15: 3: 1) is developing solvent, launches, and takes out, dry, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
C. get emodin and chrysophanol reference substance in addition, chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography, draw each the 2 μ l of need testing solution, emodin and chrysophanol reference substance solution under the above-mentioned discriminating b item, putting respectively on same silica gel g thin-layer plate, is developing solvent with the upper solution of petroleum ether (60 ℃～90 ℃)-ethyl acetate-formic acid (15: 3: 1), launches, take out, dry, put under the visible light and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
D. get present composition preparation 5～10g, carry out microsublimation, sublimate adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum control medicinal material 20mg, adds ethanol 2ml and makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, draw need testing solution 2～5 μ l, control medicinal material solution 1 μ l, put respectively on same silica gel g thin-layer plate, so that petroleum ether (60 ℃～90 ℃)-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Content assaying method is as follows:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 0.1% phosphoric acid solution (25: 75) of acetonitrile-0.05mol/L potassium dihydrogen phosphate is a mobile phase; Detect wavelength 265nm.Number of theoretical plate should be not less than 2000 by the berberine hydrochloride peak.
It is an amount of that the berberine hydrochloride reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 30 μ g, promptly.
Present composition preparation 1～2g is got in the preparation of need testing solution, and accurate the title decides, and puts in the apparatus,Soxhlet's, extracts 3 hours with petroleum ether 200ml, and petroleum ether liquid discards; Take out filter paper packet, cold wind dries up, and puts in the conical flask, precision adds 1% hydrochloric acid methanol 50ml, claims to decide weight, supersound process 30 minutes, supply bodies lost weight with 1% hydrochloric acid methanol, filter, get subsequent filtrate 25ml, evaporate to dryness adds water 15ml and makes dissolving, with ether extraction three times, each 20ml, ether solution discards, surplus water liquid evaporate to dryness, add methanol 2～5ml and make dissolving, be added on the neutral alumina post,, collect eluent 50ml mixing with methanol-eluted fractions, the accurate 25ml that draws, evaporate to dryness, residue add the mutual-assistance dissolving of flowing, and quantitatively are transferred in the l0ml volumetric flask, filter with 0.45 μ m microporous filter membrane, promptly.
Accurate respectively reference substance and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This composite preparation per unit amount contains Cortex Phellodendri with berberine hydrochloride (C
20H
17NO
4HCl) meter must not be less than 2.0mg.
Above-mentioned unit quantity is meant the finished medicines dosage that contains suitable 2g crude drug.
The specific embodiment:
Pharmaceutical preparation of the present invention has the function of heat clearing and damp drying, killing parasites for relieving itching, can be used for the treatment of damp heat downward flowing type colpitis mycotica, trichomonal vaginitis.The inventor cures mainly according to its function, from aspects such as antiinflammatory, anti-trichomonas vaginitises its pharmacodynamics is verified.
Be subjected to the reagent thing: No. 1,2, the preparation that makes according to two kinds of different process of optimal proportion of the present invention, contain the 2g crude drug/piece suppository.
FUYANXIAO PAOTENGPIAN: Guangzhou Zhongyi Medicine Industry Co., Ltd produces, lot number: 20030418.
Instrument: PB303-N electronic balance, Mettler-Toledo Instrument (Shanghai) Co., Ltd..
Animal: Kunming mouse 18～22g, the male and female dual-purpose is provided by Shandong University's Experimental Animal Center.
Test 1: the influence of xylol induced mice auricular concha swelling
Get 40 of mices, male and female half and half, be divided into four groups at random, subcutaneous injection this product preparation and positive drug, behind the 4th day administration 1h left auricular concha melted paraxylene 0.02ml/ only, the 30min execution that dislocates, cut two ears with shears along the auricle baseline of mice, perforator at same position with 0.6cm sweeps away auricle, and two auricles are weighed and asked poor, the results are shown in Table 1.
