CN1538173A - Method for control quality of Chinese medicinal preparation - Google Patents
Method for control quality of Chinese medicinal preparation Download PDFInfo
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- CN1538173A CN1538173A CNA03121889XA CN03121889A CN1538173A CN 1538173 A CN1538173 A CN 1538173A CN A03121889X A CNA03121889X A CN A03121889XA CN 03121889 A CN03121889 A CN 03121889A CN 1538173 A CN1538173 A CN 1538173A
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Abstract
A quality control method for the Chinese medicine 'Naoxueshuan table' features that part of its components are discriminated and their contents are measured.
Description
Invention field
The present invention relates to a kind of method of quality control, particularly a kind of method of quality control of Chinese medicine preparation.
Background technology
Anti-cerebral-thrombosis tablet has promoting blood circulation and removing blood stasis, brain-refreshing and channel obstruction-removing, and the suppressing hyper-yang to eliminate wind effect is used for because of hemostasis, the premonitory apoplexy of liver-yang hyperactivity appearance, disease prevention and treatments such as the aphasia from apoplexy that occurs as extremity numbness, cerebral thrombosis such as have a dizzy spell, facial paralysis, hemiplegia.From producing, because of determined curative effect, effect is subjected to liking of numerous doctors and patient rapidly deeply, and this just requires us to produce high-quality product, but the initial quality control method is difficult to product is carried out effective quality control.
Press described anti-cerebral-thrombosis tablet prescription of the Sanitation Ministry medicine standard and preparation method: safflower 900g; Radix Angelicae Sinensis 900g; leech (system) 900g; red spoon 900g; peach kernel 900g; Ligusticum wallichii 900g; red sage root 900g; ground bettle 225g; antelope's horn 112.5g; cow-bezoar 12.5g; more than ten the flavor; red spoon; leech is ground into fine powder; the safflower poach is condensed into cream twice; Radix Angelicae Sinensis; Ligusticum wallichii; the red sage root; peach kernel; the five tastes such as ground bettle are with twice of 70% alcohol extract; be condensed into cream; with above water; the alcohol condensed cream merges, with red spoon; leech fine powder and right amount of auxiliary materials are mixed, and add antelope's horn; the cow-bezoar fine powder; mixing; make particle, drying, compressing tablet; sugar coating or film-coating, promptly.
Summary of the invention
The objective of the invention is to disclose a kind of method of quality control of Chinese medicine preparation.
The present invention seeks to be achieved through the following technical solutions:
A kind of described anti-cerebral-thrombosis tablet prescription of Chinese Pharmacopoeia of pressing, the method for quality control of making the formulation of clinical practice comprises to be differentiated and/or assay: (following unit quantity is meant: quite take each preparation output of crude drug amount every day)
Discrimination method: differentiate: get 5/9 unit quantity preparation, porphyrize places conical flask, add the 40ml alcohol immersion 3-5 hour, and sonicated 25-35 minute, left standstill cooling, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, place separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, the photograph thin-layered chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution respectively, put in same silica G F respectively
254On the thin layer plate, with 6-9: 0.5-2: 0.5-2 ethyl acetate one glacial acetic acid one water is developping agent, launches, and takes out, and dries, and inspects under the 240-260nm ultraviolet lamp, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material;
Assay: the photograph high performance liquid chromatography (" 2000 editions appendix VID of Chinese pharmacopoeia) to measure, chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; 16-20: 78-90 acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution is a moving phase, and the detection wavelength is 220-240nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 30-40 hour Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; Preparation 1.5g under the content uniformity item is got in the preparation of need testing solution, and accurate the title decides, put in the tool plug conical flask, the accurate methyl alcohol 25ml that adds claims to decide weight, soaked 3-5 hour, and sonicated 15-25 minute, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, the accurate subsequent filtrate 2ml that draws puts in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The per unit amount contains the radix paeoniae rubrathe with Paeoniflorin (C
23H
28O
11) meter, must not be less than 27-31.5mg.
This method of quality control can carry out effective quality control to anti-cerebral-thrombosis tablet.The former cerebral thrombus tablet quality of the Sanitation Ministry medicine standard standard only differentiates to cow-bezoar in the prescription that this method of quality control has increased the thin layer of leech on the proper mass standard base differentiates, and to effective constituent Paeoniflorin (C in the preparation
23H
28O
11) carry out assay with high performance liquid chromatography, regulation per unit amount contains the radix paeoniae rubrathe with Paeoniflorin (C
23H
28O
11) meter, must not be less than 27-31.5mg.Thereby clever tablet quality has carried out effective control to quenching one's thirst.
