CN103869041B - A kind of detection method of cough-relieving combination of oral medication - Google Patents
A kind of detection method of cough-relieving combination of oral medication Download PDFInfo
- Publication number
- CN103869041B CN103869041B CN201210549017.3A CN201210549017A CN103869041B CN 103869041 B CN103869041 B CN 103869041B CN 201210549017 A CN201210549017 A CN 201210549017A CN 103869041 B CN103869041 B CN 103869041B
- Authority
- CN
- China
- Prior art keywords
- solution
- developing solvent
- volume ratio
- mixed solution
- chloroform
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000001514 detection method Methods 0.000 title claims description 18
- 206010011224 Cough Diseases 0.000 title description 4
- 229940126701 oral medication Drugs 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 110
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 241000255791 Bombyx Species 0.000 claims abstract description 17
- 210000000582 semen Anatomy 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 263
- 238000012360 testing method Methods 0.000 claims description 179
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 123
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 123
- 239000002904 solvent Substances 0.000 claims description 97
- 239000011259 mixed solution Substances 0.000 claims description 72
- 239000013642 negative control Substances 0.000 claims description 57
- 239000000463 material Substances 0.000 claims description 56
- 238000002360 preparation method Methods 0.000 claims description 52
- 239000000706 filtrate Substances 0.000 claims description 51
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 48
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 43
- 229960004756 ethanol Drugs 0.000 claims description 43
- 239000007788 liquid Substances 0.000 claims description 38
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 31
- 239000012467 final product Substances 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Substances OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 26
- 238000011161 development Methods 0.000 claims description 25
- 238000000605 extraction Methods 0.000 claims description 25
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 21
- 239000003208 petroleum Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 15
- 239000000741 silica gel Substances 0.000 claims description 14
- 229910002027 silica gel Inorganic materials 0.000 claims description 14
- 238000004809 thin layer chromatography Methods 0.000 claims description 14
- 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 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 235000019253 formic acid Nutrition 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- QSKWJTXWJJOJFP-UHFFFAOYSA-N chloroform;ethoxyethane Chemical compound ClC(Cl)Cl.CCOCC QSKWJTXWJJOJFP-UHFFFAOYSA-N 0.000 claims description 9
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 9
- NJUISRMVIKYYCN-UHFFFAOYSA-N acetic acid;chloroform;methanol;hydrate Chemical compound O.OC.CC(O)=O.ClC(Cl)Cl NJUISRMVIKYYCN-UHFFFAOYSA-N 0.000 claims description 8
- 238000012850 discrimination method Methods 0.000 claims description 7
- SIHHLZPXQLFPMC-UHFFFAOYSA-N chloroform;methanol;hydrate Chemical compound O.OC.ClC(Cl)Cl SIHHLZPXQLFPMC-UHFFFAOYSA-N 0.000 claims description 6
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 4
- JYHBPKNOVQWAPT-UHFFFAOYSA-N chloroform;formic acid Chemical compound OC=O.ClC(Cl)Cl JYHBPKNOVQWAPT-UHFFFAOYSA-N 0.000 claims description 4
- GLMWWMZIEZJGMT-UHFFFAOYSA-N chloroform;formic acid;propan-2-one Chemical compound OC=O.CC(C)=O.ClC(Cl)Cl GLMWWMZIEZJGMT-UHFFFAOYSA-N 0.000 claims description 4
- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- -1 potassium ferricyanide Chemical compound 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- IWYDHOAUDWTVEP-ZETCQYMHSA-N (S)-mandelic acid Chemical compound OC(=O)[C@@H](O)C1=CC=CC=C1 IWYDHOAUDWTVEP-ZETCQYMHSA-N 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 239000012567 medical material Substances 0.000 claims description 3
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- OAIVIYSBZFEOIU-UHFFFAOYSA-N chloroform;propan-2-one Chemical compound CC(C)=O.ClC(Cl)Cl OAIVIYSBZFEOIU-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 2
- 229930182490 saponin Natural products 0.000 claims description 2
- 150000007949 saponins Chemical class 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 238000003018 immunoassay Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims 1
- 235000012141 vanillin Nutrition 0.000 claims 1
- BALXUFOVQVENIU-GNAZCLTHSA-N Ephedrine hydrochloride Chemical compound Cl.CN[C@@H](C)[C@H](O)C1=CC=CC=C1 BALXUFOVQVENIU-GNAZCLTHSA-N 0.000 abstract description 26
- 229960002534 ephedrine hydrochloride Drugs 0.000 abstract description 26
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 abstract description 25
- 238000003556 assay Methods 0.000 abstract description 19
- 238000003908 quality control method Methods 0.000 abstract description 12
- 239000003814 drug Substances 0.000 abstract description 9
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 abstract description 8
- 238000007689 inspection Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 abstract description 4
- 229960002179 ephedrine Drugs 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 73
- 239000013558 reference substance Substances 0.000 description 50
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- 239000008187 granular material Substances 0.000 description 12
- 239000012071 phase Substances 0.000 description 12
- 239000012528 membrane Substances 0.000 description 10
- 238000011084 recovery Methods 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000033228 biological regulation Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000000945 filler Substances 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 239000004141 Sodium laurylsulphate Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012496 blank sample Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 230000003252 repetitive effect Effects 0.000 description 4
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 3
- 244000303040 Glycyrrhiza glabra Species 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 235000011477 liquorice Nutrition 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000002137 ultrasound extraction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 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 description 2
- 206010062717 Increased upper airway secretion Diseases 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 241001254606 Peucedanum praeruptorum Species 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N anhydrous methyl chloride Natural products ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 208000026435 phlegm Diseases 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 208000011580 syndromic disease Diseases 0.000 description 2
- 241000132092 Aster Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010067193 Naevus flammeus Diseases 0.000 description 1
- 238000012952 Resampling Methods 0.000 description 1
- 238000001467 acupuncture Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to the method for quality control of a kind of compositions being made up of the Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata, belong to technical field of medicine quality control.Method of quality control of the present invention includes differentiating, part or all of in assay and character inspection project.Wherein differentiating to include the indentification by TLC of the Radix Stemonae, Radix Peucedani, ephedrine, Radix Glycyrrhizae, content includes the assay of ephedrine hydrochloride, ammonium glycyrrhizinate and protostermonine.Method of quality control precision of the present invention is high, favorable reproducibility, and the response rate is high, and measurement result is accurate, can effectively control product quality, thus ensure curative effect.