The influence of table 1 xylol induced mice auricular concha swelling (X ± S)
| Group | Dosage ml | Number of animals/only | Two auricles weight difference/μ g |
| The blank group | 10 | 2.00±0.66 | |
| This product preparation 1 | 10 | 1.20±0.41* | |
| This product preparation 2 | 10 | 1.30±0.17* | |
| The positive drug group | 10 | 1.36±0.20* |
Annotate: compare * P＜0.05 with matched group, * * P＜0.01
Table 1 is the result show, this product preparation has remarkable inhibitory action to mice auricular concha inflammation.
Test 2: external trichomonas vaginitis effect extremely
Separate from patient's vaginal secretions, be inoculated in the liver-peptone-sugar culture-medium that contains penicillin and streptomycin, every 4d transferred species 1 time is inoculated 4 times repeatedly, and counting makes when the infusorian number reaches 10,000/ml in the culture fluid, is for experiment.Culture medium is divided 4 groups, medicine carries out the two-fold dilution, in every pipe liver-peptone-sugar culture-medium, add 0.1ml trichomonal vaginitis culture fluid then, in 37 ℃ of following continuous culture 3d (under optical microscope, observing 1 time the infusorian active situation every day), 3d, every pipe is got the 0.1ml culture fluid, observes trichomonas vaginitis quantity and death condition, the results are shown in Table 2.
The effect of the external infusorian extremely of table 2
| Group | The medicinal liquid extension rate | |||||
| 1∶32 | 1∶16 | 1∶8 | 1∶4 | 1∶2 | 1∶1 | |
| The blank group | + | + | + | + | + | + |
| This product preparation 1 | + | + | + | - | - | - |
| This product preparation 2 | + | + | + | - | - | - |
| The positive drug group | + | + | + | + | - | - |
Annotate :+trichomonas vaginitis motion, active, cell is glossy, and infusorian quantity increases;-trichomonas vaginitis is in heaven, can not move cell tarnish, the cracking of part polypide.
Table 2 result shows that this product preparation has killing action to trichomonas vaginitis, and the medicinal liquid extension rate is visible infusorian death in 1: 4 o'clock, the cracking of part polypide.
Test 3: extracorporeal bacteria inhibitor test
This product preparation water proof is in 80 ℃ of water-bath sterilization 2h, and in the meat soup blood serum medium, in 37 ℃ of following continuous culture 18h, the bacterium number reaches 900,000,000/ml in the bacterium liquid with above-mentioned bacterial classification inoculation, gets broth bouillon and is diluted to 900,000/ml, uses for experiment.Candida albicans increases bacterium to be cultivated when reaching 5,000,000/ml, takes out and is diluted to 50,000/ml, standby.Make the training ware with chocolate blood meida, broth agar culture medium, blood agar culture-medium, sabouraud culture medium respectively, in the dish pipe of each bacterial strain training ware, add preparation, cultivate, survey inhibition zone behind 37 ℃ of following 18h, the result is the strongest to the streptococcus inhibitory action, and inferior is Candida albicans, sees Table 3.
Table 3 pair Candida albicans etc. suppress effect
| Strain name | Inhibition zone (mm) | |
| This product preparation 1 | This product preparation 2 | |
| Gold Portugal bacterium | 16.3±0.5 | 16.1±0.7 |
| Escherichia coli | 9.7±0.5 | 9.5±0.5 |
| Bacillus proteus | 10.0±0.8 | 9.8±0.4 |
| Streptococcus | 21.0±0.8 | 21.6±0.9 |
| Gonococcus | 11.7±0.5 | 11.4±0.5 |
| Read bacterium in vain | 20.0±0.8 | 20.5±0.6 |
Result of the test shows: this product preparation is external to have certain inhibitory action to Candida albicans.
