CN101524433B - Analytical method of gynecological inflammation clearance tablet - Google Patents
Analytical method of gynecological inflammation clearance tablet Download PDFInfo
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Abstract
The invention belongs to the technical field of traditional Chinese medicine, more specifically discloses an analytical method of a gynecological inflammation clearance tablet. The embodiment of the method can improve content accuracy of each component in the gynecological inflammation clearance tablet and product quality.
Description
[technical field]
The invention belongs to the traditional Chinese medicine technology technical field, be specifically related to a kind of analytical approach of gynecological inflammation clearance tablet.
[background technology]
Gynecological inflammation clearance tablet is to be guidance with the traditional Chinese medical theory, by meticulous preparation, is made up of through seat, persimmon leaf bitter radix scrophulariae, elephants-foot, Radix Angelicae Sinensis, reticulate millettia, Radix zanthoxyli, Thlaspi, radix fici simplicissimae, horizontal stroke, and its function is treatment clearing heat and expelling damp, adjusting meridian and stopping leukorrhea.Be used for the irregular menstruation due to the damp-heat accumulation, dysmenorrhoea; Adnexitis, pelvic infecton, cards such as endometritis are one of gynaecology's essential drugses commonly used.
The basic prescription of gynecological inflammation clearance tablet is:
The bitter radix scrophulariae 250g of Radix Angelicae Sinensis 250g reticulate millettia 375g
Elephants-foot 375g Thlaspi 375g radix fici simplicissimae 500g
Horizontal in seat 375g Radix zanthoxyli 375g persimmon leaf 375g
The method for making of gynecological inflammation clearance tablet is: above nine flavors, and bitter radix scrophulariae 125g is ground into fine powder, twice of eight flavor medicinal material boiling such as remaining bitter radix scrophulariae and Radix Angelicae Sinensis, 3 hours for the first time, 2 hours for the second time, collecting decoction, filter, filtrate is condensed into the thick paste shape, adds bitter radix scrophulariae fine powder, mixing, drying is pulverized, be pressed into 1000, dressing, packing, namely.This product is Film coated tablets, removes to show sepia behind the film-coating; The little perfume (or spice) of gas, bitter.
The main application of gynecological inflammation clearance tablet is a large amount of audients' such as Urban Women white collar, climacteric women and the women of child-bearing age medicine, thereby need provide and can guarantee pharmaceutical effectiveness, also needs and can medicine analytical approach accurate, easy, easy row ensure drug quality.
Simultaneously, the detection of traditional Chinese compound medicine often uses analytical equipments such as chromatography of gases and liquid chromatography, during check fee, effort, expensive, based on these problems, also needs to provide a kind of or analytical approach that a class is simple and efficient is determined the true and false of medicine.
For the check of workshop medicine finished product and tablet, also need to establish its analytical approach simultaneously, guarantee the quality of medicine.
[summary of the invention]
The object of the present invention is to provide a kind of analytical approach of gynecological inflammation clearance tablet.The analytical approach of gynecological inflammation clearance tablet of the present invention is simple and easy to do, and is convenient and swift, and the rapid true and false of differentiating medicine of energy is a kind of analytical approach that basic unit promotes that is suitable for tersely.
Particularly, the analytical approach of gynecological inflammation clearance tablet of the present invention, adopt following method: get 3 of this product, porphyrize adds ethanol 10ml, puts in the water-bath and heats 5 minutes, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets bitter radix scrophulariae control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with methenyl choloride-methyl alcohol (4: 1), launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, about 5 minutes of 105 ℃ of heating.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Said method can also further be analyzed: get 5 of this product, porphyrize is put in the mortar, adds ethanol 20ml, grinds 2 minutes, filters, and filtrate evaporate to dryness, residue add methenyl choloride 1ml makes dissolving, as need testing solution.Other gets Radix zanthoxyli control medicinal material 1.9g, and boiling 20 minutes filters, and filtrate is concentrated into dried, adds ethanol and makes dissolving in right amount, filters, and filtrate evaporate to dryness, residue add methenyl choloride 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-methenyl choloride (1: 3), with ammoniacal liquor saturated 30 minutes, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Said method can also further be analyzed: get 12 of this product, porphyrize adds water 50ml and makes dissolving, extracts 2 times with the ether jolting, and each 40ml merges ether solution, and evaporate to dryness, the residue 2ml that adds diethyl ether makes dissolving, as need testing solution.Other gets elephants-foot 3.2g, add water 50ml, decocted 1 hour, and filtered, it is 45% to containing the alcohol amount that filtrate adds ethanol, leave standstill, filter, evaporate to dryness, residue add water 50ml, shine medicinal material solution in pairs with legal system, according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with toluene-absolute ethyl alcohol (30: 1.5), launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with 1% aluminium choride ethanolic solution.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Said method can also further be analyzed: the test of chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.05mol/L triethylamine (30: 70) (with phosphoric acid adjust pH to 2.40) is the phase that flows; The detection wavelength is 328nm.Number of theoretical plate calculates by the Nitidine Chloride peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Nitidine Chloride reference substance, adds methyl alcohol and make the solution that every 1ml contains 4 μ g, namely;
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got the about 2.0g of powder, the accurate title, decide, and puts in the 50ml tool plug conical flask, adds 0.1mol/L hydrochloric acid 20ml, ultrasonic processing (power is 160W, frequency 40KHz) 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake with 0.1mol/L hydrochloric acid, change in the separating funnel, extract 3 times each 20ml, water intaking liquid ammonia solution adjust pH to 9～10 with the methenyl choloride jolting, extract 3 times with the methenyl choloride jolting again, each 20ml merges methenyl choloride liquid, evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 25ml measuring bottle, be diluted to scale with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 10ml, put in the 25ml measuring bottle, be diluted to scale with methyl alcohol, shake up, filter, get subsequent filtrate as need testing solution;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures, that is, every of this product contains Radix zanthoxyli in Nitidine Chloride, must not be less than 45ug.