Description
Technical field: the present invention relates to a kind of have relieving cough and resolving phlegm, lung qi dispersing promoting the circulation of QI, relieving the exterior syndrome dissipate the Chinese medicine composition of evil function
Method of quality control, belong to technical field of medicine quality control.The active component of described Chinese medicine composition by the Radix Stemonae, Radix Asteris,
Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata composition.
Background technology: the Chinese patent application of Application No. 201210005887.4, describes by the Radix Stemonae 2～3.5 parts, purple
Aster 1.5～3 parts, Radix Peucedani 1.5～3 parts, Radix Platycodonis 1.5～3 parts, Bombyx Batryticatus 1.0～2.5 parts, Periostracum Cicadae 0.8～2 parts, Herba Ephedrae 0.8～2
Part, Semen Armeniacae Amarum 1.0～2.5 parts, Fructus Mume 0.8～2 parts, Rhizoma Phragmitis 1.5～3 parts, Radix Glycyrrhizae 0.8～2 parts of Chinese medicine compositions made, should
Compositions has relieving cough and resolving phlegm, lung qi dispersing promoting the circulation of QI, the scattered evil function of relieving the exterior syndrome.
The quality controlling said composition the most fast and accurately is to be badly in need of solving the technical problem that.
The technical problem to be solved in the present invention: compositions described in the patent of a kind of Application No. 201210005887.4 is provided
(active component is made up of the Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata)
Method of quality control.
It is an object of the invention to: (the activity group of compositions described in the patent of a kind of Application No. 201210005887.4 is provided
Point be made up of the Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata) quality control
Method, the method can the quality of control composition fast and accurately.
The technical scheme is that
The technical scheme is that compositions described in the patent of Application No. 201210005887.4 (active component by
The Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata composition) quality control side
Method, is characterized in that including differentiating.
Discriminating of the present invention includes:
(1) discriminating of the Radix Stemonae (uprightly) in side:
Take this product 10g, finely ground, add 0.1mol/L hydrochloric acid solution 40ml merceration overnight, supersound process 10 minutes, filter, filter
Liquid to 12, adds chloroform extraction 3 times with saturated sodium hydroxide solution regulation pH value, and each 30ml merges chloroform liquid, steams
Dry, residue adds methanol 2ml makes dissolving, as need testing solution.Separately take Radix Stemonae 4g, be made in the same way of control medicinal material solution.According to
One annex VI B thin layer chromatography test of Chinese Pharmacopoeia, draws each 20 μ l of above two solution, puts respectively in same silica gel G
On lamellae, with ethyl acetate-methanol-strong ammonia solution (7: 0.25: 0.1, volume ratio) for developing solvent, launch, take out, dry,
Spray is with bismuth potassium iodide test solution.In test sample chromatograph, on position corresponding with control medicinal material chromatograph, aobvious identical salmon patch
Point.
This method negative control is noiseless.
(2) discriminating of Peucedanum praeruptorum DUNN in side:
Take this product 8g, finely ground, add diethyl ether 20ml merceration overnight, filter, filtrate is evaporated, and residue adds methanol 2ml makes dissolving, make
For need testing solution.Separately take Peucedanum praeruptorum DUNN control medicinal material 1g, be made in the same way of control medicinal material solution.According to one annex of Chinese Pharmacopoeia
VIB thin layer chromatography is tested, and draws each 5 μ l of above two solution, puts respectively on same silica gel g thin-layer plate, with petroleum ether (60
～90 DEG C)-ethyl acetate (4: 2, volume ratio) is developing solvent, launches, take out, dry, put and inspect under ultra-violet lamp (365nm).
In test sample chromatograph, on position corresponding with control medicinal material chromatograph, the fluorescence speckle of aobvious same color.
This method negative control is noiseless.
(3) discriminating of main component ephedrine contained by side's epheday intermedia:
Take the need testing solution under discriminating (1) item, as need testing solution.Separately take ephedrine hydrochloride reference substance, add methanol
Make every 1ml solution containing 1mg, as reference substance solution.According to one annex VIB thin layer chromatography test of Chinese Pharmacopoeia, draw
The each 5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, are the chloroform-first of 20: 3: 0.2 with volume ratio
Alcohol-strong ammonia solution is developing solvent, launches, and takes out, dries, and spray is with 0.2% ninhydrin solution, and 105 DEG C to be heated to spot development clear
Clear.In test sample chromatograph, on position corresponding with reference substance chromatograph, aobvious identical punctation.
This method negative control is noiseless.
(4) discriminating of Radix Glycyrrhizae Preparata in side:
Taking this product 5g, finely ground, add diethyl ether 40ml, is heated to reflux 1 hour, filters, and filtrate discards, and medicinal residues add methanol 30ml,
Being heated to reflux 1 hour, filter, filtrate is evaporated, and the residue 40ml that adds water makes dissolving, with n-butanol extraction 3 times, each 20ml, merges
N-butyl alcohol liquid, washes with water 3 times, is evaporated, and residue adds methanol 5ml makes dissolving, as need testing solution.Another extracting liquorice control medicinal material
1g, is made in the same way of control medicinal material solution.According to one annex VIB thin layer chromatography test of Chinese Pharmacopoeia, draw need testing solution 5 μ
L, control medicinal material solution 2 μ l, put respectively on silica gel g thin-layer plate prepared by same 1% sodium hydroxide solution, with volume ratio be
Ethyl acetate-formic acid-glacial acetic acid-the water of 15: 1: 1: 2 is developing solvent, launches, and takes out, dries, spray molten with 10% sulphuric acid ethanol
Liquid, is heated to spot development at 105 DEG C clear, puts and inspect under ultra-violet lamp (365nm).In test sample chromatograph, with compare medicine
Wood color is composed on corresponding position, the fluorescence speckle of aobvious same color.
