CN102018755A - Quality detection method of furan lightyellow sophora root berberine tablet - Google Patents

Quality detection method of furan lightyellow sophora root berberine tablet Download PDF

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CN102018755A
CN102018755A CN 201010574307 CN201010574307A CN102018755A CN 102018755 A CN102018755 A CN 102018755A CN 201010574307 CN201010574307 CN 201010574307 CN 201010574307 A CN201010574307 A CN 201010574307A CN 102018755 A CN102018755 A CN 102018755A
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berberine
solution
furan
radix sophorae
sophorae flavescentis
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CN102018755B (en
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张芝庭
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Guizhou Shenqi Pharmaceutical Co ltd
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Shenqi Phamaceutical Co Ltd Guizhou
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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

The quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet
Technical field
The present invention relates to the quality determining method of medicine, the quality determining method of especially a kind of (mystery) furan Radix Sophorae Flavescentis Berberine Tablet belongs to technical field of Chinese medicines.
Background technology
Bacillary dysentery (abbreviation bacillary dysentery) is the common infectious intestinal disease that is caused by dysentery bacterium, be feature 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 antibacterial, virus, fungus 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.Furan Radix Sophorae Flavescentis 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 problem to be solved by this invention is to provide a kind of quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet.The quality determining method that the present invention formulated can be controlled the quality of furan Radix Sophorae Flavescentis Berberine Tablet fully and effectively, thereby guarantees the clinical efficacy of furan Radix Sophorae Flavescentis Berberine Tablet.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet.Described furan Radix Sophorae Flavescentis Berberine Tablet is to make 1000 by furazolidone 31.5g, Radix Sophorae Flavescentis fluid extract 150g, berberine 32.5g and right amount of auxiliary materials, the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet mainly comprises character, discriminating, inspection, assay, and wherein assay is respectively according to spectrophotography 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 furan Radix Sophorae Flavescentis Berberine Tablet and is peelled off coating, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 furan Radix Sophorae Flavescentis Berberine Tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes; (3) get furan Radix Sophorae Flavescentis Berberine Tablet fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Thin layer chromatography test according to 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 adhesive with the sodium carboxymethyl cellulose, with acetone: toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The quality determining method of above-mentioned furan Radix Sophorae Flavescentis Berberine Tablet, the character of described quality determining method is: be coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coat, bitter in the mouth.
The quality determining method of aforementioned furan Radix Sophorae Flavescentis Berberine Tablet, the inspection of described quality determining method is: should meet relevant every regulation under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item.
The quality determining method of aforementioned furan Radix Sophorae Flavescentis Berberine Tablet, the assay of described quality determining method may further comprise the steps:
(1) 10 of furan Radix Sophorae Flavescentis Berberine Tablets are got in furazolidone lucifuge operation, remove coating, weigh, porphyrize, precision takes 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, thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution; Get above-mentioned two kinds of solution,, measure trap 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 spectrophotography;
Labelled amount %=(W RΔ A XP/31.5 * W XΔ A R) * 100%
In the formula: W RWeighing (mg) for reference substance;
Δ A RTrap difference (Δ A for reference substance R2-Δ A R1);
W XWeigh (mg) for test sample;
Δ A XTrap 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 are filler with octadecylsilane chemically bonded silica, with methanol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000;
Algoscopy is got 10 of furan Radix Sophorae Flavescentis Berberine Tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to berberine hydrochloride 10mg, put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
The quality determining method of aforementioned furan Radix Sophorae Flavescentis Berberine Tablet, furan Radix Sophorae Flavescentis Berberine Tablet Furanzolidon-containing should be 90.0%~110.0% of labelled amount, and hydrochloric berberine should be 90.0%~110.0% of labelled amount.
The quality determining method of aforementioned furan Radix Sophorae Flavescentis Berberine Tablet, described Radix Sophorae Flavescentis fluid extract is preparation like this: get and choose clean Radix Sophorae Flavescentis, pulverize, add 6~8 times 1% aqueous sulfuric acid digestion 3 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 filtrate transferred to neutrality, concentrate fluid extract.
