CN101239117A - Quality control method of traditional Chinese medicine formulations for treating gynaecologic disease - Google Patents
Quality control method of traditional Chinese medicine formulations for treating gynaecologic disease Download PDFInfo
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Abstract
The present invention relates a method for preparing gongyanping tablet and controlling quality. The gongyanping tablet is prepared from five Chinese traditional medicines including diren, shinyleaf pricklyash root, angelica, chuanposhi (tuomu), wuzhimaotao. The method comprises identifying and content determinating which takes octadecylsilane chemically bonded silica as filling agent; acetonitrile -0.05% phosphoric acid (3:97) as flowing phase; detecting wavelength 272nm; detecting the amount of gallic acid contained in manufactured goods each unit.
Description
Invention field
The present invention relates to a kind of preparation and method of quality control of gynecological Chinese medicine preparation, particularly a kind of preparation and method of quality control thereof of the GONGYANPING tablet of making by Chinese medicine of the five flavours such as Herba Melastomatis dodecandri, Radix Zanthoxyli, Radix Angelicae Sinensis, Radix Cudraniae (Lignum Cudraniae tricuspidatae), Herba Fici Simplicissimae.
Background technology:
China Patent No.: 00103132.5 " coated Gongyanping tablet in special shape and manufacture method thereof " discloses a kind of preparation method of GONGYANPING tablet.In recent years, further investigation along with Gongyanping preparation, the preparation method of GONGYANPING novel form has obtained concern, patent application as application number 03118640.8 relates to the capsular preparation of a kind of GONGYANPING, relate to a kind of preparation of GONGYANPING dispersible tablet as the application of application number 200410045022.6, relate to the preparation of several novel forms of GONGYANPING as the application of application number 200410058353.3.
In the GONGYANPING PIAN standard,, only there is the thin layer of Herba Melastomatis dodecandri and Radix Zanthoxyli control medicinal material to differentiate in " Chinese traditional patent formulation preparation " the 17, the quality that this quality standard can not the better controlled Gongyanping preparation for the quality control of Gongyanping preparation.For guaranteeing the safe and effective of Gongyanping preparation, the quality standard of said preparation has been carried out improving research.
2004 4 phases of Guiyang Medical College journal disclose the method for a kind of " content of gallic acid in the high effective liquid chromatography for measuring GONGYANPING capsule ", Chinese Journal of Pharmaceuticals-2006 year 11 phases, documents such as " quality standard researches of GONGYANPING PIAN " is significantly different with the present invention.
Summary of the invention:
The invention discloses the detection method of quantitative control Gongyanping preparation quality, this method specificity is strong, and sensitivity, precision, repeatability all satisfy the requirement of drug quality control:
Technical scheme of the present invention is:
1, the method for making of preparation of the present invention by pharmaceuticals industry drug standard convention form is:
[prescription] Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae (Lignum Cudraniae tricuspidatae) 140g
[method for making] above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
Wherein Herba Melastomatis dodecandri is meant: the dry herb of Melastomataceae plant Herba Melastomatis dodecandri Melastoma dodecandrum Lou..
Herba Fici Simplicissimae is meant: the dry root of moraceae plants ficus simplicissima Ficus hirta vahl..
Radix Cudraniae is meant: dry root and the stem branch of nearly source plants such as moraceae plants three-bristle cudrania tree Cudrania tricuspidata (Carr.) Bur. or Moraceae three-bristle cudrania platymiscium cudrania cochinchinensis Cudrania cochinchensis (Lour.) Kudo et Masam..Be called Lignum Cudraniae tricuspidatae again.
Radix Zanthoxyli, Radix Angelicae Sinensis are pressed the Chinese Pharmacopoeia regulation and are used.