This method negative control is noiseless.
Technical scheme, also includes Radix Asteris, Rhizoma Phragmitis, Radix Platycodonis, Fructus Mume, amygdalate discriminating.
The discrimination method of Radix Asteris of the present invention, it is characterised in that:
Method one:
Prepared by need testing solution: take this product powder 0.50g, adds methanol 25ml, supersound process 30 minutes, filters, and filtrate is waved
Dry, residue adds ethyl acetate 1ml, makes dissolving, to obtain final product.
Prepared by control medicinal material solution: take control medicinal material powder 1.00g, with above-mentioned need testing solution preparation method, makes comparison medicine
Material solution.
Prepared by negative control solution: take negative control powder 0.52g, and with above-mentioned need testing solution preparation method, it is negative right to make
According to solution.
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications.With petroleum ether-ether (9: 1) as developing solvent, use
10% ethanol solution of sulfuric acid colour developing, 105 DEG C to be heated to spot development clear.
Method two:
The preparation of need testing solution: take this product 4g, adds methanol 25ml, supersound process 30 minutes, filters, and filtrate volatilizes, residual
Slag adds ethyl acetate 1ml, makes dissolving, to obtain final product.
Prepared by negative control solution: take negative control powder 4g, with above-mentioned need testing solution preparation method, makes negative control molten
Liquid.
Prepared by control medicinal material solution: take control medicinal material powder 1.00g, with above-mentioned need testing solution preparation method, makes comparison medicine
Material solution.
Point sample amount: need testing solution 15ul, negative control 15ul, control medicinal material 5ul.
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications.Make developing solvent with petroleum ether-ether (100: 1), use
10% ethanol solution of sulfuric acid colour developing, 105 DEG C to be heated to spot development clear.
The discrimination method of Rhizoma Phragmitis of the present invention: it is characterized in that:
Method one
Method for making sample: weigh test sample 1.00g, control medicinal material 1.00g, negative control 1.00g respectively, add methanol 25ml,
Supersound process 30 minutes, filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml, makes dissolving, obtains need testing solution, control medicinal material
Solution, negative control solution.
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications.Developing solvent one in following developing solvent, with perfume (or spice)
Oxalaldehyde-10% ethanol solution of sulfuric acid develops the color, and 105 DEG C to be heated to spot development clear.
Developing solvent: 1. chloroform-formic acid (100: 1)；2. petroleum ether-chloroform (1: 1)；3. petroleum ether-three chloromethane
Alkane (4: 1)；5. petroleum ether-chloroform (2: 1).
Method two
Method for making sample: weigh Rhizoma Phragmitis medical material 0.50g, test sample 2.00g, negative control 2.00g respectively, add methanol 25ml,
Supersound process 30 minutes, filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml, makes dissolving, obtains control medicinal material solution, test sample
Solution, negative control solution.
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications.Developing solvent be petroleum ether-chloroform-formic acid (4: 1:
0.05), developing the color with vanillin-10% ethanol solution of sulfuric acid, 105 DEG C to be heated to spot development clear.
The discrimination method of Radix Platycodonis of the present invention: it is characterized in that:
Method one
Need testing solution is prepared by thin-layer identification method under 2010 editions pharmacopeia Radix Platycodonis items
Take sample particle 0.56g, add 7% sulphuric acid alcohol-water (1: 3) mixed solution 20ml, be heated to reflux 3h, let cool, use
Chloroform shaking is extracted 2 times, and each 20ml merges chloroform liquid, and add water washing 2 times, and each 30ml discards washing liquid, and three
Chloromethanes liquid anhydrous sodium sulfate dehydration, filters, and filtrate is evaporated, and residue adds methanol 1ml makes dissolving, obtains need testing solution.Again
Take control medicinal material, negative control 1.06g, 0.55g respectively, with the preparation method of need testing solution, prepare control medicinal material respectively molten
Liquid, negative control solution.And three kinds of solution are put respectively on same silica gel g thin-layer plate, select in following developing solvent
Plant and launch, with 10% ethanol solution of sulfuric acid colour developing, be heated to spot development at 105 DEG C clear.
1. developing solvent: chloroform-ether mixed solution (2: 1).
2. developing solvent: chloroform-ether mixed solution (1: 1).
3. developing solvent: chloroform-petroleum ether mixed solution (1: 5).
4. developing solvent: chloroform-petroleum ether mixed solution (1: 1).
Method two
Extracting directly saponin component prepares need testing solution
Take sample particle 0.50g, add 15ml water, ultrasonic 10min, with n-butanol extraction 2 times, each 15ml, take n-butyl alcohol
Layer, heating is concentrated into 5ml, obtains need testing solution.Take negative control 0.50g, with need testing solution preparation method, prepare feminine gender
Contrast solution.Take Radix Platycodonis control medicinal material 1.0g again, be ground into powder, add 30ml water, decoct 30min, filter, obtain filtrate, cooling, use
N-butanol extraction 2 times, each 20ml, take n-butanol layer, heating is concentrated into 5ml, obtains reference substance solution.And three kinds of solution are divided
Other point, on same silica gel g thin-layer plate, is selected a kind of expansion in following developing solvent, is developed the color with 10% ethanol solution of sulfuric acid,
It is heated to spot development clear at 105 DEG C.
1. developing solvent: n-butyl alcohol-ethyl acetate-water mixed solution (4: 1: 5), upper strata.
2. developing solvent: n-butyl alcohol-ethyl acetate-water (1: 4: 5), upper strata.
3. developing solvent: chloroform-methanol-water mixed solution (13: 7: 2), lower floor.