Further specify technical scheme of the present invention below by embodiment:
Embodiment one
[prescription] Cortex Phellodendri 350g Radix Et Rhizoma Rhei 350g Radix Salviae Miltiorrhizae 350g Olibanum 80g
Myrrha 80g Radix Arnebiae (Radix Lithospermi) 350g Concha Meretricis Seu Cyclinae 150g Borneolum Syntheticum 15g
[method for making] above eight flavors are got Concha Meretricis Seu Cyclinae powder and are broken into fine powder, and are standby; Cortex Phellodendri, Radix Et Rhizoma Rhei are measured 70% alcohol reflux three times with 8 times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, filter, merging filtrate is evaporated to relative density and is 1.20～1.25 (50 ℃), and is standby.Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae are measured ethanol warm macerating (40～45 ℃) three times with 10 times, and 3 days for the first time, second and third time each 2 days filtered, and merging filtrate is evaporated to relative density and is 1.20～1.25 (50 ℃), and is standby.Olibanum, Myrrha add 8 times of water gagings, and distillation extraction 6 hours is collected volatile oil, and aqueous solution filters, and medicinal residues add 8 times of water gagings again and decocted 1.5 hours, filter, and filtrate merges, and is evaporated to relative density and is 1.20～1.25 (50 ℃), and is standby.With above-mentioned three parts of concentrated back clear paste, merge, being evaporated to relative density again is the thick paste of 1.30～1.35 (50 ℃), adds above-mentioned fine powder, mixing, drying under reduced pressure is pulverized, and powder gets dry extract.Volatile oil and Borneolum Syntheticum are added the small amount of ethanol dissolving, join in the lump in the fused 36 type mixed aliphatic esters with above-mentioned dried cream powder, mixing is made 2750g, moulding, and take out the cooling back, makes 1000 pieces of bolts, promptly.
Embodiment two
[prescription] Cortex Phellodendri 450g Radix Et Rhizoma Rhei 450g Radix Salviae Miltiorrhizae 450g Olibanum (system) 100g
Myrrha (processed) 100g Radix Arnebiae (Radix Lithospermi) 450g Concha Meretricis Seu Cyclinae 250g Borneolum Syntheticum 25g
[method for making] above eight flavors are got Concha Meretricis Seu Cyclinae powder and are broken into fine powder, and are standby; Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae be with 70% alcohol reflux secondary, and each 2 hours, filter, merging filtrate is evaporated to relative density and is 1.12～1.15 (50 ℃), and is standby.Olibanum, Myrrha distillating extracting oil, aqueous solution filters, medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, being evaporated to relative density is the thick paste of 1.30～1.35 (50 ℃), add above-mentioned fine powder, mixing, oven drying at low temperature, pulverize, the powder that gets dry extract adds the small amount of ethanol dissolving with volatile oil and Borneolum Syntheticum, joins in the lump in the fused 36 type mixed aliphatic esters with above-mentioned dried cream powder, mixing, make 2750g, moulding, take out the cooling back, make 1000 pieces of bolts, promptly.
Embodiment three
[prescription] Cortex Phellodendri 400g Radix Et Rhizoma Rhei 400g Radix Salviae Miltiorrhizae 400g Olibanum 90g
Myrrha 90g Radix Arnebiae (Radix Lithospermi) 400g Concha Meretricis Seu Cyclinae 200g Borneolum Syntheticum 20g
[method for making] above eight flavors are got Concha Meretricis Seu Cyclinae powder and are broken into fine powder, and are standby; Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae be with 70% alcohol reflux secondary, and each 2 hours, filter, merging filtrate is evaporated to relative density and is 1.12～1.15 (50 ℃), and is standby.Olibanum, Myrrha distillating extracting oil, aqueous solution filters, medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, being evaporated to relative density is the thick paste of 1.30～1.35 (50 ℃), add above-mentioned fine powder, mixing, oven drying at low temperature, pulverize, the powder that gets dry extract adds the small amount of ethanol dissolving with volatile oil and Borneolum Syntheticum, joins in the lump in the fused 36 type mixed aliphatic esters with above-mentioned dried cream powder, mixing, make 2750g, moulding, take out the cooling back, make 1000 pieces of bolts, promptly.