Embodiment 1
Safflower 90g; Radix Angelicae Sinensis 90g; leech (system) 90g; red spoon 90g; peach kernel 90g; Ligusticum wallichii 90g; red sage root 90g; ground bettle 22.5g; antelope's horn 11.25g; cow-bezoar 1.25g; more than ten the flavor; the radix paeoniae rubrathe; leech is ground into fine powder; the safflower poach is condensed into cream twice; Radix Angelicae Sinensis; Ligusticum wallichii; the red sage root; peach kernel; the five tastes such as ground bettle are with twice of 70% alcohol extract; be condensed into cream, with above water; the alcohol condensed cream merges, with the radix paeoniae rubrathe; leech fine powder and right amount of auxiliary materials are mixed; add antelope's horn; the cow-bezoar fine powder; mixing is made particle, drying; make 1000; the bag film-coating promptly gets anti-cerebral-thrombosis tablet, and is oral; one time 6; 3 times on the one, every heavy 0.31g, quite raw medicinal material 0.875g.To take the said preparation output that the crude drug amount calculates every day is that unit quantity is 18.
The method of quality control of anti-cerebral-thrombosis tablet is: a. differentiates: get this preparation 5/9 unit quantity, porphyrize places conical flask, added the 40ml alcohol immersion 4 hours, sonicated 30 minutes leaves standstill cooling, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, place separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, the photograph thin-layered chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution respectively, put in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, under the 254nm ultraviolet lamp, inspect, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material with 7: 1: 1 ethyl acetate one glacial acetic acid one water;
B. assay: measure according to high performance liquid chromatography (" 2000 editions appendix VID of Chinese pharmacopoeia), chromatographic condition is tested with system suitability: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution was a moving phase in 18: 82; The detection wavelength is 230nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 36 hours Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; This preparation under the content uniformity item is got in the preparation of need testing solution, removes dressing, porphyrize, get fine powder 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, claim to decide weight, soaked sonicated 20 minutes 4 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, the accurate subsequent filtrate 2ml that draws, put in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; This preparation per unit amount contains the radix paeoniae rubrathe with Paeoniflorin (C
23H
28O
11) meter, must not be less than 29.7mg.
Claims (6)
1, a kind of method of quality control of making the clinical practice formulation by the described anti-cerebral-thrombosis tablet prescription of Chinese Pharmacopoeia, it is characterized in that the discrimination method in this method is: get 5/9 unit quantity preparation, porphyrize, place conical flask, added the 40ml alcohol immersion 3-5 hour, sonicated 25-35 minute, leave standstill cooling, filter, the filtrate evaporate to dryness, residue adds 10ml water makes dissolving, places separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, according to the thin-layered chromatography test, draws each 10 μ l of above-mentioned two kinds of solution respectively, puts in same silica G F respectively
254On the thin layer plate, with 6-9: 0.5-2: 0.5-2 ethyl acetate one glacial acetic acid one water is developping agent, launches, and takes out, and dries, and inspects under the 240-260nm ultraviolet lamp, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material.
2, method of quality control as claimed in claim 1 is characterized in that the discrimination method in this method is:
Get preparation 5/9 unit quantity, porphyrize places conical flask, added the 40ml alcohol immersion 4 hours, sonicated 30 minutes leaves standstill cooling, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, place separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, according to the thin-layered chromatography test, draws each 10 μ l of above-mentioned two kinds of solution respectively, puts in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, under the 254nm ultraviolet lamp, inspect, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material with 7: 1: 1 ethyl acetate one glacial acetic acid one water.
3, method of quality control as claimed in claim 1, it is characterized in that content assaying method is: with octadecylsilane chemically bonded silica is filling agent; 16-20: 78-90 acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution is a moving phase, and the detection wavelength is 220-240nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 30-40 hour Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; Preparation 1.5g under the content uniformity item is got in the preparation of need testing solution, and accurate the title decides, put in the tool plug conical flask, the accurate methyl alcohol 25ml that adds claims to decide weight, soaked 3-5 hour, and sonicated 15-25 minute, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, the accurate subsequent filtrate 2ml that draws puts in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The per unit amount contains the radix paeoniae rubrathe in Paeoniflorin, must not be less than 27-31.5mg.
4, method of quality control as claimed in claim 3 is characterized in that content assaying method is:
With octadecylsilane chemically bonded silica is filling agent; Acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution was a moving phase in 18: 82; The detection wavelength is 230nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 36 hours Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; This preparation under the content uniformity item is got in the preparation of need testing solution, removes dressing, porphyrize, get fine powder 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, claim to decide weight, soaked sonicated 20 minutes 4 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, the accurate subsequent filtrate 2ml that draws, put in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; Preparation per unit amount contains the radix paeoniae rubrathe in Paeoniflorin, must not be less than 29.7mg.
