CN1824250A - Quality control method of scourge repelling capsule - Google Patents
Quality control method of scourge repelling capsule Download PDFInfo
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- CN1824250A CN1824250A CN 200510132499 CN200510132499A CN1824250A CN 1824250 A CN1824250 A CN 1824250A CN 200510132499 CN200510132499 CN 200510132499 CN 200510132499 A CN200510132499 A CN 200510132499A CN 1824250 A CN1824250 A CN 1824250A
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- 238000003908 quality control method Methods 0.000 title claims abstract description 18
- 239000002775 capsule Substances 0.000 title claims abstract description 9
- 230000001846 repelling effect Effects 0.000 title 1
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 claims abstract description 18
- 239000003814 drug Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 40
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000000047 product Substances 0.000 claims description 30
- 238000012360 testing method Methods 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 21
- 239000013558 reference substance Substances 0.000 claims description 21
- NOOLISFMXDJSKH-UHFFFAOYSA-N p-menthan-3-ol Chemical compound CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000796 flavoring agent Substances 0.000 claims description 12
- 235000019634 flavors Nutrition 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004809 thin layer chromatography Methods 0.000 claims description 11
- 241000972155 Moschus Species 0.000 claims description 10
- 241000628997 Flos Species 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000003208 petroleum Substances 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- FZRCKLPSHGTOAU-UHFFFAOYSA-N 6-amino-1,4-dimethylcyclohexa-2,4-diene-1-carbaldehyde Chemical compound CC1=CC(N)C(C)(C=O)C=C1 FZRCKLPSHGTOAU-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 6
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007689 inspection Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- QXKXDIKCIPXUPL-UHFFFAOYSA-N sulfanylidenemercury Chemical compound [Hg]=S QXKXDIKCIPXUPL-UHFFFAOYSA-N 0.000 claims description 6
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 6
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 6
- 235000012141 vanillin Nutrition 0.000 claims description 6
- 239000000341 volatile oil Substances 0.000 claims description 6
- 238000003556 assay Methods 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 4
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005770 Eugenol Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- XGGLLRJQCZROSE-UHFFFAOYSA-K ammonium iron(iii) sulfate Chemical compound [NH4+].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGGLLRJQCZROSE-UHFFFAOYSA-K 0.000 claims description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 3
- RTEXIPZMMDUXMR-UHFFFAOYSA-N benzene;ethyl acetate Chemical compound CCOC(C)=O.C1=CC=CC=C1 RTEXIPZMMDUXMR-UHFFFAOYSA-N 0.000 claims description 3
- MDHYEMXUFSJLGV-UHFFFAOYSA-N beta-phenethyl acetate Natural products CC(=O)OCCC1=CC=CC=C1 MDHYEMXUFSJLGV-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 230000008034 disappearance Effects 0.000 claims description 3
- 125000004494 ethyl ester group Chemical group 0.000 claims description 3
- 229960002217 eugenol Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000002304 perfume Substances 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 235000013599 spices Nutrition 0.000 claims description 3
- 239000012085 test solution Substances 0.000 claims description 3
- 150000007970 thio esters Chemical class 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 1
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 abstract 1
- JHGWQSGWUPCKNT-UHFFFAOYSA-N 2-tert-butyl-4-methyl-1,3,5-trinitrobenzene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C(C(C)(C)C)=C1[N+]([O-])=O JHGWQSGWUPCKNT-UHFFFAOYSA-N 0.000 abstract 1
- 241000213006 Angelica dahurica Species 0.000 abstract 1
- 208000035473 Communicable disease Diseases 0.000 abstract 1
- 240000000513 Santalum album Species 0.000 abstract 1
- 235000008632 Santalum album Nutrition 0.000 abstract 1
- 230000001154 acute effect Effects 0.000 abstract 1
- 229940116229 borneol Drugs 0.000 abstract 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 abstract 1
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 229940079593 drug Drugs 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- 206010028748 Nasal obstruction Diseases 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 208000012886 Vertigo Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052956 cinnabar Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 201000003152 motion sickness Diseases 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000889 vertigo Toxicity 0.000 description 1
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- Medicinal Preparation (AREA)
Abstract
A Chinese medicine in the form of capsule for preventing acute infectious diseases is prepared from 13 Chinese-medicinal materials including sandal wood, dahurian angelica root, artificial musk, borneol, etc. Its quality control method is also disclosed.
