CN100476424C - Method for controlling quality of 'Jinwugutong' capsule - Google Patents
Method for controlling quality of 'Jinwugutong' capsule Download PDFInfo
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- CN100476424C CN100476424C CNB2004101555494A CN200410155549A CN100476424C CN 100476424 C CN100476424 C CN 100476424C CN B2004101555494 A CNB2004101555494 A CN B2004101555494A CN 200410155549 A CN200410155549 A CN 200410155549A CN 100476424 C CN100476424 C CN 100476424C
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Abstract
The invention is a quality control method of Jinwu Gutong capsules, adding a method able to effectively identify psoralen and icraiin components in the existing product manufacturing course, making the psoralen and icraiin components in the finished products relatively determinate so as to offset the shortages of the original quality control method, and the control level of product quality is largely improved. The invention is beneficial for manufacturers and management departments to monitoring the products and can also provide better safeguard for the therapy of medial departments and suffers.
Description
Technical field
The present invention relates to the method for quality control of a kind of method of quality control of Chinese medicine pharmaceutical composition, particularly a kind of Chinese medicinal capsule.
Technical background
'Jinwugutong ' capsule is a kind of medicine of developing on seedling medicine theoretical foundation.Have nourishing liver and kidneyly, dispel rheumatism function promoting blood circulation and removing obstruction in channels.Be used for the treatment of kidney deficiency and liver, wind-cold-dampness arthralgia, osteoporosis, diseases such as the waist and leg ache that osteoproliferation causes, extremity numbness.Psoralen and icariin are respectively the characteristic index components of used medicinal material Psoralea corylifolia of 'Jinwugutong ' capsule and Herba Epimedii.In existing 'Jinwugutong ' capsule process of producing product, owing to lack effective discrimination method, for psoralen in the finished product and icariin is not do composition to differentiate, the one-tenth branch of main drug ingedient psoralen in the finished product and icariin is uncertain like this, make product quality variance bigger, certainly will cause the instability of curative effect, both be unfavorable for the control of manufacturer and administrative authority, also influence the reputation of product in medical department and patient product.
Summary of the invention
The object of the invention is: the method for quality control that a kind of new 'Jinwugutong ' capsule is provided.The present invention is on initial quality control basis, increased the method that effectively to differentiate psoralen and icariin, remedied the deficiency of proper mass control method, improved the quality control level of product, also helped administrative authority product monitoring.
Technical scheme of the present invention is achieved in that the method for quality control of 'Jinwugutong ' capsule; Comprise production method: get scythian lamb rhizome 160g, zaocys dhumnade 120g, root of kudzu vine 200g, barrenwort 200g, pawpaw 120g, achyranthes aspera 120g, Companumoea root 120g, turmeric 120g, root of Chinese clematis 160g, Psoralea corylifolia 160g are raw material; With the root of kudzu vine, turmeric oven dry, be ground into fine powder, cross 80 mesh sieves, standby; All the other scythian lamb rhizomes etc. eight flavor boilings three times, each 2 hours, collecting decoction filtered, and it is 1.10 clear cream that filtrate is concentrated into relative density, puts coldly, adds above-mentioned fine powder, mixing, drying is pulverized, and incapsulates, and makes 1000 of capsules; Also comprise the discrimination method to the 'Jinwugutong ' capsule that makes as stated above: a, get finished capsule product, put microscopically and observe; The many bunchys of fiber, wall thickness, lignify, peripheral cell contains prism of calcium oxalate mostly, forms crystal fiber; B, get finished capsule product content 1.8g, add methyl alcohol 20ml, sonicated 1 hour filters, and filtrate evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, as need testing solution; Other gets the Puerarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin-layered chromatography test, draw each 4～10 μ l of above-mentioned two kinds of solution put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with 8: 2 chloroform-methanols, launch, take out, dry; Put under the ultraviolet lamp of 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color; C, get finished product