2, the finished product of above-mentioned acquisition can carry out identification check, assay in the following manner
[discriminating]
(1) gets the manufactured goods that are equivalent to raw medicinal herbs amount 10g, remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
(2) get the manufactured goods that are equivalent to raw medicinal herbs amount 6g, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get the manufactured goods that this product is equivalent to raw medicinal herbs amount 4g, remove coating, porphyrize, add methanol 20ml supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia current edition), draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
(4) get the manufactured goods that are equivalent to raw medicinal herbs amount 8g, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, extracted with diethyl ether 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)～Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
When this product manufactured goods are sugar-coat or film coated tablet:
(1) gets 10 of this product, remove coating, porphyrize, add methanol 30ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
(2) get 6 of this product, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get 4 of this product, remove coating, porphyrize adds methanol 20ml supersound process 30 minutes, filters, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B) according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B) test, draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
(4) get 8 of this product, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling is immediately extracted 2 times with the ether jolting, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
[inspection] should meet every regulation relevant under the tablet item (an appendix I of Chinese Pharmacopoeia current edition D).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia current edition D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly.
10 of this product are got in the preparation of need testing solution, remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Herba Melastomatis dodecandri with gallic acid (C
7H
6O
5) meter, must not be less than 0.1mg.
Obviously, formulation method of the present invention can be by obtaining other peroral dosage forms such as capsule, dispersible tablet, drop pill, soft capsule, effervescent tablet, and assay of the present invention is differentiated to be equally applicable to various peroral dosage forms.
Effect of the present invention:
Though GONGYANPING PIAN is recorded in " Chinese traditional patent formulation preparation " the 17, the method for making that relevant said preparation is detailed, adjuvant use, the discriminating and the assay of effective ingredient are rarely put down in writing.
The present invention confirms that by research the tablet quality controllability of Herba Melastomatis dodecandri, Radix Zanthoxyli, Radix Angelicae Sinensis, Radix Cudraniae, Herba Fici Simplicissimae being made GONGYANPING by specific extracting method is good.
Modern pharmacological research shows, Gongyanping preparation has multiple effects such as antiinflammatory, analgesia, spasmolytic, has close dependency with contained gallic acid in the preparation, by gallic acid quantitatively being reached the foundation of other qualitative indexes, the inherent quality that can reflect preparation, the correct capacity of control raw medicinal material is used, and helps preventing the appearance of counterfeit drug, substandard drug.
The present invention has set up the discriminating of the relevant medical material of GONGYANPING of system, matches with the gallic acid content assay method, effectively controls the GONGYANPING product quality comparatively comprehensively.
Specific embodiment:
Embodiment 1: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
The detection method of gallic acid is:
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia current edition D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly.
10 of this product are got in the preparation of need testing solution, remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Herba Melastomatis dodecandri with gallic acid (C
7H
6O
5) meter, must not be less than 0.1mg.
Embodiment 2: a kind of GONGYANPING capsule preparations and assay
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
(1) the above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), adds ethanol and reaches 50% to containing the alcohol amount, leaves standstill 24 hours, filter, filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃, be ground into fine powder, add right amount of auxiliary materials such as starch, mixing is made granule, dry below 80 ℃
(2) filled capsules is 500, promptly.
The detection method of gallic acid is:
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia current edition D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly.
5 of this product are got in the preparation of need testing solution, remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Herba Melastomatis dodecandri with gallic acid (C
7H
6O
5) meter, must not be less than 0.2mg.
Embodiment 3: a kind of GONGYANPING dropping pill formulation and assay
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
(1) the above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), adds ethanol and reaches 50% to containing the alcohol amount, leaves standstill 24 hours, filter, filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃, be ground into fine powder, add right amount of auxiliary materials, mixing drips system or is pressed into ball, dry below 80 ℃
(2) make 5000, promptly.
The detection method of gallic acid is:
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia current edition D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly.
50 of this product are got in the preparation of need testing solution, remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Per 10 of this product contains Herba Melastomatis dodecandri with gallic acid (C
7H
6O
5) meter, must not be less than 0.2mg.
Embodiment 4: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, coating, promptly.