Description
Technical field
The present invention relates to a kind of method of quality control of Chinese medicine preparation, be specifically related to the method for quality control of Chinese medicine BIWEN JIAONANG.
Background technology
The present invention relates to BIWEN JIAONANG, described BIWEN JIAONANG prescription is composed as follows: (prescription)
Lignum Santali Albi 26g Herba Lysimachiae foenum-graeci 3g Radix Angelicae Dahuricae 7g
Herba lysimachiae capillipedis 30g Rhizoma Curcumae Longae 3g Flos Rosae Rugosae 7g
Radix Et Rhizoma Nardostachyos 3g Flos Caryophylli 7g Radix Aucklandiae 6g
Artificial Moschus 0.23g Borneolum Syntheticum 23g Cinnabaris 110g
Mentholum 23g
(function and main method) dispel the administration keep away dirty, the pain relieving of having one's ideas straightened out.Be used for the vertigo that summer, pathogenic summer-heat caused, headache nasal obstruction is felt sick, is told, carsickness is seasick.
(usage and consumption) is oral, one time 2.External, content is an amount of, sucks the nostril.
(specification) every dress 0.25g Chinese medicine preparation for a long time, difficult quality is effectively controlled, and the quality of effectively controlling tcm product is a great problem, and the method for available technology adopting is imperfect, the minority specific aim is not strong, uses these methods to be difficult to reach the purpose of real control of quality.Above BIWEN JIAONANG is difficult to the quality of controlling agent owing to lack method of quality control well; Brought difficulty for normal production and operation, utilize more known technology to be difficult to the method for quality control that the said preparation product is provided, the present invention is directed to the deficiencies in the prior art, adopt new means that the quality of BIWEN JIAONANG is controlled, solved the difficult problem of said preparation quality control.The present invention is directed to BIWEN JIAONANG characteristics and
The present invention fills a prescription, and a kind of method of quality control of practicality is provided.
The present invention has proposed method of quality control to BIWEN JIAONANG.Quality standard after the raising can be controlled the quality of medicine better, and it is effective, quality controllable really to embody drug safety.
Summary of the invention
The invention provides a kind of method of quality control of BIWEN JIAONANG, this method comprises Borneolum Syntheticum in the preparation, Mentholum, and Flos Caryophylli, Lignum Santali Albi and contained chemical constituent thereof utilize thin layer chromatography to differentiate, and with the content of the cinnabar in the titration measuring Cinnabaris.
BIWEN JIAONANG of the present invention prepares by the following method:
BIWEN JIAONANG
(prescription) Lignum Santali Albi 26g Herba Lysimachiae foenum-graeci 3g Radix Angelicae Dahuricae 7g
Herba lysimachiae capillipedis 30g Rhizoma Curcumae Longae 3g Flos Rosae Rugosae 7g
Radix Et Rhizoma Nardostachyos 3g Flos Caryophylli 7g Radix Aucklandiae 6g
Artificial Moschus 0.23g Borneolum Syntheticum 23g Cinnabaris 110g
Above 13 flavors of Mentholum 23g (method for making), except that artificial Moschus, Borneolum Syntheticum, Mentholum, Cinnabaris water flies into impalpable powder, and it is done, and nine flavors such as Lignum Santali Albi are ground into fine powder, sieve, mixing.Borneolum Syntheticum, Herba Menthae with grinding to liquefaction, are stirred evenly.With artificial Moschus's porphyrize and the rotten facing-up of above-mentioned powder, sieve, mixing, even with liquid lapping-ins such as Borneolum Syntheticums, incapsulate.Make 1000, promptly.
Method of quality control of the present invention comprises character, differentiates, and the step of inspection and assay, wherein said discriminating is the characteristics at this medicine, its content is measured, to control the composition of its content.
Method of quality control of the present invention, step is as follows:
(character) this product and capsule, content are the vermilion powder, gas perfume (or spice), and flavor is cool.
It is tolerant that this product 1 intragranular is got in (discriminating) (1), adds the mixed liquor 4ml of hydrochloric acid-nitric acid (3: 1), stirs and make dissolving, puts to steam in the water-bath near and do, and adds water 2ml again, stirs and make dissolving, filters, and hydro-oxidation sodium test solution 1ml in the filtrate promptly generates the foresythia precipitation.