The present invention adopts fast and convenient one or more thin-layered chromatography or liquid phase chromatography, and independence or combine and carry out the analyzing and testing of gynecological inflammation clearance tablet agent is the safety of such medicine separately, and guarantee effectively is provided.
[embodiment]
Following embodiment further describes the present invention, but described embodiment only is used for explanation the present invention rather than restriction the present invention.Following examples are all got the gynecological inflammation clearance tablet agent of 3 lot numbers, and lot number is respectively 080926-1,080917-2 and 081002.
Embodiment 1
Get each 3 of 3 lot number this product, porphyrize adds ethanol 10ml, puts in the water-bath and heats 5 minutes, filters, and filtrate evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.Other gets bitter radix scrophulariae control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with methenyl choloride-methyl alcohol (4: 1), launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, about 5 minutes of 105 ℃ of heating.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Embodiment 2
Get each 5 of 3 lot number this product, porphyrize is put in the mortar, adds ethanol 20ml, grinds 2 minutes, filters, and filtrate evaporate to dryness, residue add methenyl choloride 1ml makes dissolving, as need testing solution.Other gets Radix zanthoxyli control medicinal material 1.9g, and boiling 20 minutes filters, and filtrate is concentrated into dried, adds ethanol and makes dissolving in right amount, filters, and filtrate evaporate to dryness, residue add methenyl choloride 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-methenyl choloride (1: 3), with ammoniacal liquor saturated 30 minutes, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Embodiment 3
Get each 12 of 3 lot number this product, porphyrize adds water 50ml and makes dissolving, extracts 2 times with the ether jolting, and each 40ml merges ether solution, and evaporate to dryness, the residue 2ml that adds diethyl ether makes dissolving, as need testing solution.Other gets elephants-foot 3.2g, adds water 50ml, decocts 1 hour, filters, and it is 45% to containing the alcohol amount that filtrate adds ethanol, leaves standstill, and filters, and evaporate to dryness, residue add water 50ml, shine medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with toluene-absolute ethyl alcohol (30: 1.5), launch, take out, dry, spray is put under the ultraviolet lamp (365nm) and is inspected with 1% aluminium choride ethanolic solution.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Embodiment 4
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.05mol/L triethylamine (30: 70) (with phosphoric acid adjust pH to 2.40) is the phase that flows; The detection wavelength is 328nm.Number of theoretical plate calculates by the Nitidine Chloride peak should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the Nitidine Chloride reference substance, adds methyl alcohol and make the solution that every 1ml contains 4 μ g, namely.
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got the about 2.0g of powder, the accurate title, decide, and puts in the 50ml tool plug conical flask, adds 0.1mol/L hydrochloric acid 20ml, ultrasonic processing (power is 160W, frequency 40KHz) 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake with 0.1mol/L hydrochloric acid, change in the separating funnel, extract 3 times each 20ml, water intaking liquid ammonia solution adjust pH to 9～10 with the methenyl choloride jolting, extract 3 times with the methenyl choloride jolting again, each 20ml merges methenyl choloride liquid, evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 25ml measuring bottle, be diluted to scale with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 10ml, put in the 25ml measuring bottle, be diluted to scale with methyl alcohol, shake up, filter, get subsequent filtrate as need testing solution.
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures, namely.
Every of gained this product contains Radix zanthoxyli with Nitidine Chloride (C
21H
19NO
4Cl) meter is respectively 48.1 (080926-1), 48.7 (080917-2) and 47.2 (081002-1) ug.
