CN102018755B - Quality detection method of furan lightyellow sophora root berberine tablet - Google Patents
Quality detection method of furan lightyellow sophora root berberine tablet Download PDFInfo
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Abstract
The invention discloses a quality detection method of a furan lightyellow sophora root berberine tablet. The quality detection method mainly comprises character, authentication, check and content measurement, wherein character comprises the following step of removing a sugar coating or a film coating from a sugar coated tablet or film coated tablet to show yellow color and bitter taste; content measurement comprises the following step of measuring the content of furazolidone and berberine in a preparation respectively according to spectrophotometry and high performance liquid chromatography. The quality detection method of the invention is scientific and reasonable, has high accuracy and good repeatability and can comprehensively and effectively control the quality of the furan lightyellow sophora root berberine tablet, and thus, the clinical effects of the preparation are ensured.
Description
Technical field
The present invention relates to the quality determining method of medicine, the quality determining method of especially a kind of (mystery) furans kuh-seng berberine tablet belongs to technical field of traditional Chinese medicines.
Background technology
Bacillary dysentery (abbreviation bacillary dysentery) is the common enteric infectious disease that is caused by shigella dysenteriae; Be characteristic with heating, stomachache, diarrhoea, tenesmus sense and mucopurulent bloody stool clinically, the infringement of its basic pathology is the congestion and edema of mucous membrane of colon, exudative inflammation such as hemorrhage.Enteritis is gastroenteritis, enteritis and the colitis that bacterium, virus, fungi and parasite etc. cause.That clinical manifestation has is nauseating, vomiting, stomachache, diarrhoea, rare water just or mucopurulent bloody stool.Part patient can have heating and tenesmus sensation, so also claim infectious diarrhea.Furans kuh-seng berberine tablet is a kind of antibiosis anti-inflammatory drug.Be used for acute bacillary dysentery, enteritis etc.The applicant studies this medicine, in the hope of exploring quality how effectively to control this medicine, to guarantee its clinical efficacy.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of quality determining method of furans kuh-seng berberine tablet.The quality determining method that the present invention formulated can be controlled the quality of furans kuh-seng berberine tablet fully and effectively, thereby guarantees the clinical efficacy of furans kuh-seng berberine tablet.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: the quality determining method of furans kuh-seng berberine tablet.Described furans kuh-seng berberine tablet is to process 1000 by furazolidone 31.5g, kuh-seng liquid extract 150g, berberine 32.5g and right amount of auxiliary materials; The quality determining method of furans kuh-seng berberine tablet mainly comprises proterties, discriminating, inspection, assay, and wherein assay is respectively according to AAS with according to the assay of high performance liquid chromatography to furazolidone in the preparation and berberine; Discriminating may further comprise the steps: (1) is got furans kuh-seng berberine tablet and is peelled off dressing, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, adds N; Dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shakes up, and filters; Get filtrating 1ml, add sodium nitroprusside test solution 1ml and sodium hydroxide test solution 1ml, shake up; Placed 2 minutes, solution just shows olive-green, fades to blackish green; (2) get furans kuh-seng berberine tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, in 10 minutes, does not disappear; (3) get furans kuh-seng berberine tablet fine powder 0.5g, add methyl alcohol 15ml, sonicated 30 minutes filters, and filtrating is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; According to the test of the thin-layered chromatography of two appendix VB of Chinese Pharmacopoeia version in 2005, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With acetone: toluene: ethyl acetate: strong aqua=3: 2: 1: 0.1 is developping agent, launches, and takes out; Dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram; With reference substance chromatogram relevant position on, show the spot of same color; (4) get need testing solution 0.5ml in the above-mentioned discriminating (3), be diluted to 5ml, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin-layered chromatography; Draw each 1～3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developping agent; Launch; Take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color.
The quality determining method of above-mentioned furans kuh-seng berberine tablet, the proterties of said quality determining method is: be sugar coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coating, bitter.
The quality determining method of aforementioned furans kuh-seng berberine tablet, the inspection of said quality determining method is: should meet each item regulation relevant under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item.