[discriminating]
A. get 5 pieces of this product, chopping accurately takes by weighing 8g, and the 20ml that adds methylene chloride makes dissolving, add ethanol 10ml, stir evenly, add methanol 300ml, jolting 20 minutes freezing 1 hour, filters, filtrate evaporate to dryness, residue add 20ml hot water makes dissolving, with ether extraction three times, each 20ml merges ether solution, with 1% sodium hydroxide extraction three times, each 20ml merges alkali liquor, and is standby; Surplus ether solution volatilizes, and adds methanol 5ml and makes dissolving, as need testing solution; Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetate (19: 1), launch, take out, dry, with the corresponding position of reference substance chromatograph on, the speckle of apparent same color.
B. get [discriminating] (a) following alkali liquor, add hydrochloric acid and transfer pH4～5, with ether extraction three times, each 20ml, the merging ether solution volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution; Other gets the Shikonin reference substance, adds ethanol and makes the solution that every 1ml contains 0.1mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether (60 ℃～90 ℃)-ethyl acetate-formic acid (15: 3: 1) is developing solvent, launches, and takes out, dry, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
C. get emodin and chrysophanol reference substance in addition, chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography, draw each the 2 μ l of need testing solution, emodin and chrysophanol reference substance solution under above-mentioned [discriminating] (2) item, putting respectively on same silica gel g thin-layer plate, is developing solvent with the upper solution of petroleum ether (60 ℃～90 ℃)-ethyl acetate-formic acid (15: 3: 1), launches, take out, dry, put under the visible light and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
D. get 5 pieces of this product, chopping accurately takes by weighing 8g, carries out microsublimation, and sublimate adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum control medicinal material 20mg, adds ethanol 2ml and makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, draw need testing solution 2～5 μ l, control medicinal material solution 1 μ l, put respectively on same silica gel g thin-layer plate, so that petroleum ether (60 ℃～90 ℃)-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
A. the test of chromatographic condition and system suitability is a filler with octadecylsilane chemically bonded silica; 0.1% phosphoric acid solution (25: 75) of acetonitrile-0.05mol/L potassium dihydrogen phosphate is a mobile phase; Detect wavelength 265nm.Number of theoretical plate should be not less than 2000 by the berberine hydrochloride peak.
B. it is an amount of that the berberine hydrochloride reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 30 μ g, promptly.
C. 5 pieces of this product are got in the preparation of need testing solution, chopping, and mixing takes by weighing 1g, and accurate the title, decide, and puts in the apparatus,Soxhlet's, extracted 3 hours with petroleum ether (60 ℃～90 ℃) 200ml, and petroleum ether liquid discards; Take out filter paper packet, cold wind dries up, and puts in the conical flask, precision adds 1% hydrochloric acid methanol 50ml, claims to decide weight, ultrasonic (250W, 20kHz) handled 30 minutes, supply bodies lost weight, filter with 1% hydrochloric acid methanol, get subsequent filtrate 25ml, evaporate to dryness adds water 15ml and makes dissolving, with ether extraction three times, each 20ml, ether solution discards, surplus water liquid evaporate to dryness adds methanol 2～5ml and makes dissolving, is added on neutral alumina post (5g, 120～160 orders, the wet method upper prop, d=1.5cm), with methanol-eluted fractions, collect eluent 50ml mixing, the accurate 25ml that draws, evaporate to dryness, residue add the mutual-assistance dissolving of flowing, and quantitatively are transferred in the 10ml volumetric flask, filter with 0.45 μ m microporous filter membrane, promptly.
D. accurate respectively reference substance and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This product contains Cortex Phellodendri with berberine hydrochloride (C for every piece
20H
17NO
4HCl) meter must not be less than 2.0mg.
Every piece of bolt is 2.75g, is equivalent to crude drug 2g.