Capsule 's content 1.8g adds absolute ethyl alcohol 10ml, and dipping spends the night, and filters, and filtrate is concentrated into 1ml, as need testing solution; Other gets turmeric control medicinal material 0.1g, adds absolute ethyl alcohol 10ml, shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 4～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-chloroforms of 49: 49: 4-ethanol, launch, take out, dry; Put under the ultraviolet lamp of 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; It is characterized in that, discrimination method is further comprising the steps of: d, get 'Jinwugutong ' capsule content 2g, add the ultrasonic 30min of 95% ethanol 30ml, filter, filtrate is waved near in water-bath and is done, add water 20ml and made dissolving in ultrasonic 1 minute, with ethyl acetate extraction 3 times, each 10ml, combined ethyl acetate liquid, steam to 2ml, as need testing solution; Other gets the psoralen reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin-layered chromatography test, draw each 10～15 μ l of above-mentioned two kinds of solution respectively, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-ethyl acetates of 9.5: 0.5, launch, take out, dry; Under the 365nm uviol lamp, inspect, test sample with the corresponding speckle displacement of reference substance on, show same color fluorescence spot; E, get 'Jinwugutong ' capsule content 5g, add water and stir 2 minutes 2 times, each 15ml, double-deck filter paper suction filtration, merging filtrate is used ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, evaporate to dryness, residue adds the abundant agitator treating of chloroform 2 times, and each 1ml discards chloroform solution, residue adds water 1ml washing 1 time, discard water liquid, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets icariin, adds methyl alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned two kinds of each 5-10ul of solution respectively, put respectively on same silica gel g thin-layer plate, with 10: 1: 1: ethyl acetate-butanone of 1-formic acid-water is developping agent, launch, take out, dry, spray aluminium choride alcoholic solution with 5%, in 105 ℃ of heating 5 minutes, under the 365nm uviol lamp, inspect, test sample with the corresponding principal spot of reference substance position on, show the fluorescence spot of same color.
In the method for quality control of above-mentioned 'Jinwugutong ' capsule, also comprise following content assaying method, according to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica, and 280: 720: 0.15 methanol-water-phosphoric acid is a moving phase, and the detection wavelength is 250nm.Theoretical cam curve is calculated by puerarin peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the Puerarin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, shakes up, promptly; The preparation of need testing solution: get the content under this product content uniformity item, porphyrize is got 0.1g, and accurate the title decides, add ethanol 10ml, reflux 30 minutes filters, and with small amount of ethanol gradation washing container and residue, filter merging filtrate, evaporate to dryness, residue adds water 10ml makes dissolving, adds chloroform and extracts 2 times, each 10ml, discard chloroform solution, water bath method, residue add dissolve with methanol and are transferred in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, promptly; Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; Every of this product contains the root of kudzu vine with Puerarin (C
21H
20O
9) meter, must not be less than 1.3mg.
Compared with the prior art, the present invention has increased the method that can effectively differentiate psoralen and icariin composition in existing process of producing product.Make that the composition of main drug ingedient psoralen in the finished product and icariin is more definite, the controllable quality level improves a lot.Application of the present invention had both helped manufacturer and administrative authority to product monitoring, also can provide better guarantees for medical department and patient's treatment.
Embodiment
The embodiment of the invention: the method for quality control of 'Jinwugutong ' capsule.Comprise production method, discrimination method and content assaying method.
Production method is: get scythian lamb rhizome 160g, zaocys dhumnade 120g, root of kudzu vine 200g, barrenwort 200g, pawpaw 120g, achyranthes aspera 120g, Companumoea root 120g, turmeric 120g, root of Chinese clematis 160g, Psoralea corylifolia 160g are raw material; With the root of kudzu vine, turmeric oven dry, be ground into fine powder, cross 80 mesh sieves, standby; All the other scythian lamb rhizomes etc. eight flavor boilings three times, each 2 hours, collecting decoction filtered, and it is 1.10 clear cream that filtrate is concentrated into relative density, puts coldly, adds above-mentioned fine powder, mixing, drying is pulverized, and incapsulates, and makes 1000 of capsules.