Above-mentioned tablet is differentiated in the following ways:
Get 10 of this product, remove coating, porphyrize, add methanol 30ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
Embodiment 5: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
(1) gets 10 of this product, remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color;
(2) get 6 of this product, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color;
(3) get 4 of this product, remove coating, porphyrize adds methanol 20ml supersound process 30 minutes, filters, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
(4) get 8 of this product, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling is immediately extracted 2 times with the ether jolting, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Lignum Cudraniae tricuspidatae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
Embodiment 6: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
Above-mentioned tablet is differentiated in the following ways:
Get 6 of this product, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
Embodiment 7: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
Above-mentioned tablet is differentiated in the following ways:
Get 4 of this product, remove coating, porphyrize adds methanol 20ml supersound process 30 minutes, filters, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
Embodiment 8: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
Above-mentioned tablet is differentiated in the following ways:
Get 8 of this product, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling is immediately extracted 2 times with the ether jolting, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
Embodiment 9: a kind of GONGYANPING PIAN preparation
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, and coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), add ethanol and reach 50% to containing the alcohol amount, left standstill 24 hours, and filtered filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃ is ground into fine powder, adds right amount of auxiliary materials such as starch, mixing, make granule, dry below 80 ℃, be pressed into 1000, sugar coating or film-coat, promptly.
[discriminating]
(1) gets 10 of this product, remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
(2) get 6 of this product, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get 4 of this product, remove coating, porphyrize adds methanol 20ml supersound process 30 minutes, filters, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
(4) get 8 of this product, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling is immediately extracted 2 times with the ether jolting, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia current edition B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly.
10 of this product are got in the preparation of need testing solution, remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Herba Melastomatis dodecandri with gallic acid (C
7H
6O
5) meter, must not be less than 0.1mg.
Embodiment 10: the linear dependence of getting gallic acid content in the commercially available GONGYANPING is measured:
The preparation precision of gallic acid reference substance storing solution takes by weighing the gallic acid reference substance 10.45mg through the dry constant weight of phosphorus pentoxide, puts in the 100ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up, and promptly gets (every 1ml contains gallic acid 0.1045mg).
The above-mentioned gallic acid reference substance storing solution 10ml of the accurate absorption of the preparation of gallic acid reference substance solution I puts in the 25ml measuring bottle, adds methanol and is diluted to scale, shake up, that is, and (every 1ml contains gallic acid 41.80 μ g).
The above-mentioned gallic acid reference substance storing solution 5ml of the accurate absorption of the preparation of gallic acid reference substance solution II puts in the 100ml measuring bottle, adds methanol and is diluted to scale, shake up, that is, and (every 1ml contains gallic acid 5.225 μ g).
Accurate respectively gallic acid reference substance solution I 1,2,4,6,8,10,12,15, the 18 μ l that draw, gallic acid reference substance solution II 2,4 μ l, injecting chromatograph, press above-mentioned chromatographic condition parallel assay each twice, with the reference substance sample size is abscissa, average peak area is a vertical coordinate, the drawing standard curve.In 0.01045～0.7524 μ g scope, get regression equation: y=6691890.0354x-19235.0016 (R
2=1.0000).The results are shown in following table.
The linear test result
| The sample introduction sequence number | Sample size (μ g) | Peak area 1 | Peak area 2 | Average peak area |
| 1 | 0.01045 | 53438 | 53141 | 53289.5 |
| 2 3 4 5 6 7 8 9 10 11 | 0.0209 0.0418 0.0836 0.1672 0.2508 0.3344 0.4180 0.5016 0.6270 0.7524 | 116739 256396 529608 1143085 1655589 2217695 2770266 3333699 4170572 5004022 | 112380 256069 535254 1106396 1641390 2217852 2784197 3360532 4174790 5020930 | 114559.5 256232.5 532431 1124741 1648490 2217756 2777232 3347116 4172681 5012476 |
Result of the test shows: gallic acid sample size peak area in 0.01045～0.7524 μ g scope has good linear relationship.