The quality determining method of aforementioned furan Radix Sophorae Flavescentis Berberine Tablet, on the whole, the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet mainly comprises character, discriminating, inspection, assay, furan Radix Sophorae Flavescentis Berberine Tablet is to make 1000 by furazolidone 31.5g, Radix Sophorae Flavescentis fluid extract 150g, berberine 32.5g and right amount of auxiliary materials
[character] is coated tablet or Film coated tablets, removes displaing yellow behind sugar-coat or the film-coat, bitter in the mouth;
[discriminating] (1) is got furan Radix Sophorae Flavescentis Berberine Tablet and is peelled off coating, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 furan Radix Sophorae Flavescentis Berberine Tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes;
(3) get furan Radix Sophorae Flavescentis Berberine Tablet fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Thin layer chromatography test according to 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 adhesive with the sodium carboxymethyl cellulose, with acetone: toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
[inspection] should meet relevant every regulation under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item;
10 of furan Radix Sophorae Flavescentis Berberine Tablets are got in the operation of [assay] furazolidone lucifuge, remove coating, weigh, porphyrize, precision takes 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, thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution; Get above-mentioned two kinds of solution,, measure trap 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 spectrophotography;
Labelled amount %=(W RΔ A XP/31.5 * W XΔ A R) * 100%
In the formula: W RWeighing (mg) for reference substance;
Δ A RTrap difference (Δ A for reference substance R2-Δ A R1);
W XWeigh (mg) for test sample;
Δ A XTrap 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 are filler with octadecylsilane chemically bonded silica, with methanol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000;
Algoscopy is got 10 of furan Radix Sophorae Flavescentis Berberine Tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to berberine hydrochloride 10mg, put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
In order to verify feasibility of the present invention, the applicant has carried out following experimentation.
One, the research of character
According to ten batch samples trial-production situation, furan Radix Sophorae Flavescentis Berberine Tablet (hereinafter to be referred as this product) character: be coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coat, bitter in the mouth.List the quality determining method text in.
Two, the research of discrimination method
(1) get this product and peel off coating, porphyrize takes by weighing fine powder an amount of (being equivalent to furazolidone 10mg approximately), add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 this product, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes.
(3) get this product fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (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 adhesive with the sodium carboxymethyl cellulose, with acetone-toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Three, check the research of item
[inspection] should meet every regulation relevant under the tablet item (two appendix I of Chinese Pharmacopoeia version in 2005 A).
Four, the research of assay
Furazolidone (lucifuge operation) is got 10 of this product, removes coating, weighs, porphyrize, precision take by weighing in right amount (being equivalent to furazolidone 15mg approximately) and 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, thin up shakes up to scale, as need testing solution.Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution.Get above-mentioned two kinds of solution,, measure trap respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to spectrophotography (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 trap difference (Δ AR2-Δ AR1) of reference substance;
WX is weigh (mg) of test sample;
Δ AX is the trap 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 are filler with octadecylsilane chemically bonded silica, with methanol-acetonitrile-0.02mol/l phosphate aqueous solution [10: 27: 63] is mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000.
Algoscopy is got 10 of this product, porphyrize, and precision takes by weighing in right amount (being equivalent to berberine hydrochloride 10mg approximately), put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes (250W 30kHz) is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
Above experimental studies results shows that method of the present invention is reasonable, feasible, is control furan Radix Sophorae Flavescentis 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 furan Radix Sophorae Flavescentis Berberine Tablet, character, discriminating, inspection and assay to furan Radix Sophorae Flavescentis Berberine Tablet are studied and are screened, the quality determining method that is adopted is scientific and reasonable, the accuracy height, favorable reproducibility can be controlled the quality of furan Radix Sophorae Flavescentis Berberine Tablet fully and effectively, reach the purpose of effective control drug quality, thereby guaranteed the clinical efficacy of said preparation.
The present invention is further illustrated below in conjunction with the specific embodiment.
The specific embodiment
Embodiment.The quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet.This furan Radix Sophorae Flavescentis Berberine Tablet is to make 1000 by furazolidone 31.5g, Radix Sophorae Flavescentis fluid extract 150g, berberine 32.5g and right amount of auxiliary materials.Radix Sophorae Flavescentis fluid extract wherein is preparation like this: get and choose clean Radix Sophorae Flavescentis, take the circumstances into consideration to pulverize, the 1% aqueous sulfuric acid digestion 3 times that adds 6~8 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 filtrate transferred to neutrality, concentrate fluid extract (every 1g fluid extract is equivalent to the 3g crude drug).