4. developing solvent: chloroform-methanol-water mixed solution (15: 5: 2), lower floor.
5. developing solvent: chloroform-methanol-water mixed solution (9: 1: 1), lower floor.
The discrimination method of Fructus Mume of the present invention: it is characterized in that:
Method one
Taking sample particle 1.00g, add methanol 25ml, supersound process 30min, filter, filtrate is evaporated, and residue adds ethyl acetate
1ml, makes dissolving, as need testing solution.Take negative control 1.00g again, take Fructus Mume medical material (Fructus Mume) 1.00g, pound and fragmentate,
With the preparation method of need testing solution, prepare control medicinal material solution, negative control solution respectively.And three kinds of solution are put respectively in
On same silica gel g thin-layer plate, select a kind of expansion in following developing solvent, with vanillin-concentrated sulfuric acid solution colour developing, 105
It is clear DEG C to be heated to spot development.
1. developing solvent: chloroform-acetone-formic acid mixed solution (5: 2: 0.8).
2. developing solvent: cyclohexane-ethyl acetate-glacial acetic acid mixed solution (4: 1: 0.1).
3. developing solvent: chloroform-acetone-formic acid mixed solution (9: 0.5: 0.5).
4. developing solvent: chloroform.
5. developing solvent: chloroform-acetone mixed solution (50: 1).
6. developing solvent: chloroform-formic acid mixed solution (100: 1).
Method two
Method by extracting organic acid: take test sample 1.00g, negative control 1.04g, control medicinal material 1.06g respectively, be ground into
Powder, adds dilute hydrochloric acid 20ml, supersound process 30min, takes supernatant, and add diethyl ether extraction 2 times, and each 15ml merges ether solution, waves
Dry solvent, residue adds dehydrated alcohol 1ml, makes dissolving, prepares need testing solution, negative control solution, control medicinal material the most respectively molten
Liquid.And three kinds of solution are put on same silica gel g thin-layer plate respectively, select a kind of expansion in following developing solvent, and develop the color,
Observe.
1. developing solvent: hexamethylene-dichloromethane-glacial acetic acid mixed solution (8: 8: 1)
Colour developing: 1% ferric chloride ethanol solution and 1% potassium ferricyanide solution mixed in equal amounts (now joining), it is seen that light is inspected.
2. developing solvent: hexamethylene-chloroform (1: 10), colour developing: vanillin-concentrated sulfuric acid solution, it is heated to speckle at 105 DEG C
Point colour developing is clear.
3. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 5: 5).
4. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 5: 5) ,+2 formic acid.
5. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 2: 2) ,+2 formic acid.
6. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 2: 4) ,+4 formic acid.
7. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 1: 1) ,+4 formic acid.
8. developing solvent: hexamethylene-dichloromethane-ethyl acetate-formic acid mixed solution (4: 1: 1: 0.1).
When selecting 3.-8. described developing solvent to launch, with 5% vanillin-concentrated sulfuric acid solution colour developing, it is heated at 105 DEG C
Spot development is clear.
Method three
By official method: take test sample 4.00g, negative control 4.00g, control medicinal material 1.00g respectively, be ground into powder, add
Methanol 30ml, supersound process 30min, filter, take filtrate, be evaporated, residue adds 20ml water, dissolves, then the extraction 2 times that adds diethyl ether, often
Secondary 20ml, merges ether solution, is evaporated, and residue petroleum ether soaks 2 times, and each 15ml, incline petroleum ether, and residue 2ml is anhydrous
Ethanol dissolves, and prepares need testing solution, negative control solution, control medicinal material solution the most respectively.And three kinds of solution are put respectively in
On same silica gel g thin-layer plate, select a kind of expansion in following developing solvent, with 10% ethanol solution of sulfuric acid colour developing, at 105 DEG C
It is heated to spot development clear.
1. developing solvent: hexamethylene-dichloromethane-ethyl acetate-formic acid mixed solution (20: 5: 8: 0.1), colour developing:
2. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 1: 1) ,+1 formic acid.
3. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution (1: 3: 3) ,+2 formic acid.
The amygdalate discrimination method of the present invention: it is characterized in that:
By official method sample preparation: separately sampled product 5.51g, control medicinal material 1.03g, negative control 5.35g, put surname extraction
In device, adding 50ml dichloromethane, be heated to reflux 2h, discard dichloromethane solution, medicinal residues volatilize, then add methanol 50ml, heat back
Stream 40min, lets cool, and filters, and obtains filtrate, reclaims methanol, is concentrated into 15ml, obtains three kinds of solution.And by three kinds of solution point respectively
On same silica gel g thin-layer plate, if selecting a kind of expansion in the developing solvent of following (1)-(5), with the 15% of 0.8% phosphomolybdic acid
Ethanol solution of sulfuric acid leaching plate colour developing, 105 DEG C to be heated to spot development clear；If selecting developing solvent (6) to launch, with 0.8% phosphorus molybdenum
15% ethanol solution of sulfuric acid leaching plate colour developing of acid, 105 DEG C to be heated to spot development clear；If selecting developing solvent (7) to launch, with perfume (or spice)
Oxalaldehyde concentrated sulphuric acid develops the color, and 105 DEG C to be heated to spot development clear.
(1) chloroform-acetate-methanol-water mixed solution (15: 40: 22: 10), lower floor, 5～10 DEG C of placements
12h。
(2) chloroform-acetate-methanol-water mixed solution (2: 4: 1: 1), lower floor.
(3) chloroform-acetate-methanol-water mixed solution (4: 1: 1: 1), lower floor.
(4) chloroform-acetate-methanol-water mixed solution (8: 1: 0.5: 1), lower floor.
(5) chloroform.
(6) chloroform-methanol mixed solution (1: 1).
(7) chloroform-methanol mixed solution (1: 5).
