CN102018755A - 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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- 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
- Authority
- CN
- China
- Prior art keywords
- berberine
- solution
- furan
- radix sophorae
- sophorae flavescentis
- Prior art date
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 title claims abstract description 117
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229940093265 berberine Drugs 0.000 title claims abstract description 82
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000001514 detection method Methods 0.000 title claims abstract description 10
- MFYSUUPKMDJYPF-UHFFFAOYSA-N 2-[(4-methyl-2-nitrophenyl)diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC1=CC=C(C)C=C1[N+]([O-])=O MFYSUUPKMDJYPF-UHFFFAOYSA-N 0.000 title abstract 3
- 241000219784 Sophora Species 0.000 title abstract 3
- 239000003826 tablet Substances 0.000 claims abstract description 70
- PLHJDBGFXBMTGZ-WEVVVXLNSA-N furazolidone Chemical compound O1C([N+](=O)[O-])=CC=C1\C=N\N1C(=O)OCC1 PLHJDBGFXBMTGZ-WEVVVXLNSA-N 0.000 claims abstract description 50
- 229960001625 furazolidone Drugs 0.000 claims abstract description 50
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000007941 film coated tablet Substances 0.000 claims abstract description 7
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 84
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 66
- 238000012360 testing method Methods 0.000 claims description 60
- 238000000034 method Methods 0.000 claims description 59
- 239000013558 reference substance Substances 0.000 claims description 48
- 238000005303 weighing Methods 0.000 claims description 42
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000000047 product Substances 0.000 claims description 31
- 239000000706 filtrate Substances 0.000 claims description 30
- VKJGBAJNNALVAV-UHFFFAOYSA-M Berberine chloride (TN) Chemical compound [Cl-].C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 VKJGBAJNNALVAV-UHFFFAOYSA-M 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000012085 test solution Substances 0.000 claims description 18
- 238000003556 assay Methods 0.000 claims description 15
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
- 239000000741 silica gel Substances 0.000 claims description 12
- 229910002027 silica gel Inorganic materials 0.000 claims description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 238000004809 thin layer chromatography Methods 0.000 claims description 12
- 238000007689 inspection Methods 0.000 claims description 11
- 230000029087 digestion Effects 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 claims description 6
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- XEYBHCRIKKKOSS-UHFFFAOYSA-N disodium;azanylidyneoxidanium;iron(2+);pentacyanide Chemical compound [Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].[O+]#N XEYBHCRIKKKOSS-UHFFFAOYSA-N 0.000 claims description 6
- 238000010812 external standard method Methods 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- 230000002045 lasting effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229930014456 matrine Natural products 0.000 claims description 6
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229940083618 sodium nitroprusside Drugs 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000011003 system suitability test Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 238000000184 acid digestion Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract 2
- 235000019658 bitter taste Nutrition 0.000 abstract 1
- 230000007012 clinical effect Effects 0.000 abstract 1
- 239000008298 dragée Substances 0.000 abstract 1
- 239000007888 film coating Substances 0.000 abstract 1
- 238000009501 film coating Methods 0.000 abstract 1
- 238000002798 spectrophotometry method Methods 0.000 abstract 1
- 239000007940 sugar coated tablet Substances 0.000 abstract 1
- 238000009495 sugar coating Methods 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 208000004429 Bacillary Dysentery Diseases 0.000 description 3
- 208000004232 Enteritis Diseases 0.000 description 3
- 206010017915 Gastroenteritis shigella Diseases 0.000 description 3
- 201000005113 shigellosis Diseases 0.000 description 3
- 206010000087 Abdominal pain upper Diseases 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 2
- 206010057071 Rectal tenesmus Diseases 0.000 description 2
- 239000002260 anti-inflammatory agent Substances 0.000 description 2
- 229940124599 anti-inflammatory drug Drugs 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 208000027503 bloody stool Diseases 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 208000001848 dysentery Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 208000035861 hematochezia Diseases 0.000 description 2
- XYKIUTSFQGXHOW-UHFFFAOYSA-N propan-2-one;toluene Chemical compound CC(C)=O.CC1=CC=CC=C1 XYKIUTSFQGXHOW-UHFFFAOYSA-N 0.000 description 2
- 208000012271 tenesmus Diseases 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
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- 241000233866 Fungi Species 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 206010009887 colitis Diseases 0.000 description 1
- 210000001072 colon Anatomy 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
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- 150000002240 furans Chemical class 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 208000028774 intestinal disease Diseases 0.000 description 1
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- Nitrogen Condensed Heterocyclic Rings (AREA)
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) 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.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| 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 |
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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 |
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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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