Claims (9)
1. Chinese medicine composition is characterized in that this pharmaceutical composition made by following raw material medicaments:
80～100 parts of 350～450 parts of Olibanums of 350～450 parts of Radix Salviae Miltiorrhizaes of 350～450 parts of Radix Et Rhizoma Rhei of Cortex Phellodendri
15～25 parts of 150～250 parts of Borneolum Syntheticums of 350～450 portions of Concha Meretricis Seu Cyclinaes of 80～100 portions of Radix Arnebiae (Radix Lithospermi)s of Myrrha
2. Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw materials according:
90 parts of 400 parts of Olibanums of 400 parts of Radix Salviae Miltiorrhizaes of 400 parts of Radix Et Rhizoma Rhei of Cortex Phellodendri
20 parts of 200 parts of Borneolum Syntheticums of 400 portions of Concha Meretricis Seu Cyclinaes of 90 portions of Radix Arnebiae (Radix Lithospermi)s of Myrrha
3. Chinese medicine composition as claimed in claim 1 or 2 is characterized in that Olibanum and the Myrrha in the crude drug is respectively Olibanum (processed) and Myrrha (processed).
4. Chinese medicine composition as claimed in claim 3 is characterized in that said composition can be made into clinical required various dosage forms, comprises suppository and lotion.
5. the preparation method of the described Chinese medicine composition suppository of claim 4 is characterized in that this method has comprised any in following two kinds of processing steps:
1) get Concha Meretricis Seu Cyclinae powder and be broken into fine powder, standby; Cortex Phellodendri, Radix Et Rhizoma Rhei be with 70% alcohol reflux three times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, filter, merging filtrate, relative density is 1.12～1.15 when being evaporated to 50 ℃, and is standby; Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae ethanol warm macerating three times, 3 days for the first time, second and third time each 2 days filtered, merging filtrate, relative density is 1.12～1.15 when being evaporated to 40 ℃, and is standby; Olibanum, Myrrha distillating extracting oil, aqueous solution filters, and medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, relative density is 1.30～1.35 thick paste when being evaporated to 50 ℃, add above-mentioned fine powder, mixing, oven drying at low temperature is pulverized, powder gets dry extract, add the volatile oil and the Borneolum Syntheticum of beta-schardinger dextrin-inclusion, mixing makes pharmaceutical intermediate;
2) get Concha Meretricis Seu Cyclinae powder and be broken into fine powder, standby; Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Salviae Miltiorrhizae be with 70% alcohol reflux secondary, and each 2 hours, filter, merging filtrate, relative density is 1.12～1.15 () when being evaporated to 50 ℃, and is standby; Olibanum, Myrrha distillating extracting oil, aqueous solution filters, and medicinal residues decoct with water 1.5 hours again, filter, after twice filtrate and the merging of above-mentioned concentrated solution, relative density is 1.30～1.35 thick paste when being evaporated to 50 ℃, add above-mentioned fine powder, mixing, oven drying at low temperature is pulverized, powder gets dry extract, add the volatile oil and the Borneolum Syntheticum of beta-schardinger dextrin-inclusion, mixing makes pharmaceutical intermediate.
6. the preparation method of suppository as claimed in claim 5 is characterized in that the pharmaceutical intermediate that two kinds of methods make all can add corresponding auxiliary material, makes suppository.