The quality determining method of aforementioned furans kuh-seng berberine tablet, the assay of said quality determining method may further comprise the steps:
(1) 10 of furans kuh-seng berberine tablets are got in furazolidone lucifuge operation, remove dressing, weigh; Porphyrize, precision take by weighing the fine powder that is equivalent to furazolidone 15mg, put in the 200ml measuring bottle, add N; Dinethylformamide 30ml dissolving, thin up shakes up to scale, filters; Precision is measured in subsequent filtrate 5ml to the 50ml volumetric flask, and thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, as reference substance solution; Get above-mentioned two kinds of solution,, measure absorbance log respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to two appendix IV of Chinese Pharmacopoeia version in 2005 A AAS;
Labelled amount %=(W
RΔ A
XP/31.5 * W
XΔ A
R) * 100%
In the formula: W
RWeighing (mg) for reference substance;
Δ A
RAbsorbance log difference (Δ A for reference substance
R2-Δ A
R1);
W
XWeigh (mg) for test sample;
Δ A
XAbsorbance log difference (Δ A for test sample
X2-Δ A
X1);
P is average sheet heavy (a mg/ sheet);
31.5 be the labelled amount (mg/ sheet) of furazolidone;
(2) berberine is according to two appendix VD of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; With methyl alcohol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a moving phase; The detection wavelength is 350nm, and number of theoretical plate calculates by the Berberine hydrochloride peak should be not less than 2000;
Determination method is got 10 of furans kuh-seng berberine tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to Berberine hydrochloride 10mg, puts in the 100ml volumetric flask; Add the 80ml that makes an appointment that flows, sonicated 45 minutes is put cold; Be diluted to scale with moving phase, shake up, filter; Get subsequent filtrate, precision is measured 10 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that precision takes by weighing the Berberine hydrochloride reference substance in addition, with moving phase dissolving and the quantitative solution of processing hydrochloric jamaicin 0.1mg among every 1ml that dilutes, measures with method,, promptly gets with calculated by peak area by external standard method.
The quality determining method of aforementioned furans kuh-seng berberine tablet, furans kuh-seng berberine tablet Furanzolidon-containing should be 90.0%～110.0% of labelled amount, and hydrochloric jamaicin should be 90.0%～110.0% of labelled amount.
The quality determining method of aforementioned furans kuh-seng berberine tablet, described kuh-seng liquid extract are preparations like this: get and choose clean kuh-seng, pulverize; The 1% aqueous sulfuric acid digestion 3 times that adds 6～8 times, the primary digestion time is 3 hours, secondary digestion time is 2 hours; The digestion time for the third time is 1 hour, filters merging filtrate respectively; And filtrating transferred to neutrality, concentrate liquid extract.
The quality determining method of aforementioned furans kuh-seng berberine tablet; On the whole; The quality determining method of furans kuh-seng berberine tablet mainly comprises proterties, discriminating, inspection, assay; Furans kuh-seng berberine tablet is to process 1000 by furazolidone 31.5g, kuh-seng liquid extract 150g, berberine 32.5g and right amount of auxiliary materials
[proterties] is sugar coated tablet or Film coated tablets, removes displaing yellow behind sugar-coat or the film-coating, bitter;
[discriminating] (1) is got furans kuh-seng berberine tablet and is peelled off dressing, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, adds N; Dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shakes up, and filters; Get filtrating 1ml, add sodium nitroprusside test solution 1ml and sodium hydroxide test solution 1ml, shake up; Placed 2 minutes, solution just shows olive-green, fades to blackish green;
(2) get furans kuh-seng berberine tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, in 10 minutes, does not disappear;
(3) get furans kuh-seng berberine tablet fine powder 0.5g, add methyl alcohol 15ml, sonicated 30 minutes filters, and filtrating is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; According to the test of the thin-layered chromatography of two appendix VB of Chinese Pharmacopoeia version in 2005, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With acetone: toluene: ethyl acetate: strong aqua=3: 2: 1: 0.1 is developping agent, launches, and takes out; Dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram; With reference substance chromatogram relevant position on, show the spot of same color;
(4) get need testing solution 0.5ml in the above-mentioned discriminating (3), be diluted to 5ml, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin-layered chromatography; Draw each 1～3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developping agent; Launch; Take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
[inspection] should meet each item regulation relevant under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item;