The thin layer of Radix Cudraniae in embodiment 11, the GONGYANPING PIAN (Lignum Cudraniae tricuspidatae) is differentiated:
Get 8 of this product, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, extracted with diethyl ether 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
The thin layer of embodiment 12, GONGYANPING PIAN Herba Melastomatis dodecandri is differentiated:
Get 10 of this product, remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
Embodiment 13: the thin layer of Radix Zanthoxyli is differentiated in the GONGYANPING PIAN:
Get 6 of this product, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, with water saturated n-butanol extraction twice, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
Embodiment 14: the thin layer of the Herba Fici Simplicissimae in the GONGYANPING PIAN is differentiated:
Get 4 of this product, remove coating, porphyrize adds methanol 20ml supersound process 30 minutes, filters, filtrate evaporate to dryness, residue add water 15ml dissolving, use ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and hot blast blows to colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
Embodiment 15: a kind of Gongyanping preparation and assay
Herba Melastomatis dodecandri 450g Radix Zanthoxyli 170g Radix Angelicae Sinensis 140g
Herba Fici Simplicissimae 100g Radix Cudraniae 140g
The above five tastes, four Chinese medicine material such as all the other Radix Zanthoxylis is ground into coarse powder except that Herba Melastomatis dodecandri, coarse powder and Herba Melastomatis dodecandri decoct with water secondary together, each 2 hours, filter, merging filtrate, vacuum concentration below 80 ℃ to relative density is the clear paste of 1.23～1.28 (55～60 ℃), adds ethanol and reaches 50% to containing the alcohol amount, leaves standstill 24 hours, filter, filtrate recycling ethanol, being evaporated to relative density is the clear paste of 1.25～1.30 (55～60 ℃), vacuum drying below 90 ℃, be ground into fine powder, add right amount of auxiliary materials such as starch, mixing is made granule, dry below 80 ℃, make suitable oral finished product.
(1) gets the manufactured goods that are equivalent to raw medicinal herbs 10g, remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.An appendix VI of Chinese Pharmacopoeia version in 2005 B is according to the thin layer chromatography test, draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-formic acid (6: 3: 1) is developing solvent, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color.
(2) get the manufactured goods that are equivalent to raw medicinal herbs 6g, remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system.An appendix VI of Chinese Pharmacopoeia version in 2005 B is according to the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (15: 4: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get the manufactured goods that this product is equivalent to raw medicinal herbs 4g, remove coating, porphyrize, add methanol 20ml supersound process 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml dissolving, extract 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system.An appendix VI of Chinese Pharmacopoeia version in 2005 B is according to the thin layer chromatography test, draw each 8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
(4) get the manufactured goods that are equivalent to raw medicinal herbs 8g, remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, extracted with diethyl ether 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shines medical material solution in pairs with legal system.An appendix VI of Chinese Pharmacopoeia version in 2005 B is according to the 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, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1.0.1) be developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
Claims (5)
1, a kind of method of quality control for the treatment of the Chinese medicine preparation of gynaecopathia, described preparation is 45: 17: 14 with the medical material weight portion: 10: 14 Herba Melastomatis dodecandri, Radix Zanthoxyli, Radix Cudraniae (Lignum Cudraniae tricuspidatae), Herba Fici Simplicissimae, Radix Angelicae Sinensis are made, and it is characterized in that:
Measure gallic acid (C in its finished product by high-efficient liquid phase technique
7H
6O
5) content, be mobile phase with acetonitrile-0.05% phosphoric acid (3: 97); The detection wavelength is 272nm; Reference substance solution 1ml contains the methanol solution of 10 μ g gallic acids; Get the manufactured goods that are equivalent to raw medicinal herbs amount 10g, have coating to remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly get need testing solution.