Bombyx Batryticatus of the present invention and the discrimination method of Periostracum Cicadae: it is characterized in that:
Bombyx Batryticatus, the preparation of the double-negative contrast solution of Periostracum Cicadae: weigh Radix Stemonae 16.59g, Radix Peucedani 12.52g, Herba Ephedrae 6.24g, hardship
Semen Armeniacae Amarum 9.38g, 70% alcohol reflux 3 times (358ml × 2h, 234ml × 1h, 234ml × 0.5h), united extraction liquid, filter, filter
Liquid decompression recycling ethanol is concentrated into paste, and thick paste is standby.
Weigh Radix Asteris 12.50g, Radix Platycodonis 12.48g, Radix Glycyrrhizae 6.25g, Rhizoma Phragmitis 12..52g, Fructus Mume 6.21g, soak by water 2 times
(600ml × 1h, 500ml × 1h), merges decocting liquid, filters, and it is 1.03～1.05 (50 DEG C) that filtrate is concentrated into relative density, then
Adding ethanol makes alcohol content reach 60% (after concentration volume 50ml, ethanol consumption is 75ml), stands 24h, takes supernatant and filter, filter
Liquid decompression recycling ethanol is concentrated into paste, and thick paste is standby.
By two kinds of thick paste mixings, obtain negative thick paste.
Weigh negative thick paste 1.28g, put in tool plug conical flask, accurate addition 70% ethanol 5ml, close plug, supersound process
30min, filters, takes subsequent filtrate and get final product.
The preparation of need testing solution: weigh sample particle 3.19g, puts in tool plug conical flask, accurate addition 70% ethanol
5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product.
Prepared by Bombyx Batryticatus control medicinal material solution: take Bombyx Batryticatus control medicinal material 0.64g, puts in tool plug conical flask, accurate addition 70%
Ethanol 5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product.
Prepared by Periostracum Cicadae control medicinal material solution: take Periostracum Cicadae control medicinal material 0.40g, puts in tool plug conical flask, accurate addition 70%
Ethanol 5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product.
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications.Wherein, developing solvent one in following developing solvent,
Develop the color with ninhydrin solution (0.11g → 54ml ethanol).
1. developing solvent: n-butyl alcohol-glacial acetic acid-water mixed solution (8: 3: 3).
2. developing solvent: n-butyl alcohol-glacial acetic acid-water mixed solution (8: 3: 3).
3. developing solvent: n-butyl alcohol-glacial acetic acid-water mixed solution (3: 1: 1.2).
Technical scheme of the present invention, also includes the mensuration of Determination of ephedrine hydrochloride.
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica；With water-acetonitrile-phosphoric acid-ten
Sodium dialkyl sulfate (520ml: 480ml: 1ml: 5 grams) for flowing phase (flowing prepare mutually time, first with water by lauryl sulphate acid
Sodium dissolves, then is proportionally added into acetonitrile, phosphoric acid successively, mixing, filters with 0.45 μm microporous filter membrane, to obtain final product)；Detection wavelength is
210nm；Column temperature 25 DEG C, flow velocity 1.0ml/min.
Currently preferred technical scheme is that number of theoretical plate should be not less than 5000 by the calculating of ephedrine hydrochloride peak.
The preparation of reference substance solution: take ephedrine hydrochloride reference substance appropriate, accurately weighed, add methanol and make every 1ml and contain
The solution of 0.043mg, to obtain final product.
The preparation of need testing solution: take this product under content uniformity item, finely ground, take 1g, accurately weighed, put tool plug conical flask
In, add 1% hydrochloric acid-methanol solution 20ml, close plug, weighed weight, supersound process (power 250W, frequency 20kHz) 30 minutes,
Let cool, more weighed weight, supply the weight of less loss with 1% hydrochloric acid-methanol solution, shake up, filter with microporous filter membrane (0.45 μm),
Take subsequent filtrate, to obtain final product.
Measure: precision measures reference substance solution, each 10 μ l of need testing solution respectively, is injected separately into chromatograph of liquid, measure,
Obtain.This assay measures according to the relevant regulations of Chinese Pharmacopoeia annex VID high performance liquid chromatography.
Technical scheme of the present invention, also includes the mensuration of ammonium glycyrrhizinate content.
Chromatographic condition and system suitability: the chromatographic column: (Hypersil with octadecylsilane chemically bonded silica as filler
ODS, 4.6mm × 250mm, 5 μm)；Flowing phase: second eyeball-0.05% phosphate aqueous solution (35: 65)；Detection wavelength: 250nm；Stream
Speed: 1.0ml/min；Column temperature: room temperature.
The preparation of need testing solution: take sample particle (20111101 crowdes) about 1.6g, accurately weighed, put tool plug conical flask
In, accurate addition 70% ethanol 100ml, close plug, weigh, supersound process (250w, 40kHZ) 30 minutes, let cool, more weighed heavy
Amount, supplies less loss weight with 70% ethanol, shakes up, and filters, takes subsequent filtrate, to obtain final product.
The preparation of reference substance solution: extracting liquorice acid ammonium reference substance is appropriate, accurately weighed, adds 70% ethanol and makes every 1ml and contain
The solution of ammonium glycyrrhizinate 0.2mg, then dilute 10 times and get final product.
Measure: draw ammonium glycyrrhizinate reference substance solution, need testing solution, each 10 μ l of negative control solution respectively, enter respectively
Sample, measures, to obtain final product.This assay measures according to the relevant regulations of Chinese Pharmacopoeia annex VI D high performance liquid chromatography.
Technical scheme of the present invention, also includes the mensuration of protostermonine content.
Chromatographic condition: chromatographic column: with octadecylsilane chemically bonded silica as filler (Hypersil ODS, 4.6mm ×
250mm, 5 μm)；Flowing phase: second eyeball-0.1% triethylamine aqueous solution (36: 64)；Detection wavelength: 305nm；Flow velocity: 1.0ml/
min；Column temperature: room temperature.