10 of furans kuh-seng berberine tablets are got in the operation of [assay] furazolidone lucifuge, remove dressing, weigh; Porphyrize, precision take by weighing the fine powder that is equivalent to furazolidone 15mg, put in the 200ml measuring bottle, add N; Dinethylformamide 30ml dissolving, thin up shakes up to scale, filters; Precision is measured in subsequent filtrate 5ml to the 50ml volumetric flask, and thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, as reference substance solution; Get above-mentioned two kinds of solution,, measure absorbance log respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to two appendix IV of Chinese Pharmacopoeia version in 2005 A AAS;
Labelled amount %=(W
RΔ A
XP/31.5 * W
XΔ A
R) * 100%
In the formula: W
RWeighing (mg) for reference substance;
Δ A
RAbsorbance log difference (Δ A for reference substance
R2-Δ A
R1);
W
XWeigh (mg) for test sample;
Δ A
XAbsorbance log difference (Δ A for test sample
X2-Δ A
X1);
P is average sheet heavy (a mg/ sheet);
31.5 be the labelled amount (mg/ sheet) of furazolidone;
Berberine is according to two appendix VD of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; With methyl alcohol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a moving phase; The detection wavelength is 350nm, and number of theoretical plate calculates by the Berberine hydrochloride peak should be not less than 2000;
Determination method is got 10 of furans kuh-seng berberine tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to Berberine hydrochloride 10mg, puts in the 100ml volumetric flask; Add the 80ml that makes an appointment that flows, sonicated 45 minutes is put cold; Be diluted to scale with moving phase, shake up, filter; Get subsequent filtrate, precision is measured 10 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that precision takes by weighing the Berberine hydrochloride reference substance in addition, with moving phase dissolving and the quantitative solution of processing hydrochloric jamaicin 0.1mg among every 1ml that dilutes, measures with method,, promptly gets with calculated by peak area by external standard method.
In order to verify feasibility of the present invention, the applicant has carried out following experimental study.
One, the research of proterties
According to ten lot sample article trial-production situation, furans kuh-seng berberine tablet (hereinafter to be referred as these article) proterties: be sugar coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coating, bitter.List the quality determining method text in.
Two, the research of discrimination method
(1) get these article and peel off dressing, porphyrize takes by weighing fine powder an amount of (being equivalent to furazolidone 10mg approximately), adds N; Dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shakes up, and filters; Get filtrating 1ml, add sodium nitroprusside test solution 1ml and sodium hydroxide test solution 1ml, shake up; Placed about 2 minutes, solution just shows olive-green, fades to blackish green.
(2) get these article, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, in 10 minutes, does not disappear.
(3) get these article fine powder 0.5g, add methyl alcohol 15ml, sonicated 30 minutes filters, and filtrating is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin-layered chromatography (two appendix VB of Chinese Pharmacopoeia version in 2005) test, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With acetone-toluene: ethyl acetate: strong aqua=3: 2: 1: 0.1 is developping agent, launches, and takes out; Dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram; With reference substance chromatogram relevant position on, show the spot of same color.
(4) get need testing solution 0.5ml in the discriminating 3, be diluted to 5ml, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.Test according to thin-layered chromatography (two appendix VB of Chinese Pharmacopoeia version in 2005); Draw each 1～3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developping agent; Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color.
Three, the research of inspection item
[inspection] should meet each item regulation (two appendix I of Chinese Pharmacopoeia version in 2005 A) relevant under the tablet item.
Four, the research of assay
Furazolidone (lucifuge operation) is got 10 of these article, removes dressing, weighs porphyrize; Precision takes by weighing in right amount (being equivalent to furazolidone 15mg approximately) and puts in the 200ml measuring bottle, adds N, dinethylformamide 30ml dissolving, and thin up is to scale; Shake up, filter, precision is measured in subsequent filtrate 5ml to the 50ml volumetric flask; Thin up shakes up to scale, as need testing solution.Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, as reference substance solution.Get above-mentioned two kinds of solution,, measure absorbance log respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to AAS (two appendix IV of Chinese Pharmacopoeia version in 2005 A).