This product Furanzolidon-containing (C8H7N3O5) should be 90.0%~110.0% of labelled amount, and hydrochloric berberine (C20H18NO4) should be 90.0%~110.0% of labelled amount.
[character] this product is coated tablet or Film coated tablets, removes displaing yellow behind sugar-coat or the film-coat, bitter in the mouth.
[discriminating] (1) is got this product and is peelled off coating, and porphyrize takes by weighing fine powder an amount of (being equivalent to furazolidone 10mg approximately), add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 this product, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes.
(3) get this product fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (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 adhesive with the sodium carboxymethyl cellulose, with acetone-toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet every regulation relevant under the tablet item (two appendix I of Chinese Pharmacopoeia version in 2005 A).
[assay] furazolidone (lucifuge operation) is got 10 of this product, removes coating, weighs, porphyrize, precision take by weighing in right amount (being equivalent to furazolidone 15mg approximately) and 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, thin up shakes up to scale, as need testing solution.Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution.Get above-mentioned two kinds of solution,, measure trap respectively, obtain Δ A, calculate the content of furazolidone at 367nm and 438nm place according to spectrophotography (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 trap difference (Δ AR2-Δ AR1) of reference substance;
WX is weigh (mg) of test sample;
Δ AX is the trap 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 are filler with octadecylsilane chemically bonded silica, with methanol-acetonitrile-0.02mol/l phosphate aqueous solution [10: 27: 63] is mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000.
Algoscopy is got 10 of this product, porphyrize, and precision takes by weighing in right amount (being equivalent to berberine hydrochloride 10mg approximately), put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes (250W 30kHz) is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
[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.
[effect duration] 24 months.
Embodiments of the present invention are not limited to the foregoing description, and the various variations of making under the prerequisite that does not break away from aim of the present invention all belong within protection scope of the present invention.

Claims (7)

1. the quality determining method of a furan Radix Sophorae Flavescentis Berberine Tablet, described furan Radix Sophorae Flavescentis Berberine Tablet is to make 1000 by furazolidone 31.5g, Radix Sophorae Flavescentis fluid extract 150g, berberine 32.5g and right amount of auxiliary materials, it is characterized in that: described quality determining method mainly comprises character, discriminating, inspection, assay, and wherein assay is respectively according to spectrophotography with according to the assay of high performance liquid chromatography to furazolidone in the preparation and berberine; Discriminating may further comprise the steps:
(1) get furan Radix Sophorae Flavescentis Berberine Tablet and peel off coating, porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 furan Radix Sophorae Flavescentis Berberine Tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes;
(3) get furan Radix Sophorae Flavescentis Berberine Tablet fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Thin layer chromatography test according to 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 adhesive with the sodium carboxymethyl cellulose, with acetone: toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
2. the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet according to claim 1 is characterized in that: the character in the described quality determining method: be coated tablet or Film coated tablets, remove displaing yellow behind sugar-coat or the film-coat, bitter in the mouth.
3. the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet according to claim 1 is characterized in that: the inspection in the described quality determining method: should meet relevant every regulation under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item.
4. the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet according to claim 1 is characterized in that: the assay in the described quality determining method may further comprise the steps:
10 of furan Radix Sophorae Flavescentis Berberine Tablets are got in the operation of furazolidone lucifuge, remove coating, weigh, porphyrize, precision takes 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, thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution; Get above-mentioned two kinds of solution,, measure trap 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 spectrophotography;
Labelled amount %=(W RΔ A XP/31.5 * W XΔ A R) * 100%
In the formula: W RWeighing (mg) for reference substance;
Δ A RTrap difference (Δ A for reference substance R2-Δ A R1);
W XWeigh (mg) for test sample;
Δ A XTrap 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 are filler with octadecylsilane chemically bonded silica, with methanol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000;
Algoscopy is got 10 of furan Radix Sophorae Flavescentis Berberine Tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to berberine hydrochloride 10mg, put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
5. the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet according to claim 4 is characterized in that: furan Radix Sophorae Flavescentis Berberine Tablet Furanzolidon-containing should be 90.0%~110.0% of labelled amount, and hydrochloric berberine should be 90.0%~110.0% of labelled amount.