Claims (1)
1. the analytical approach of a gynecological inflammation clearance tablet is characterized in that, adopts following methods analyst: get 3 of this product, porphyrize adds 10 milliliters of ethanol, puts in the water-bath and heats 5 minutes, filters, and filtrate evaporate to dryness, residue add ethanol makes dissolving for 1 milliliter, as need testing solution; Other gets bitter radix scrophulariae control medicinal material 1g, shines medicinal material solution in pairs with legal system; According to thin-layered chromatography test, draw each 10 microlitre of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, launch with methenyl choloride and the methyl alcohol developping agent according to preparation in 4: 1, take out, to dry, spray is with 5% vanillic aldehyde sulfuric acid solution, 105 ℃ of heating 5 minutes; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
Get 5 of this product, porphyrize is put in the mortar, adds 20 milliliters of ethanol, grinds 2 minutes, filters, and filtrate evaporate to dryness, residue add methenyl choloride makes dissolving for 1 milliliter, as need testing solution; Other gets Radix zanthoxyli control medicinal material 1.9g, and boiling 20 minutes filters, and filtrate is concentrated into dried, adds ethanol and makes dissolving in right amount, filters, and filtrate evaporate to dryness, residue add methenyl choloride makes dissolving for 1 milliliter, in contrast medicinal material solution; Test according to thin-layered chromatography, draw each 10 microlitre of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ammoniacal liquor saturated 30 minutes, launch with the developping agent of normal hexane-methenyl choloride according to preparation in 3: 1, take out, dry, put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
Get 12 of this product, porphyrize adds water and makes dissolving for 50 milliliters, extract 2 times with the ether jolting, and each 40 milliliters, merge ether solution, evaporate to dryness, residue add diethyl ether 2 milliliters and make dissolving, as need testing solution; Other gets elephants-foot 3.2g, adds 50 milliliters in water, decocts 1 hour, filter, it is 45% to containing the alcohol amount that filtrate adds ethanol, leaves standstill, and filters, evaporate to dryness, residue adds 50 milliliters in water, shines medicinal material solution in pairs with legal system, according to the thin-layered chromatography test, draw each 10 microlitre of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, launch with toluene and the absolute ethyl alcohol developping agent according to preparation in 30: 1.5, take out, dry, spray is put under the 365nm ultraviolet lamp and is inspected with 1% aluminium choride ethanolic solution, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
Chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-0.05mol/L triethylamine is according to 30: 70 ratio proportionings, and is the phase that flows with phosphoric acid adjust pH to 2.40 back; The detection wavelength is 328nm; Number of theoretical plate calculates by the Nitidine Chloride peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Nitidine Chloride reference substance, adds methyl alcohol and make per 1 milliliter of solution that contains 4 micrograms, namely;
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got the about 2.0g of powder, the accurate title, decide, and puts in 50 milliliters of tool plug conical flasks, adds 20 milliliters of 0.1mol/L hydrochloric acid, power is 160W, the ultrasonic processing of frequency 40KHz 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with 0.1mol/L hydrochloric acid, change in the separating funnel, extract 3 times with the methenyl choloride jolting, each 20 milliliters, water intaking liquid extracts 3 times each 20 milliliters again with ammonia solution adjust pH to 9～10 with the methenyl choloride jolting, merge methenyl choloride liquid, evaporate to dryness, residue dissolves with methyl alcohol and is transferred in 25 milliliters of measuring bottles, is diluted to scale with methyl alcohol, shake up, filter, precision is measured 10 milliliters of subsequent filtrates, puts in 25 milliliters of measuring bottles, be diluted to scale with methyl alcohol, shake up, filter, get subsequent filtrate as need testing solution;
Determination method is accurate reference substance solution and each 10 microlitre of need testing solution drawn respectively, injects liquid chromatograph, measures, that is, every of this product contains Radix zanthoxyli in Nitidine Chloride, must not be less than 45 micrograms;
The bulk drug prescription of described gynecological inflammation clearance tablet is:
The bitter radix scrophulariae 250g of Radix Angelicae Sinensis 250g reticulate millettia 375g
Elephants-foot 375g Xi is 375g radix fici simplicissimae 500g not
Horizontal in seat 375g Radix zanthoxyli 375g persimmon leaf 375g.
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| CN101822743A (en) * | 2010-05-01 | 2010-09-08 | 秦皇岛皇威制药有限公司 | Medicine for treating inflammation of female reproductive system and preparation and quality control method thereof |
| CN106970167A (en) * | 2017-04-28 | 2017-07-21 | 广西壮族自治区梧州食品药品检验所 | A kind of method of Nitidine Chloride content in measure shiny pricklyash toothpaste |
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Non-Patent Citations (3)
| Title |
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| 刘鹏翰.HPLC 法测定妇炎净片中氯化两面针碱的含量.《食品与药品》.2005,第7卷(第10A期), * |
| 国家药典委员会.妇炎净胶囊.《中华人民共和国药典2000版一部》.2000, * |
| 张辉.止泻灵片主要成分的薄层鉴别.《天津药学》.2004,第16卷(第6期), * |
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