(2) get this product content 0.5g, put in the tool plug conical flask, add petroleum ether (60-90 ℃) 3ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Mentholum, Borneolum Syntheticum reference substance, adds petroleum ether (60-90 ℃) and makes the mixed solution that every 1ml contains 1mg.Product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B).Draw above-mentioned need testing solution 2 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with cyclohexane extraction-ether acid ethyl ester (17: 3), launch, and take out, and dry, and spray is with 2% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product content 5g, according to determination of volatile oil method (an appendix XD of Chinese Pharmacopoeia version in 2000 second method), add ethyl acetate 0.5ml, slowly be heated to and boil, and keep little and boiled about 30 minutes, get ethyl acetate liquid as need testing solution.Other gets the eugenol reference substance, add ethyl acetate and make the solution that every 1ml contains 2 μ l, product solution in contrast, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate (9: 1), launches, take out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 105 ℃, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical khaki fluorescence speckle.
(4) get this product content 5g, put when heating was waved to no Borneolum Syntheticum, Mentholum flavor in 3 hours in the water-bath,, add the solution that ethyl acetate 1ml contains 5 μ l, in contrast product solution according to determination of volatile oil method (an appendix X of Chinese Pharmacopoeia version in 2000 D first method).Draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 ℃)-ethyl acetate (85: 15) is developing solvent, launches, and takes out, dry, spray (is got paradime thylaminobenzaldehyde 0.25h, is dissolved among the glacial acetic acid 50g, add 85% phosphoric acid 5% and water 20ml with paradime thylaminobenzaldehyde solution, mixing), it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the principal spot of same color.
(inspection) should meet every regulation relevant under the capsule item (appendix IL of Chinese Pharmacopoeia version in 2000).(assay) gets the content 0.7g under the content uniformity item, and accurate the title decides, and puts in the conical flask, add thioesters 20ml and potassium nitrate 2.0g, straight fire heating keeps little boiling, after treating that solution becomes yellow, reheat 40 minutes is put cold, add water 50ml, put coldly, add 1% potassium permanganate solution to showing pink (redness is not moved back in 2 minutes), drip 2% copperas solution again to red the disappearance, add ammonium ferric sulfate indicator solution 2ml, with ammonium thiocyanate volumetric solution (0.1mol/L) titration, promptly.
The ammonium thiocyanate volumetric solution (0.1mol/L) of every 1ml is equivalent to the cinnabar (HgS) of 11.63mg.
Every of this product contains Cinnabaris in cinnabar (HgS), should be 95.0-115.0mg.
Method of quality control of the present invention is to utilize thin layer chromatography to differentiate each flavour of a drug in this compound preparation, detects simultaneously that content of effective has formed new method of quality control in the related content thing.This method has guaranteed that the BIWEN JIAONANG quality inspection standard can have accuracy and advance than the qualitative character of effectively controlling preparation comprehensively, can be used as the effective technology means of the stability of BIWEN JIAONANG quality control and investigation technology.Be of great importance to improving the quality of products.
The specific embodiment
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1
BIWEN JIAONANG
(prescription) Lignum Santali Albi 26g Herba Lysimachiae foenum-graeci 3g Radix Angelicae Dahuricae 7g
Herba lysimachiae capillipedis 30g Rhizoma Curcumae Longae 3g Flos Rosae Rugosae 7g
Radix Et Rhizoma Nardostachyos 3g Flos Caryophylli 7g Radix Aucklandiae 6g
Artificial Moschus 0.23g Borneolum Syntheticum 23g Cinnabaris 110g
Mentholum 23g
(method for making) above 13 flavors, except that artificial Moschus, Borneolum Syntheticum, Mentholum, Cinnabaris water flies into impalpable powder, and it is done, and nine flavors such as Lignum Santali Albi are ground into fine powder, sieve, mixing.Borneolum Syntheticum, Herba Menthae with grinding to liquefaction, are stirred evenly.With artificial Moschus's porphyrize and the rotten facing-up of above-mentioned powder, sieve, mixing, even with liquid lapping-ins such as Borneolum Syntheticums, incapsulate.Make 1000, promptly.