2, a kind of method of quality control for the treatment of the Chinese medicine preparation of gynaecopathia according to claim 1 is characterized in that measuring gallic acid (C in its finished product by high-efficient liquid phase technique
7H
6O
5) content:
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g;
The manufactured goods that are equivalent to raw medicinal herbs amount 10g are got in the preparation of need testing solution, have coating to remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure; The preparation that per 1 gram raw medicinal herbs is made contains gallic acid (C
7H
6O
5) content is no less than 0.1mg.
3, a kind of method of quality control for the treatment of the Chinese medicine preparation of gynaecopathia is characterized in that differentiating by the following method its quality:
(1) gets the manufactured goods that are equivalent to raw medicinal herbs amount 10g, have coating to remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, gets Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system, other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution, test according to thin layer chromatography, draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with chloroform-ethyl acetate-formic acid (6: 3: 1), launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, in the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color
(2) get the manufactured goods that are equivalent to raw medicinal herbs amount 6g, have coating to remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, in the dislocation separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 15ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system, test according to thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with chloroform-acetone-formic acid (15: 4: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color
(3) get the manufactured goods that this product is equivalent to raw medicinal herbs amount 4g, have coating to remove coating, porphyrize, add methanol 20ml supersound process 30 minutes, filter the filtrate evaporate to dryness, residue adds water 15ml dissolving, extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution, other gets Herba Fici Simplicissimae control medicinal material 1g, shines medical material solution in pairs with legal system, according to the thin layer chromatography test, draw each 8 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-ethyl acetate-formic acid (4: 1: 0.1), launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color
(4) get the manufactured goods that are equivalent to raw medicinal herbs amount 8g, have coating to remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, extracted with diethyl ether 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, and as need testing solution, other gets Radix Cudraniae (Lignum Cudraniae tricuspidatae) control medicinal material 1g, shine medical material solution in pairs with legal system, according to the 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, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
4, according to claim 1 or 2 or 3 described a kind of method of quality control for the treatment of the Chinese medicine preparation of gynaecopathia, it is characterized in that comprising following discriminating and content assaying method:
(1) gets the manufactured goods that are equivalent to raw medicinal herbs amount 10g, there is coating to remove coating, porphyrize, add methanol 30ml, ultrasonic 30 minutes, filter, the filtrate evaporate to dryness, residue adds water 10ml dissolving, add hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, cooled aqueous solution extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, get Herba Melastomatis dodecandri control medicinal material 1g, shine medical material solution in pairs with legal system, other gets the gallic acid reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution is tested according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography in contrast, draw need testing solution, control medicinal material solution each 10 μ l and reference substance solution 5 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-ethyl acetate-formic acid (6: 3: 1), launches, take out, dry, spray is with 1% ferric chloride alcoholic solution, in the test sample chromatograph, with control medicinal material and reference substance chromatograph relevant position on, show the speckle of same color;
(2) get the manufactured goods that are equivalent to raw medicinal herbs amount 6g, have coating to remove coating, porphyrize, put in the conical flask, after soaking into proper ammonia, add methanol 20ml, supersound process 30 minutes is put coldly, filters, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, in the dislocation separatory funnel, extracts twice with water saturated n-butyl alcohol jolting, each 15ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution, other gets Radix Zanthoxyli control medicinal material 1g, shines medical material solution in pairs with legal system, according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 10 μ l, control medicinal material solution 5 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-acetone-formic acid (15: 4: 1), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color;