Labelled amount %=(WR Δ AXP/31.5 * WX Δ AR) * 100%
In the formula: WR is the weighing (mg) of reference substance;
Δ AR is the absorbance log difference (Δ AR2-Δ AR1) of reference substance;
WX is weigh (mg) of test sample;
Δ AX is the absorbance log difference (Δ AX2-Δ AX1) of test sample;
P is average sheet heavy (a mg/ sheet);
31.5 be the labelled amount (mg/ sheet) of furazolidone;
Berberine is measured according to high performance liquid chromatography (two appendix VD of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; With methyl alcohol-acetonitrile-0.02mol/l phosphate aqueous solution [10: 27: 63] is moving phase; The detection wavelength is 350nm, and number of theoretical plate calculates by the Berberine hydrochloride peak should be not less than 2000.
Determination method is got 10 of these article, porphyrize, and precision takes by weighing in right amount (being equivalent to Berberine hydrochloride 10mg approximately), puts in the 100ml volumetric flask; Add the 80ml that makes an appointment that flows, sonicated 45 minutes (250W 30kHz) is put cold; Be diluted to scale with moving phase, shake up, filter; Get subsequent filtrate, precision is measured 10 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that precision takes by weighing the Berberine hydrochloride reference substance in addition, with moving phase dissolving and the quantitative solution of processing hydrochloric jamaicin 0.1mg among every 1ml that dilutes, measures with method,, promptly gets with calculated by peak area by external standard method.
Above experimental studies results shows that method of the present invention is reasonable, feasible, is control furans kuh-seng berberine tablet quality method preferably.
Beneficial effect of the present invention: compared with prior art, the present invention has set up the quality determining method of furans kuh-seng berberine tablet, and proterties, discriminating, inspection and the assay of furans kuh-seng berberine tablet are studied and screened; The quality determining method that is adopted is scientific and reasonable; Accuracy is high, and favorable reproducibility can be controlled the quality of furans kuh-seng berberine tablet fully and effectively; Reach the purpose of effective control drug quality, thereby guaranteed the clinical efficacy of said preparation.
Below in conjunction with embodiment the present invention is further described.
Embodiment
Embodiment.The quality determining method of furans kuh-seng berberine tablet.This furans kuh-seng berberine tablet is to process 1000 by furazolidone 31.5g, kuh-seng liquid extract 150g, berberine 32.5g and right amount of auxiliary materials.Kuh-seng liquid extract wherein is like this preparation: get and choose clean kuh-seng, take the circumstances into consideration to pulverize, add 6～8 times 1% aqueous sulfuric acid digestion 3 times; The primary digestion time is 3 hours, and secondary digestion time is 2 hours, and the digestion time for the third time is 1 hour; Filter respectively; Merging filtrate, and filtrating transferred to neutrality, concentrate liquid extract (every 1g liquid extract is equivalent to the 3g crude drug).
These article Furanzolidon-containing (C8H7N3O5) should be 90.0%～110.0% of labelled amount, and hydrochloric jamaicin (C20H18NO4) should be 90.0%～110.0% of labelled amount.
[proterties] these article are sugar coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coating, bitter.
[discriminating] (1) is got these article and is peelled off dressing, and porphyrize takes by weighing fine powder an amount of (being equivalent to furazolidone 10mg approximately), adds N; Dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shakes up, and filters; Get filtrating 1ml, add sodium nitroprusside test solution 1ml and sodium hydroxide test solution 1ml, shake up; Placed about 2 minutes, solution just shows olive-green, fades to blackish green.
(2) get these article, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, in 10 minutes, does not disappear.
(3) get these article fine powder 0.5g, add methyl alcohol 15ml, sonicated 30 minutes filters, and filtrating is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin-layered chromatography (two appendix VB of Chinese Pharmacopoeia version in 2005) test, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With acetone-toluene: ethyl acetate: strong aqua=3: 2: 1: 0.1 is developping agent, launches, and takes out; Dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram; With reference substance chromatogram relevant position on, show the spot of same color.
(4) get need testing solution 0.5ml in the discriminating 3, be diluted to 5ml, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.Test according to thin-layered chromatography (two appendix VB of Chinese Pharmacopoeia version in 2005); Draw each 1～3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developping agent; Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color.
[inspection] should meet each item regulation (two appendix I of Chinese Pharmacopoeia version in 2005 A) relevant under the tablet item.