Discrimination method is:
A, get finished capsule product, put microscopically and observe; The many bunchys of fiber, wall thickness, lignify, peripheral cell contains prism of calcium oxalate mostly, forms crystal fiber;
B, get finished capsule product content 1.8g, add methyl alcohol 20ml, sonicated 1 hour filters, filtrate steam in, residue adds methyl alcohol 0.5ml makes dissolving, as need testing solution; Other gets the Puerarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 4～10 μ l of above-mentioned two kinds of solution put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with 8: 2 chloroform-methanols, launch, take out, dry; Put under the ultraviolet lamp of 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
C, get finished capsule product content 1.8g, add absolute ethyl alcohol 10ml, dipping spends the night, and filters, and filtrate is concentrated into 1ml, as need testing solution; Other gets turmeric control medicinal material 0.1g, adds absolute ethyl alcohol 10ml, shines medicinal material solution in pairs with legal system; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw each 4～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-chloroforms of 49: 49: 4-ethanol, launch, take out, dry; Put under the ultraviolet lamp of 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;
D, get 'Jinwugutong ' capsule content 2g, add the ultrasonic 30min of 95% ethanol 30ml, filter, filtrate is waved near in water-bath and is done, add water 20ml and made dissolving in ultrasonic 1 minute, use ethyl acetate extraction 3 times, each 10ml, combined ethyl acetate liquid steams to 2ml, as need testing solution; Other gets the psoralen reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw each 10～15 μ l of above-mentioned two kinds of solution respectively, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-ethyl acetates of 9.5: 0.5, launch, take out, dry; Under the 365nm uviol lamp, inspect, test sample with the corresponding speckle displacement of reference substance on, show same color fluorescence spot;
E, get 'Jinwugutong ' capsule content 5g, add water and stir 2 minutes 2 times, each 15ml, double-deck filter paper suction filtration, merging filtrate is used ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, evaporate to dryness, residue adds the abundant agitator treating of chloroform 2 times, and each 1ml discards chloroform solution, residue adds water 1ml washing 1 time, discard water liquid, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets icariin, adds methyl alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw above-mentioned two kinds of each 5-10ul of solution respectively, put respectively on same silica gel g thin-layer plate, with 10: 1: 1: ethyl acetate-butanone of 1-formic acid-water is developping agent, launch, take out, dry, spray aluminium choride alcoholic solution with 5%, in 105 ℃ of heating 5 minutes, under the 365nm uviol lamp, inspect, test sample with the corresponding principal spot of reference substance position on, show the fluorescence spot of same color.
Content assaying method is: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D); Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica, and 280: 720: 0.15 methanol-water-phosphoric acid is a moving phase, and the detection wavelength is 250nm.Theoretical cam curve is calculated by puerarin peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the Puerarin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, shakes up, promptly; The preparation of need testing solution: get the content under this product content uniformity item, porphyrize is got 0.1g, and accurate the title decides, add ethanol 10ml, reflux 30 minutes filters, and with small amount of ethanol gradation washing container and residue, filter merging filtrate, evaporate to dryness, residue adds water 10ml makes dissolving, adds chloroform and extracts 2 times, each 10ml, discard chloroform solution, water bath method, residue add dissolve with methanol and are transferred in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, promptly; Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; Every of this product contains the root of kudzu vine with Puerarin (C
21H
20O
9) meter, must not be less than 1.3mg.