The preparation of need testing solution: take sample about 1.5g, accurately weighed, put in 100ml tool plug conical flask, accurate addition
50ml methanol, close plug, weigh, ultrasonic 30min, after letting cool, it is re-weighed, supplies the weight of less loss, shake up, filter, take subsequent filtrate
Obtain need testing solution.
The preparation of reference substance solution: precision weighs protostermonine reference substance 0.0054g, puts in volumetric flask, uses methanol constant volume
To 10ml, make dissolving, shake up, more therefrom accurate absorption 1ml, dilute 10 times, obtain the protostermonine reference substance of 0.054mg/ml
Solution.
Measure: draw need testing solution, each 10ul of reference substance solution respectively, respectively sample introduction, measure.During this assay shines
The relevant regulations of state's pharmacopeia annex VID high performance liquid chromatography measures.
Technical scheme also includes: the inspection of character.
Character: this product is tan granule；Feeble QI is fragrant, sweet and sour, micro-hardship.
The invention has the beneficial effects as follows: provide a kind of active component by the Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae,
The method of quality control of the Chinese medicine composition that Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata form, the method includes differentiating, containing
Measure in fixed and character inspection project is part or all of.Wherein differentiate to include the thin layer color of the Radix Stemonae, Radix Peucedani, ephedrine, Radix Glycyrrhizae
Spectrum differentiates, content includes the assay of ephedrine hydrochloride.Method of quality control precision of the present invention is high, favorable reproducibility, reclaims
Rate is high, and measurement result is accurate, it is possible to the quality of control composition fast and accurately, thus ensures curative effect.
Accompanying drawing explanation
Fig. 1, Determination of ephedrine hydrochloride standard curve.
Fig. 2, ammonium glycyrrhizinate assay specificity experiment chromatogram, wherein: Fig. 2 A, ammonium glycyrrhizinate reference substance specificity is real
Test chromatogram；Fig. 2 B, test sample specificity experiment chromatogram；Fig. 2 C, negative control specificity experiment chromatogram.
Fig. 3, the standard curve of ammonium glycyrrhizinate.
Fig. 4, protostermonine assay specificity test HPLC chromatogram, wherein: Fig. 4 A protostermonine reference substance is exclusive
Property experiment chromatogram；4B test sample specificity experiment chromatogram；Fig. 4 C negative control specificity experiment chromatogram.
Fig. 5, protostermonine standard curve.
Embodiment
Embodiment 1 differentiates the regulation under item by technical scheme part, to special by Application No. 201210005887.4 invention
201101,201102,201,103 3 batches of compositionss of sample of profit application preparation differentiate, result is recorded in table 1.
Table 1 three batch sample differentiates (1), (2), (3), (4) assay
Embodiment 2 Determination of ephedrine hydrochloride content assaying method is studied
Instrument and reagent
Instrument: the U.S. wears peace SUMMIT HPLC high performance liquid chromatograph, P680 type quaternary pump, ASI-100 auto injection
Device, UVD170U UV-detector, TCC-10 column oven, Chromeleon chromatographic work station.
The U.S. wears pacifies SUMMIT HPLC high performance liquid chromatograph, P680 type unitary pump, UVD170U UV-detector,
Chromeleon chromatographic work station.
Chromatographic column: C18(4.6mm × 250mm, 5 μm)
Reagent: acetonitrile (α Cygni friend fine chemistry company limited) chromatographically pure, methanol (the limited public affairs of α Cygni friend's fine chemistry
Department) chromatographically pure, sodium lauryl sulphate (Tianjin Guang Cheng chemical reagent company limited), (traditional Chinese medicines group chemical reagent has phosphoric acid
Limit company), hydrochloric acid (Tianjin Standard Science company limited) is analytical pure.
Reference substance: ephedrine hydrochloride is provided by Nat'l Pharmaceutical & Biological Products Control Institute, for assay.
Sample source: three batch samples by Disha Pharmaceutical Industry Group Corp., Ltd. by Application No. 201210005887.4 invention
Sample prepared by patent application, lot number: 201101,201102,201103；Specification: 6g/ bag.
Solvent (1% hydrochloric acid-methanol solution) is prepared: take 2.8ml hydrochloric acid in 100ml measuring bottle, adds methanol to scale, shakes
Even, to obtain final product.
Chromatography condition is tested
(1) flowing phase, column temperature, change in flow test:
The flowing basic mobile phase composition used in former method and ratio mutually, fit the ratio of water in flowing mutually with acetonitrile
When adjusting and being tested, column temperature uses conventional 25 DEG C and 40 DEG C, 50 DEG C to test respectively；Flow velocity employing 0.8ml/min,
1.0ml/min, 1.2ml/min test respectively；Concrete grammar is as follows:
Take composition grain appropriate, finely ground, take 1g, accurately weighed, put in tool plug conical flask, add 1% hydrochloric acid-methanol molten
Liquid 20ml, close plug, weighed weight, supersound process (power 250W, frequency 20kHz) 30 minutes, let cool, more weighed weight, use
1% hydrochloric acid-methanol solution supplies the weight of less loss, shakes up, and filters with microporous filter membrane (0.45 μm), measures subsequent filtrate 10 μ l respectively
Inject chromatograph of liquid, when investigating mobile phase ratio change, column temperature change, change in flow, the change of instrument chromatographic behavior, each
Under the conditions of each test twice, test result is shown in Table 2 respectively, table 3, table 4.
Table 2 mobile phase ratio change result of the test
Result of the test shows: mobile phase ratio for all energy of main peak time (620: 380: 1: 5) and (520: 480: 1: 5) and other
Impurity peaks separates, and separating degree is all higher than 1.5, but main peak t when ratio is (620: 380: 1: 5)ROversize, it is unfavorable for when producing greatly
Inspection, main peak t when ratio is (520: 480: 1: 5)RModerate, convenient inspection；Main peak t when ratio is (420: 580: 1: 5)RIt is the shortest,
Main peak separating degree is defective, it is impossible to effectively detects the content of ephedrine hydrochloride, therefore selects water-acetonitrile-phosphoric acid-lauryl sulphate acid
Sodium (520ml: 480ml: 1ml: 5g) is flowing phase.