6. the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet according to claim 1, it is characterized in that: described Radix Sophorae Flavescentis fluid extract is preparation like this: get and choose clean Radix Sophorae Flavescentis, pulverize, add 6~8 times 1% aqueous sulfuric acid digestion 3 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 filtrate transferred to neutrality, concentrate fluid extract.
7. according to the quality determining method of claim 2,3 or 4 described furan Radix Sophorae Flavescentis Berberine Tablets, it is characterized in that: the quality determining method of furan Radix Sophorae Flavescentis Berberine Tablet mainly comprises character, discriminating, inspection, assay; Furan Radix Sophorae Flavescentis Berberine Tablet is to make 1000 by furazolidone 31.5g, Radix Sophorae Flavescentis fluid extract 150g, berberine 32.5g and right amount of auxiliary materials;
[character] is coated tablet or Film coated tablets, removes displaing yellow behind sugar-coat or the film-coat, bitter in the mouth;
[discriminating] (1) is got furan Radix Sophorae Flavescentis Berberine Tablet and is peelled off coating, and porphyrize takes by weighing the fine powder that is equivalent to furazolidone 10mg, add N, dinethylformamide 1ml dissolves furazolidone fully, adds water 50ml, shake up, filter, get filtrate 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 furan Radix Sophorae Flavescentis Berberine Tablet, porphyrize takes by weighing 0.5g, adds hot water 10ml, and powerful jolting one minute promptly produces lasting foam, does not disappear in 10 minutes;
(3) get furan Radix Sophorae Flavescentis Berberine Tablet fine powder 0.5g, add methanol 15ml, supersound process 30 minutes filters, and filtrate is concentrated into about 2ml, as need testing solution; Other gets the matrine reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Thin layer chromatography test according to 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 adhesive with the sodium carboxymethyl cellulose, with acetone: toluene: ethyl acetate: strong aqua ammonia=3: 2: 1: 0.1 is developing solvent, launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to two appendix VB of Chinese Pharmacopoeia version in 2005 thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ethyl acetate: butanone: formic acid: water=10: 6: 1: 1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
[inspection] should meet relevant every regulation under two appendix I of Chinese Pharmacopoeia version in 2005 A tablet item;
10 of furan Radix Sophorae Flavescentis Berberine Tablets are got in the operation of [assay] furazolidone lucifuge, remove coating, weigh, porphyrize, precision takes 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, thin up shakes up to scale, as need testing solution; Other precision takes by weighing furazolidone reference substance 15mg and prepares with method, in contrast product solution; Get above-mentioned two kinds of solution,, measure trap 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 spectrophotography;
Labelled amount %=(W RΔ A XP/31.5 * W XΔ A R) * 100%
In the formula: W RWeighing (mg) for reference substance;
Δ A RTrap difference (Δ A for reference substance R2-Δ A R1);
W XWeigh (mg) for test sample;
Δ A XTrap 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 are filler with octadecylsilane chemically bonded silica, with methanol: acetonitrile: 0.02mol/l phosphate aqueous solution=10: 27: 63 is a mobile phase, the detection wavelength is 350nm, and number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000;
Algoscopy is got 10 of furan Radix Sophorae Flavescentis Berberine Tablets, porphyrize, and precision takes by weighing the fine powder that is equivalent to berberine hydrochloride 10mg, put in the 100ml volumetric flask, add the 80ml that makes an appointment that flows, supersound process 45 minutes is put cold, be diluted to scale with mobile phase, shake up, filter, get subsequent filtrate, precision is measured 10 μ l and is injected chromatograph of liquid, the record chromatogram; It is an amount of that precision takes by weighing the berberine hydrochloride reference substance in addition, with the solution that mobile phase is dissolved and quantitatively hydrochloric berberine 0.1mg among every 1ml is made in dilution, measures with method, presses external standard method with calculated by peak area, promptly.
CN201010574307A 2010-12-06 2010-12-06 Quality detection method of furan lightyellow sophora root berberine tablet Expired - Fee Related CN102018755B (en)

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CN106404960A (en) * 2016-11-21 2017-02-15 吉林师范大学 Quality detection method of furan sophora berberine tablets
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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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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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
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CN106404960A (en) * 2016-11-21 2017-02-15 吉林师范大学 Quality detection method of furan sophora berberine tablets
CN106404960B (en) * 2016-11-21 2018-11-06 吉林师范大学 The quality determining method of furan lightyellow sophora root berberine tablet
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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