Claims (2)
1. the method for quality control of 'Jinwugutong ' capsule; Comprise production method: get scythian lamb rhizome 160g, zaocys dhumnade 120g, root of kudzu vine 200g, barrenwort 200g, pawpaw 120g, achyranthes aspera 120g, Companumoea root 120g, turmeric 120g, root of Chinese clematis 160g, Psoralea corylifolia 160g are raw material; With the root of kudzu vine, turmeric oven dry, be ground into fine powder, cross 80 mesh sieves, standby; All the other scythian lamb rhizomes etc. eight flavor boilings three times, each 2 hours, collecting decoction filtered, and it is 1.10 clear cream that filtrate is concentrated into relative density, puts coldly, adds above-mentioned fine powder, mixing, drying is pulverized, and incapsulates, and makes 1000 of capsules; Also comprise the discrimination method to the 'Jinwugutong ' capsule that makes as stated above: a, get finished capsule product, put microscopically and observe; The many bunchys of fiber, wall thickness, lignify, peripheral cell contains prism of calcium oxalate mostly, forms crystal fiber; B, get finished capsule product content 1.8g, add methyl alcohol 20ml, sonicated 1 hour filters, and filtrate evaporate to dryness, residue add methyl alcohol 0.5ml makes dissolving, as need testing solution; Other gets the Puerarin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin-layered chromatography test, draw each 4～10 μ l of above-mentioned two kinds of solution put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with 8: 2 chloroform-methanols, launch, take out, dry; Put under the ultraviolet lamp of 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color; C, get finished capsule product content 1.8g, add absolute ethyl alcohol 10ml, dipping spends the night, and filters, and filtrate is concentrated into 1ml, as need testing solution; Other gets turmeric control medicinal material 0.1g, adds absolute ethyl alcohol 10ml, shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 4～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-chloroforms of 49: 49: 4-ethanol, launch, take out, dry; Put under the ultraviolet lamp of 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; It is characterized in that, discrimination method is further comprising the steps of: d, get 'Jinwugutong ' capsule content 2g, add the ultrasonic 30min of 95% ethanol 30ml, filter, filtrate is waved near in water-bath and is done, add water 20ml and made dissolving in ultrasonic 1 minute, with ethyl acetate extraction 3 times, each 10ml, combined ethyl acetate liquid, steam to 2ml, as need testing solution; Other gets the psoralen reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin-layered chromatography test, draw each 10～15 μ l of above-mentioned two kinds of solution respectively, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-ethyl acetates of 9.5: 0.5, launch, take out, dry; Under the 365nm uviol lamp, inspect, test sample with the corresponding speckle displacement of reference substance on, show same color fluorescence spot; E, get 'Jinwugutong ' capsule content 5g, add water and stir 2 minutes 2 times, each 15ml, double-deck filter paper suction filtration, merging filtrate is used ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, evaporate to dryness, residue adds the abundant agitator treating of chloroform 2 times, and each 1ml discards chloroform solution, residue adds water 1ml washing 1 time, discard water liquid, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets icariin, adds methyl alcohol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned two kinds of each 5-10ul of solution respectively, put respectively on same silica gel g thin-layer plate, with 10: 1: 1: ethyl acetate-butanone of 1-formic acid water is developping agent, launch, take out, dry, spray aluminium choride alcoholic solution with 5%, in 105 ℃ of heating 5 minutes, under the 365nm uviol lamp, inspect, test sample with the corresponding principal spot of reference substance position on, show the fluorescence spot of same color.
2. the method for quality control of 'Jinwugutong ' capsule according to claim 1, it is characterized in that: this method also comprises following content assaying method, according to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica, and 280: 720: 0.15 methanol-water-phosphoric acid is a moving phase, and the detection wavelength is 250nm; Theoretical cam curve is calculated by puerarin peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the Puerarin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, shakes up, promptly; The preparation of need testing solution: get the content under this product content uniformity item, porphyrize is got 0.1g, and accurate the title decides, add ethanol 10ml, reflux 30 minutes filters, and with small amount of ethanol gradation washing container and residue, filter merging filtrate, evaporate to dryness, residue adds water 10ml makes dissolving, adds chloroform and extracts 2 times, each 10ml, discard chloroform solution, water bath method, residue add dissolve with methanol and are transferred in the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, promptly; Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; Every of this product contains the root of kudzu vine with Puerarin C
21H
20O
9Meter must not be less than 1.3mg.
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| CNB2004101555494A CN100476424C (en) | 2004-12-21 | 2004-12-21 | Method for controlling quality of 'Jinwugutong' capsule |
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| CNB2004101555494A CN100476424C (en) | 2004-12-21 | 2004-12-21 | Method for controlling quality of 'Jinwugutong' capsule |
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| CN100476424C true CN100476424C (en) | 2009-04-08 |
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