(3) get the manufactured goods that are equivalent to raw medicinal herbs amount 4g, have coating to remove coating, porphyrize, add methanol 20ml supersound process 30 minutes, filter the filtrate evaporate to dryness, residue adds water 15ml dissolving, extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add chloroform 1ml makes dissolving, as need testing solution, other gets Herba Fici Simplicissimae control medicinal material 1g, shine medical material solution in pairs with legal system,, draw each 8 μ l of above-mentioned two kinds of solution according to the test of an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate-formic acid (4: 1: 0.1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
(4) get the manufactured goods that are equivalent to raw medicinal herbs amount 8g, have coating to remove coating, porphyrize, add methanol 20ml, supersound process 30 minutes filters, the filtrate evaporate to dryness, residue adds water 10ml dissolving, adds hydrochloric acid 2ml, reflux 30 minutes, cooling immediately, extract 2 times with the ether jolting, each 20ml merges ether solution, evaporate to dryness, residue adds chloroform 1ml makes dissolving, and as need testing solution, other gets Lignum Cudraniae tricuspidatae control medicinal material 1g, shine medical material solution in pairs with legal system, according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (4: 1: 0.1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color;
(5) according to an appendix VID of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid (3: 97) is mobile phase; The detection wavelength is 272nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 5000;
The preparation precision of reference substance solution takes by weighing that to be dried to the gallic acid reference substance of constant weight through phosphorus pentoxide an amount of, adds methanol and makes the solution that every 1ml contains 10 μ g, promptly;
The manufactured goods that are equivalent to raw medicinal herbs amount 10g are got in the preparation of need testing solution, have coating to remove coating, porphyrize, precision takes by weighing 0.5g, and the accurate 5% hydrochloric acid solution 100ml that adds puts in the tool plug conical flask, claim to decide weight, put in the boiling water bath back hydrolysis 4 hours, put cold, claim to decide weight once more, supply the weight that subtracts mistake with 5% hydrochloric acid solution, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, that is, the preparation that the per 1 gram raw medicinal herbs of this product is made contains gallic acid (C
7H
6O
5) content is no less than 0.1mg.
5, a kind of method of quality control for the treatment of the Chinese medicine preparation of gynaecopathia according to claim 3 is characterized in that:
Described manufactured goods include but not limited to coated tablet or Film coated tablets or capsule or soft capsule or granule or dispersible tablet or drop pill or effervescent tablet.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102707006A (en) * | 2012-05-30 | 2012-10-03 | 涂瑶生 | Quality detection method of cudrania tricuspidata formula granules |
| CN103977121A (en) * | 2014-05-26 | 2014-08-13 | 江西民济药业有限公司 | Preparation method and detection method of hysteritis-treating dispersible tablets |
| CN103983735A (en) * | 2014-05-26 | 2014-08-13 | 江西民济药业有限公司 | Detection method for preparing Gongyanping (brand) capsules |
| CN111721846A (en) * | 2019-03-21 | 2020-09-29 | 天津同仁堂集团股份有限公司 | Method for identifying traditional Chinese medicine preparation throat-clearing tablets |
| CN113791147A (en) * | 2021-08-31 | 2021-12-14 | 南京海昌中药集团有限公司 | Quality detection method of cudrania cochinchinensis |
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2008
- 2008-01-10 CN CNA2008100028798A patent/CN101239117A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102707006A (en) * | 2012-05-30 | 2012-10-03 | 涂瑶生 | Quality detection method of cudrania tricuspidata formula granules |
| CN102707006B (en) * | 2012-05-30 | 2014-03-26 | 涂瑶生 | Quality detection method of cudrania tricuspidata formula granules |
| CN103977121A (en) * | 2014-05-26 | 2014-08-13 | 江西民济药业有限公司 | Preparation method and detection method of hysteritis-treating dispersible tablets |
| CN103983735A (en) * | 2014-05-26 | 2014-08-13 | 江西民济药业有限公司 | Detection method for preparing Gongyanping (brand) capsules |
| CN103983735B (en) * | 2014-05-26 | 2015-12-02 | 江西民济药业有限公司 | A kind of detection method preparing medical capsule for treating pelvic inflammatory disease |
| CN111721846A (en) * | 2019-03-21 | 2020-09-29 | 天津同仁堂集团股份有限公司 | Method for identifying traditional Chinese medicine preparation throat-clearing tablets |
| CN113791147A (en) * | 2021-08-31 | 2021-12-14 | 南京海昌中药集团有限公司 | Quality detection method of cudrania cochinchinensis |
| CN113791147B (en) * | 2021-08-31 | 2023-08-25 | 南京海昌中药集团有限公司 | Quality detection method of cudrania root |
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