Table 3 column temperature change result of the test
Result of the test shows: column temperature is 25 DEG C, 40 DEG C, 50 DEG C time main peak all can separate with other impurity peaks, separating degree is equal
More than 1.5, the content results of same sample detection is basically identical, illustrates that, by above Same Way, testing result is affected by column temperature
Not quite, thus select 25 DEG C of conventional column temperatures.
Table 4 change in flow result of the test
Result of the test shows: when flow velocity is 0.8ml/min, 1.0ml/min, 1.2ml/min, main peak all can be with other impurity
Peak separates, and separating degree is all higher than 1.5, and the content results of same sample detection is basically identical, illustrates by above Same Way, flow velocity
Little on testing result impact, therefore select conventional 1.0ml/min flow velocity.
Above result of the test shows, flowing be mutually water-acetonitrile-phosphoric acid-sodium lauryl sulphate (520ml: 480ml: 1ml:
5g), column temperature 25 DEG C, the chromatographic condition of flow velocity 1.0ml/min, the content of product can be detected quickly and efficiently, result is stable, can
Lean on.
The selection of detection wavelength:
Take ephedrine hydrochloride reference substance about 10mg, add methanol and make in every 1ml the solution containing about 40 μ g, according to ultraviolet-visible
Spectrophotography (two annex IV A of Chinese Pharmacopoeia), carries out UV scanning in 200nm～400nm wave-length coverage, and salt is tingle
Yellow alkali has absorption maximum at 210nm wavelength, it is thus determined that 210nm checks wavelength as this product assay.
The investigation of test sample (201210005887.4 patent of invention compositions) solution manufacturing method
Accurately weighed composition grain three parts, each 1g, it is recorded as I, II, III respectively, adds 1% hydrochloric acid-methanol solution respectively
20ml, shakes up, close plug, accurately weighed.
I supersound process 30 minutes, places to room temperature；II heating and refluxing extraction 1 hour, places to room temperature；III merceration 24 is little
Time, place to room temperature.And supplement less loss weight with 1% hydrochloric acid-methanol, shake up, filter with microporous filter membrane (0.45 μm), take continuous filter
Liquid, obtains need testing solution I, II, III, and precision measures 10 μ l injection chromatograph of liquid respectively, measures, the results are shown in Table 5.
Table 5 Different Extraction Method result of the test
Result of the test shows: the Determination of ephedrine hydrochloride measured by the preparation method of three kinds of need testing solutions is basically identical,
And supersound extraction has quick, easy advantage, therefore select supersound extraction.
(3) selection of extraction time:
Accurately weighed composition grain three parts, each 1g, add 1% hydrochloric acid-methanol solution 20ml respectively, close plug, precise weighing,
Supersound process 15 minutes, 30 minutes, 45 minutes respectively, places to room temperature, shakes up, and filters with microporous filter membrane (0.45 μm), accurate
Measure subsequent filtrate 10 μ l and inject chromatograph of liquid, measure, the results are shown in Table 6.
The different extraction time result of the test of table 6
Result of the test shows: supersound process has been extracted completely for 30 minutes, therefore selects supersound process 30 minutes.
Blank is tested
Prepared by need testing solution: accurately weighed composition grain 1g, adds 1% hydrochloric acid-methanol solution 20ml, and close plug is ultrasonic
Process 30 minutes, let cool, filter with microporous filter membrane (0.45 μm), take subsequent filtrate, to obtain final product.
Prepared by blank sample solution: prepare the negative control sample without Herba Ephedrae, precise weighing by the formulation and technology of this preparation
Negative control sample 1g, adds 1% hydrochloric acid-methanol solution 20ml, close plug, supersound process 30 minutes, lets cool, use microporous filter membrane
(0.45 μm) filters, and takes subsequent filtrate, to obtain final product.
Prepared by reference substance solution: it is appropriate that precision weighs ephedrine hydrochloride reference substance, add methanol make every 1ml containing about
The solution of 0.043mg, to obtain final product.
Precision measures blank sample solution, reference substance solution, each 10 μ l of need testing solution respectively, injects chromatograph of liquid,
Measure, the results are shown in Table 7.
Table 7 blank result of the test
Result of the test shows: blank sample solution without chromatographic peak, does not disturb test sample at ephedrine hydrochloride retention time
Detection.
Blank sample solution without chromatographic peak, does not disturb the detection of test sample, the method at ephedrine hydrochloride retention time
Specificity is good.
Linear relationship is tested
Precision weighs ephedrine hydrochloride reference substance 11.47mg, puts 100ml measuring bottle, dissolves with methanol and be diluted to scale, shakes
Even, standby.Respectively precision measure above-mentioned solution 1,5,10,15,20ml, put in 25ml volumetric flask, with methanol dilution to scale, shake
Even.Draw 10 μ l respectively, inject chromatograph of liquid, record chromatogram.With ephedrine hydrochloride peak area (y) as vertical coordinate, sample introduction
Concentration (x) is abscissa, carries out linear regression analysis, the results are shown in Table 8.
Table 8 linear relationship result of the test
Result of the test shows: ephedrine hydrochloride is in the range of 4.588 μ g/ml～91.76 μ g/ml, and linear relationship is good.
Refer to accompanying drawing 1.
Detection limit test
Take ephedrine hydrochloride reference substance 11.47mg, add methanol and prepare the reference substance solution of a series of concentration, respectively precision amount
Take 10 μ l and inject chromatograph of liquid, record chromatogram, calculate detection limit with main peak signal to noise ratio 10: 1.
Result of the test: minimum detectable activity is 0.902 μ g/ml.
Result of the test shows: the method minimum detectable activity is low, and power of test is sensitive.
Solution stability testing: take same need testing solution, be measured at 0h, 2h, 4h, 8h and 12h, 24h respectively, note
Record chromatogram, calculates and get final product, the results are shown in Table 9.