7. the method for quality control of claim 5 or 6 described Chinese medicine composition suppositorys, the qualitative identification method that it is characterized in that this method comprise following one or more:
A. get present composition preparation 5～10g, the 20ml that adds methylene chloride makes dissolving, adds ethanol 10ml, stir evenly, add methanol 300ml, jolting 20 minutes, freezing 1 hour, filter the filtrate evaporate to dryness, residue adds 20ml hot water makes dissolving, with ether extraction three times, and each 20ml, merge ether solution, with 1% sodium hydroxide extraction three times, 20ml at every turn, merge alkali liquor, standby; Surplus ether solution volatilizes, and adds methanol 5ml and makes dissolving, as need testing solution; Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetates of 19: 1, launch, take out, dry, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B. get the alkali liquor under the above-mentioned a item, add hydrochloric acid and transfer pH4～5, with ether extraction three times, each 20ml merges ether solution, volatilizes, and residue adds methanol 2ml makes dissolving, as need testing solution; Other gets the Shikonin reference substance, adds ethanol and makes the solution that every 1ml contains 0.1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 2 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper solution with petroleum ether-ethyl acetates of 15: 3: 1-formic acid is developing solvent, launches, and takes out, dry, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get emodin and chrysophanol reference substance in addition, chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each the 2 μ l of need testing solution, emodin and chrysophanol reference substance solution under the above-mentioned discriminating b item, putting respectively on same silica gel g thin-layer plate, is developing solvent with the upper solution of petroleum ether-ethyl acetates of 15: 3: 1-formic acid, launches, take out, dry, put under the visible light and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D. get present composition preparation 5～10g, carry out microsublimation, sublimate adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other gets Borneolum Syntheticum control medicinal material 20mg, adds ethanol 2ml and makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw need testing solution 2～5 μ l, control medicinal material solution 1 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetates of 9: 1 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
8. the method for quality control of suppository as claimed in claim 7 is characterized in that this method comprises following quantitative approach:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 0.1% phosphoric acid solution of 25: 75 acetonitrile-0.05mol/L potassium dihydrogen phosphate is a mobile phase; Detect wavelength 265nm; Number of theoretical plate should be not less than 2000 by the berberine hydrochloride peak;
It is an amount of that the berberine hydrochloride reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 30 μ g, promptly;
Present composition preparation 1～2g is got in the preparation of need testing solution, and accurate the title decides, and puts in the apparatus,Soxhlet's, extracts 3 hours with petroleum ether 200ml, and petroleum ether liquid discards; Take out filter paper packet, cold wind dries up, and puts in the conical flask, precision adds 1% hydrochloric acid methanol 50ml, claims to decide weight, supersound process 30 minutes, supply bodies lost weight with 1% hydrochloric acid methanol, filter, get subsequent filtrate 25ml, evaporate to dryness adds water 15ml and makes dissolving, with ether extraction three times, each 20ml, ether solution discards, surplus water liquid evaporate to dryness, add methanol 2～5ml and make dissolving, be added on the neutral alumina post,, collect eluent 50ml mixing with methanol-eluted fractions, the accurate 25ml that draws, evaporate to dryness, residue add the mutual-assistance dissolving of flowing, and quantitatively are transferred in the 10ml volumetric flask, filter with 0.45 μ m microporous filter membrane, promptly.
Accurate respectively reference substance and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
9. as claim 1, the application of 2 or 3 described Chinese medicine compositions in preparation treatment damp heat downward flowing type colpitis mycotica or trichomonal vaginitis medicine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872256A (en) * | 2012-09-13 | 2013-01-16 | 顾洪 | Treatment type vagina gel and preparation method thereof |
| CN110333305A (en) * | 2019-06-30 | 2019-10-15 | 广西万寿堂药业有限公司 | The detection method of content of gynaecologic leucorrhea removing Chinese medicine composition |
| CN111714568A (en) * | 2019-10-24 | 2020-09-29 | 贵州益佰女子大药厂有限责任公司 | Preparation method of Fuyanxiao preparation |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1055297A (en) * | 1991-03-28 | 1991-10-16 | 许聿祥 | A kind of autofrettage of skin-moistening burn and scald medicine |
| CN1204516A (en) * | 1997-07-07 | 1999-01-13 | 刘明锁 | Burns oil and method for preparation thereof |
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2005
- 2005-01-19 CN CN2005102000469A patent/CN1806827B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872256A (en) * | 2012-09-13 | 2013-01-16 | 顾洪 | Treatment type vagina gel and preparation method thereof |
| CN110333305A (en) * | 2019-06-30 | 2019-10-15 | 广西万寿堂药业有限公司 | The detection method of content of gynaecologic leucorrhea removing Chinese medicine composition |
| CN111714568A (en) * | 2019-10-24 | 2020-09-29 | 贵州益佰女子大药厂有限责任公司 | Preparation method of Fuyanxiao preparation |
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