Embodiment 2
The capsule quality control method of embodiment 1, step is as follows:
(character) this product and capsule, content are the vermilion powder, gas perfume (or spice), and flavor is cool.
It is tolerant that this product 1 intragranular is got in (discriminating) (1), adds the mixed liquor 4ml of hydrochloric acid-nitric acid (3: 1), stirs and make dissolving, puts to steam in the water-bath near and do, and adds water 2ml again, stirs and make dissolving, filters, and hydro-oxidation sodium test solution 1ml in the filtrate promptly generates the foresythia precipitation.
(2) get this product content 0.5g, put in the tool plug conical flask, add petroleum ether (60-90 ℃) 3ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Mentholum, Borneolum Syntheticum reference substance, adds petroleum ether (60-90 ℃) and makes the mixed solution that every 1ml contains 1mg.Product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B).Draw above-mentioned need testing solution 2 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with cyclohexane extraction-ether acid ethyl ester (17: 3), launch, and take out, and dry, and spray is with 2% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product content 5g, according to determination of volatile oil method (an appendix X of Chinese Pharmacopoeia version in 2000 D second method), add ethyl acetate 0.5ml, slowly be heated to and boil, and keep little and boiled about 30 minutes, get ethyl acetate liquid as need testing solution.Other gets the eugenol reference substance, add ethyl acetate and make the solution that every 1ml contains 2 μ l, product solution in contrast, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate (9: 1), launches, take out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 105 ℃, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical khaki fluorescence speckle.
(4) get this product content 5g, put when heating was waved to no Borneolum Syntheticum, Mentholum flavor in 3 hours in the water-bath,, add the solution that ethyl acetate 1ml contains 5 μ l, in contrast product solution according to determination of volatile oil method (an appendix XD of Chinese Pharmacopoeia version in 2000 first method).Draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 ℃)-ethyl acetate (85: 15) is developing solvent, launches, and takes out, dry, spray (is got paradime thylaminobenzaldehyde 0.25h, is dissolved among the glacial acetic acid 50g, add 85% phosphoric acid 5% and water 20ml with paradime thylaminobenzaldehyde solution, mixing), it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the principal spot of same color.
(inspection) should meet every regulation relevant under the capsule item (appendix IL of Chinese Pharmacopoeia version in 2000).(assay) gets the content 0.7g under the content uniformity item, and accurate the title decides, and puts in the conical flask, add thioesters 20ml and potassium nitrate 2.0g, straight fire heating keeps little boiling, after treating that solution becomes yellow, reheat 40 minutes is put cold, add water 50ml, put coldly, add 1% potassium permanganate solution to showing pink (redness is not moved back in 2 minutes), drip 2% copperas solution again to red the disappearance, add ammonium ferric sulfate indicator solution 2ml, with ammonium thiocyanate volumetric solution (0.1mol/L) titration, promptly.
The ammonium thiocyanate volumetric solution (0.1mol/L) of every 1ml is equivalent to the cinnabar (HgS) of 11.63mg.Every of this product contains Cinnabaris in cinnabar (HgS), should be 95.0-115.0mg.
Claims (4)
1, a kind of method of quality control of Chinese medicine BIWEN JIAONANG is characterized in that, comprises character, differentiates the step of inspection and assay.
2, the method for claim 1 is characterized in that, described Chinese medicine BIWEN JIAONANG is made by following Chinese medicinal raw materials:
Lignum Santali Albi 26g Herba Lysimachiae foenum-graeci 3g Radix Angelicae Dahuricae 7g
Herba lysimachiae capillipedis 30g Rhizoma Curcumae Longae 3g Flos Rosae Rugosae 7g
Radix Et Rhizoma Nardostachyos 3g Flos Caryophylli 7g Radix Aucklandiae 6g
Artificial Moschus 0.23g Borneolum Syntheticum 23g Cinnabaris 110g
Mentholum 23g
3, the method for claim 1 is characterized in that, described Chinese medicine BIWEN JIAONANG, and prepare according to following method: except that artificial Moschus, Borneolum Syntheticum, Mentholum, Cinnabaris water flies into impalpable powder, and all the other Lignum Santali Albis etc. nine are distinguished the flavor of and are ground into fine powder, sieve, mixing; Borneolum Syntheticum, Mentholum are ground to liquefaction, stir evenly; With artificial Moschus's porphyrize and above-mentioned powder facing-up, sieve, mixing, even with liquid lapping-ins such as Borneolum Syntheticums, incapsulate.Make 1000, promptly.