[assay] furazolidone (lucifuge operation) is got 10 of these article, removes dressing, weighs porphyrize; Precision takes by weighing in right amount (being equivalent to furazolidone 15mg approximately) and puts in the 200ml measuring bottle, adds N, dinethylformamide 30ml dissolving, and thin up is to scale; Shake up, filter, precision is measured in subsequent filtrate 5ml to the 50ml volumetric flask; Thin up shakes up to scale, as need testing solution.Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, as reference substance solution.Get above-mentioned two kinds of solution,, measure absorbance log respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to AAS (two appendix IV of Chinese Pharmacopoeia version in 2005 A).
Labelled amount %=(WR Δ AXP/31.5 * WX Δ AR) * 100%
In the formula: WR is the weighing (mg) of reference substance;
Δ AR is the absorbance log difference (Δ AR2-Δ AR1) of reference substance;
WX is weigh (mg) of test sample;
Δ AX is the absorbance log difference (Δ AX2-Δ AX1) of test sample;
P is average sheet heavy (a mg/ sheet);
31.5 be the labelled amount (mg/ sheet) of furazolidone;
Berberine is measured according to high performance liquid chromatography (two appendix VD of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; With methyl alcohol-acetonitrile-0.02mol/l phosphate aqueous solution [10: 27: 63] is moving phase; The detection wavelength is 350nm, and number of theoretical plate calculates by the Berberine hydrochloride peak should be not less than 2000.
Determination method is got 10 of these article, porphyrize, and precision takes by weighing in right amount (being equivalent to Berberine hydrochloride 10mg approximately), puts in the 100ml volumetric flask; Add the 80ml that makes an appointment that flows, sonicated 45 minutes (250W 30kHz) is put cold; Be diluted to scale with moving phase, shake up, filter; Get subsequent filtrate, precision is measured 10 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that precision takes by weighing the Berberine hydrochloride reference substance in addition, with moving phase dissolving and the quantitative solution of processing hydrochloric jamaicin 0.1mg among every 1ml that dilutes, measures with method,, promptly gets with calculated by peak area by external standard method.
[classification] antibiosis anti-inflammatory drug.
[usage and dosage] 3-4 sheet, 2 times on the one, 3-5 days is a course of treatment.
[storage] lucifuge, sealing is preserved.
[term of validity] 24 months.
Embodiment of the present invention is not limited to the foregoing description, and the various variations of under the prerequisite that does not break away from aim of the present invention, making all belong within protection scope of the present invention.
Claims (2)
1. the detection method of a furans kuh-seng berberine tablet, it is characterized in that: the detection method of furans kuh-seng berberine tablet mainly comprises proterties, discriminating, inspection, assay; Furans kuh-seng berberine tablet is to process 1000 by furazolidone 31.5g, kuh-seng liquid extract 150g, berberine 32.5g and right amount of auxiliary materials; Described kuh-seng liquid extract is like this preparation: get and choose clean kuh-seng, pulverize, add 6～8 times 1% aqueous sulfuric acid digestion 3 times; The primary digestion time is 3 hours, and secondary digestion time is 2 hours, and the digestion time for the third time is 1 hour; Filter respectively; Merging filtrate, and filtrating transferred to neutrality, concentrate liquid extract;
[proterties] is sugar coated tablet or Film coated tablets, removes displaing yellow behind sugar-coat or the film-coating, bitter;
[discriminating] (1) is got furans kuh-seng berberine tablet and is peelled off dressing, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, adds N; Dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shakes up, and filters; Get filtrating 1ml, add sodium nitroprusside test solution 1ml and sodium hydroxide test solution 1ml, shake up; Placed 2 minutes, solution just shows olive-green, fades to blackish green;
(2) get furans kuh-seng berberine tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, in 10 minutes, does not disappear;
(3) get furans kuh-seng berberine tablet fine powder 0.5g, add methyl alcohol 15ml, sonicated 30 minutes filters, and filtrating is concentrated into 2ml, as need testing solution; Other gets the matrine reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; According to the test of the thin-layered chromatography of two appendix VB of Chinese Pharmacopoeia version in 2005, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; With acetone: toluene: ethyl acetate: strong aqua=3: 2: 1: 0.1 is developping agent, launches, and takes out; Dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram; With reference substance chromatogram relevant position on, show the spot of same color;