5, method of quality control as claimed in claim 1 is characterized in that this method may further comprise the steps:
A. differentiate: get 5/9 unit quantity preparation, porphyrize places conical flask, add the 40ml alcohol immersion 3-5 hour, and sonicated 25-35 minute, left standstill cooling, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, place separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, according to the thin-layered chromatography test, draws each 10 μ l of above-mentioned two kinds of solution respectively, puts in same silica G F respectively
254On the thin layer plate, with 6-9: 0.5-2: 0.5-2 ethyl acetate one glacial acetic acid one water is developping agent, launches, and takes out, and dries, and inspects under the 240-260nm ultraviolet lamp, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material.
B. assay: with octadecylsilane chemically bonded silica is filling agent; 16-20: 78-90 acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution is a moving phase, and the detection wavelength is 220-240nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 30-40 hour Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; Preparation 1.5g under the content uniformity item is got in the preparation of need testing solution, and accurate the title decides, put in the tool plug conical flask, the accurate methyl alcohol 25ml that adds claims to decide weight, soaked 3-5 hour, and sonicated 15-25 minute, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, the accurate subsequent filtrate 2ml that draws puts in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The per unit amount contains the radix paeoniae rubrathe in Paeoniflorin, must not be less than 27-31.5mg.
6, method of quality control as claimed in claim 5 is characterized in that this method may further comprise the steps:
A. differentiate: get preparation 5/9 unit quantity, porphyrize places conical flask, added the 40ml alcohol immersion 4 hours, sonicated 30 minutes leaves standstill cooling, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, place separating funnel, with three each 5ml of extracted with diethyl ether, discard ether solution, with the water liquid evaporate to dryness after the extraction, residue adds 1ml ethanol makes dissolving, as need testing solution; Water intaking leech medicinal material shines medicinal material solution in pairs with legal system, according to the thin-layered chromatography test, draws each 10 μ l of above-mentioned two kinds of solution respectively, puts in same silica G F respectively
254On the thin layer plate, be developping agent, launch, take out, dry, under the 254nm ultraviolet lamp, inspect, in the test sample chromatogram, at the identical fluorescent quenching spot of the position display identical with control medicinal material with 7: 1: 1 ethyl acetate one glacial acetic acid one water;
B. assay: according to high effective liquid chromatography for measuring, chromatographic condition is tested with system suitability: with octadecylsilane chemically bonded silica is filling agent; Acetonitrile-0.05mol/L potassium dihydrogen phosphate aqueous solution was a moving phase in 18: 82; The detection wavelength is 230nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 2000; It is an amount of that the preparation of reference substance solution, precision take by weighing in the phosphorus pentoxide vacuum drying apparatus dry 36 hours Paeoniflorin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, promptly; This preparation under the content uniformity item is got in the preparation of need testing solution, removes dressing, porphyrize, get fine powder 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, claim to decide weight, soaked sonicated 20 minutes 4 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, the accurate subsequent filtrate 2ml that draws, put in the 10ml volumetric flask, add methyl alcohol and be diluted to scale, promptly; Assay method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get preparation per unit amount and contain the radix paeoniae rubrathe in Paeoniflorin, must not be less than 29.7mg.
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| CN 03121889 CN1239905C (en) | 2003-04-17 | 2003-04-17 | Method for control quality of Chinese medicinal preparation |
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| CN 03121889 CN1239905C (en) | 2003-04-17 | 2003-04-17 | Method for control quality of Chinese medicinal preparation |
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| CN1239905C CN1239905C (en) | 2006-02-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703524B (en) * | 2009-12-09 | 2011-01-12 | 鲁南制药集团股份有限公司 | Quality control method for leech and preparation containing leech |
| CN102305841A (en) * | 2010-11-02 | 2012-01-04 | 河北以岭医药研究院有限公司 | Method for identifying enhanced fluorescent thin layer of calculus bovis factitius |
| CN103698464A (en) * | 2014-01-13 | 2014-04-02 | 吉林省通化博祥药业股份有限公司 | Anti-cerebral-thrombosis tablet quality standard |
| CN107930191A (en) * | 2017-11-29 | 2018-04-20 | 江苏康缘药业股份有限公司 | A kind of sweet wormwood concentrate alcohol precipitation course control method for use |
-
2003
- 2003-04-17 CN CN 03121889 patent/CN1239905C/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703524B (en) * | 2009-12-09 | 2011-01-12 | 鲁南制药集团股份有限公司 | Quality control method for leech and preparation containing leech |
| CN102305841A (en) * | 2010-11-02 | 2012-01-04 | 河北以岭医药研究院有限公司 | Method for identifying enhanced fluorescent thin layer of calculus bovis factitius |
| CN103698464A (en) * | 2014-01-13 | 2014-04-02 | 吉林省通化博祥药业股份有限公司 | Anti-cerebral-thrombosis tablet quality standard |
| CN107930191A (en) * | 2017-11-29 | 2018-04-20 | 江苏康缘药业股份有限公司 | A kind of sweet wormwood concentrate alcohol precipitation course control method for use |
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| Publication number | Publication date |
|---|---|
| CN1239905C (en) | 2006-02-01 |
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