4, the method for claim 1 is characterized in that, step is as follows:
(character) this product and capsule, content are the vermilion powder, gas perfume (or spice), and flavor is cool;
It is tolerant that this product 1 intragranular is got in (discriminating) (1), adds the mixed liquor 4ml of hydrochloric acid-nitric acid (3: 1), stirs and make dissolving, puts to steam in the water-bath near and do, and adds water 2ml again, stirs and make dissolving, filters, and hydro-oxidation sodium test solution 1ml in the filtrate promptly generates the foresythia precipitation;
(2) get this product content 0.5g, put in the tool plug conical flask, add petroleum ether (60-90 ℃) 3ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Mentholum, Borneolum Syntheticum reference substance, adds petroleum ether (60-90 ℃) and makes the mixed solution that every 1ml contains 1mg.Product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B).Draw above-mentioned need testing solution 2 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, are developing solvent with cyclohexane extraction-ether acid ethyl ester (17: 3), launch, and take out, and dry, and spray is with 2% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this product content 5g, according to determination of volatile oil method (an appendix X of Chinese Pharmacopoeia version in 2000 D second method), add ethyl acetate 0.5ml, slowly be heated to and boil, and keep little and boiled about 30 minutes, get ethyl acetate liquid as need testing solution.Other gets the eugenol reference substance, add ethyl acetate and make the solution that every 1ml contains 2 μ l, product solution in contrast, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate (9: 1), launches, take out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 105 ℃, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical khaki fluorescence speckle;
(4) get this product content 5g, put when heating was waved to no Borneolum Syntheticum, Mentholum flavor in 3 hours in the water-bath,, add the solution that ethyl acetate 1ml contains 5 μ l, in contrast product solution according to determination of volatile oil method (an appendix X of Chinese Pharmacopoeia version in 2000 D first method); Draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 ℃)-ethyl acetate (85: 15) is developing solvent, launches, and takes out, dry, spray (is got paradime thylaminobenzaldehyde 0.25h, is dissolved among the glacial acetic acid 50g, add 85% phosphoric acid 5% and water 20ml with paradime thylaminobenzaldehyde solution, mixing), it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the principal spot of same color;
(inspection) should meet every regulation relevant under the capsule item (appendix IL of Chinese Pharmacopoeia version in 2000); (assay) gets the content 0.7g under the content uniformity item, and accurate the title decides, and puts in the conical flask, add thioesters 20ml and potassium nitrate 2.0g, straight fire heating keeps little boiling, after treating that solution becomes yellow, reheat 40 minutes is put cold, add water 50ml, put coldly, add 1% potassium permanganate solution to showing pink (redness is not moved back in 2 minutes), drip 2% copperas solution again to red the disappearance, add ammonium ferric sulfate indicator solution 2ml, with ammonium thiocyanate volumetric solution (0.1mol/L) titration, promptly;
The ammonium thiocyanate volumetric solution (0.1mol/L) of every 1ml is equivalent to the cinnabar (HgS) of 11.63mg; Every of this product contains Cinnabaris in cinnabar (HgS), should be 95.0-115.0mg.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932469A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The discrimination method of borneol in a kind of hemorrhoid complicated by anal fistula lotion |
| CN109932470A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The alkalization method of silica G plate in a kind of traditional Chinese medicine of licorice root preparation indentification by TLC |
| CN112076302A (en) * | 2020-10-16 | 2020-12-15 | 贵州草喜堂医药有限公司 | Pestilence-avoiding fragrance-dispersing bag and production system thereof |
-
2005
- 2005-12-28 CN CNB2005101324992A patent/CN100364602C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932469A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The discrimination method of borneol in a kind of hemorrhoid complicated by anal fistula lotion |
| CN109932470A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The alkalization method of silica G plate in a kind of traditional Chinese medicine of licorice root preparation indentification by TLC |
| CN112076302A (en) * | 2020-10-16 | 2020-12-15 | 贵州草喜堂医药有限公司 | Pestilence-avoiding fragrance-dispersing bag and production system thereof |
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