(4) get need testing solution 0.5ml in the above-mentioned discriminating (3), be diluted to 5ml, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin-layered chromatography; Draw each 1～3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developping agent; Launch; Take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the fluorescence spot of same color;
[inspection] should meet each item regulation relevant under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item;
10 of furans kuh-seng berberine tablets are got in the operation of [assay] furazolidone lucifuge, remove dressing, weigh; Porphyrize, precision take by weighing the fine powder that is equivalent to furazolidone 15mg, put in the 200ml measuring bottle, add N; Dinethylformamide 30ml dissolving, thin up shakes up to scale, filters; Precision is measured in subsequent filtrate 5ml to the 50ml volumetric flask, and thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, as reference substance solution; Get above-mentioned two kinds of solution,, measure absorbance log respectively, obtain △ A, calculate the content of furazolidone at 367nm and 438nm place according to two appendix IV of Chinese Pharmacopoeia version in 2005 A AAS;
Labelled amount %=(W
R△ A
XP/31.5 * W
X△ A
R) * 100%
In the formula: W
RBe the weighing of reference substance, its unit is mg;
△ A
RAbsorbance log difference (△ A for reference substance
R2– △ A
R1);
W
XBe weighing of test sample, its unit is mg;
△ A
XAbsorbance log difference (△ A for test sample
X2– △ A
X1);
P is that average sheet is heavy, and its unit is the mg/ sheet;
31.5 be the labelled amount of furazolidone, its unit is the mg/ sheet;
Berberine is according to two appendix VD of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; With methyl alcohol: acetonitrile: 0.02mol/l phosphate aqueous solution=10:27:63 is a moving phase; The detection wavelength is 350nm, and number of theoretical plate calculates by the Berberine hydrochloride peak should be not less than 2000;
Determination method is got 10 of furans kuh-seng berberine tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to Berberine hydrochloride 10mg, puts in the 100ml volumetric flask; Add moving phase 80ml, sonicated 45 minutes is put cold; Be diluted to scale with moving phase, shake up, filter; Get subsequent filtrate, precision is measured 10 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that precision takes by weighing the Berberine hydrochloride reference substance in addition, with moving phase dissolving and the quantitative solution of processing hydrochloric jamaicin 0.1mg among every 1ml that dilutes, measures with method,, promptly gets with calculated by peak area by external standard method.
2. the detection method of furans kuh-seng berberine tablet according to claim 1 is characterized in that: furans kuh-seng berberine tablet Furanzolidon-containing should be 90.0%～110.0% of labelled amount, and hydrochloric jamaicin should be 90.0%～110.0% of labelled amount.
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| CN106706617A (en) * | 2016-12-07 | 2017-05-24 | 百奥森（江苏）食品安全科技有限公司 | Detection method and kit for detecting furazolidone metabolite in animal tissues |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1766606A (en) * | 2005-11-09 | 2006-05-03 | 中国科学院长春应用化学研究所 | The component detection method of liquorice-ginseng capsule |
| CN1883604A (en) * | 2006-06-13 | 2006-12-27 | 贵州神奇集团控股有限公司 | Quality control method of compound preparation with red sage root and cape jasmine for treating acute and chronic hepatitis |
| CN1971265A (en) * | 2006-12-06 | 2007-05-30 | 中国科学院长春应用化学研究所 | Method for detecting component of compound 'Xialian' capsules |
| CN101259260A (en) * | 2008-04-17 | 2008-09-10 | 陕西康惠制药有限公司 | Quality detecting method of Chinese medicine for treating chronic atrophic gastritis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1766606A (en) * | 2005-11-09 | 2006-05-03 | 中国科学院长春应用化学研究所 | The component detection method of liquorice-ginseng capsule |
| CN1883604A (en) * | 2006-06-13 | 2006-12-27 | 贵州神奇集团控股有限公司 | Quality control method of compound preparation with red sage root and cape jasmine for treating acute and chronic hepatitis |
| CN1971265A (en) * | 2006-12-06 | 2007-05-30 | 中国科学院长春应用化学研究所 | Method for detecting component of compound 'Xialian' capsules |
| CN101259260A (en) * | 2008-04-17 | 2008-09-10 | 陕西康惠制药有限公司 | Quality detecting method of Chinese medicine for treating chronic atrophic gastritis |
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