Table 9 stability test result
| Time (h) | 0 | 2 | 4 | 8 | 12 | 24 | Meansigma methods | RSD (%) |
| Peak area | 11.720 | 11.673 | 11.722 | 11.702 | 11.679 | 11.605 | 11.684 | 0.37 |
| Content, mg/g | 0.604 | 0.601 | 0.604 | 0.603 | 0.602 | 0.598 | 0.602 | 0.37 |
Result of the test shows: stability test result shows, same need testing solution sample is good at 24 hours internal stabilities
Good.
Precision test
Take same need testing solution, continuous acupuncture 6 times, record chromatogram, calculate and get final product, the results are shown in Table 10.
Table 10 Precision test result
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | Meansigma methods | RSD (%) |
| Peak area | 9.491 | 9.578 | 9.578 | 9.488 | 9.518 | 9.470 | 9.52 | 0.5 |
| Content (mg/g) | 0.589 | 0.594 | 0.594 | 0.589 | 0.590 | 0.588 | 0.591 | 0.5 |
Result of the test shows: Precision test result shows, the precision of instrument is preferable.
Repeatability is tested
Take same batch sample, prepare 6 parts of need testing solutions according to need testing solution preparation method simultaneously and be measured, record
Chromatogram, calculates and get final product, the results are shown in Table 11.
Table 11 reproducible test results
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | Meansigma methods | RSD (%) |
| Content (mg/g) | 0.604 | 0.608 | 0.606 | 0.600 | 0.601 | 0.604 | 0.604 | 0.5 |
Result of the test shows: reproducible test results shows, the repeatability of the method for inspection is good.
Average recovery is tested
Accurate six parts of same a collection of composition grain (lot number 201103, the 0.47mg/g) sample weighing known content respectively,
About 2g, puts in tool plug triangular flask, and precision adds ephedrine hydrochloride reference substance about 1.00mg respectively, adds 50ml 1% hydrochloric acid-methanol
Solution, close plug, weighed weight, supersound extraction (power 250W, frequency 20kHz) 30min, let cool, and mend with 1% hydrochloric acid-methanol
Fill less loss weight, shake up, filter with microporous filter membrane (0.45 μm), take subsequent filtrate, as need testing solution.Separately take ephedrine hydrochloride
Reference substance is appropriate, accurately weighed, adds methanol and makes every 1ml solution containing 0.043mg, as reference substance solution.
Precision measures reference substance solution and each 10 μ l of need testing solution, injects chromatograph of liquid, records chromatogram, calculates i.e.
, the results are shown in Table 12.
Table 12 average recovery result of the test
Result of the test shows, this method average recovery is good, and the method is reliable.
Content determination method of ephedrine hydrochloride
To sum up result of the test determines final content assaying method:
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler；With water-acetonitrile-phosphorus
Acid-sodium lauryl sulphate (520: 480: 1: 5) for flowing phase (flowing prepare mutually time, first with water by sodium lauryl sulphate
Dissolve, then be proportionally added into acetonitrile, phosphoric acid successively, mixing, filter with 0.45 μm microporous filter membrane, to obtain final product)；Detection wavelength is
210nm；Column temperature 25 DEG C.Number of theoretical plate is calculated by ephedrine hydrochloride peak should be not less than 5000.
It is appropriate that the preparation of reference substance solution takes ephedrine hydrochloride reference substance, accurately weighed, adds methanol and makes every 1ml and contain
The solution of 0.043mg, to obtain final product.
The preparation of need testing solution takes this product under content uniformity item, finely ground, takes 1g, accurately weighed, puts tool plug conical flask
In, add 1% hydrochloric acid-methanol solution 20ml, close plug, weighed weight, supersound process (power 250W, frequency 20kHz) 30 minutes,
Let cool, more weighed weight, supply the weight of less loss with 1% hydrochloric acid-methanol solution, shake up, filter with microporous filter membrane (0.45 μm),
Take subsequent filtrate, to obtain final product.
Algoscopy precision respectively measures reference substance solution, each 10 μ l of need testing solution, injects chromatograph of liquid, measures, i.e.
?.
Sample determination result
Take this product three batch sample and measure hydrochloric acid by the method declaring in clinical quality standard and the new method now determined respectively
The content of ephedrine, the results are shown in Table 13.
Table 13 sample determination result
Result of the test shows: measuring the Determination of ephedrine hydrochloride in sample as stated above, result shows the method science
Rationally, can effective control for product quality.
By method determined above, test agent in detection, the results are shown in Table 14.
Table 14 pilot scale sample determination result
Result of the test shows: the Determination of ephedrine hydrochloride equal conformance with standard regulation in each batch sample.
Above result of study shows that method of quality control precision of the present invention is high, favorable reproducibility, and the response rate is high, measures
Result is accurate, can effectively control product quality.
Ammonium glycyrrhizinate content assaying method research in embodiment 3, side
Chromatographic condition is groped: chromatographic column: (Hypersil ODS, 4.6mm with octadecylsilane chemically bonded silica as filler
× 250mm, 5 μm)；Flowing phase: second eyeball-0.05% phosphate aqueous solution (35: 65)；Detection wavelength: 250nm；Flow velocity: 1.0ml/
min；Column temperature: room temperature.
The preparation of need testing solution: take sample particle and (prepare by Application No. 201210005887.4 application for a patent for invention
Sample, 20111101 batches) about 1.6g, accurately weighed, put in tool plug conical flask, the accurate 70% ethanol 100ml that adds, close plug,
Weigh, supersound process (250w, 40kHZ) 30 minutes, let cool, more weighed weight, supply less loss weight with 70% ethanol, shake up,
Filter, take subsequent filtrate, to obtain final product.
The preparation of negative control solution: with reference to Application No. 201210005887.4 application for a patent for invention preparation without Radix Glycyrrhizae
Negative thick paste, take about 1.6g in proportion, accurately weighed, prepared by the preparation method further according to need testing solution, to obtain final product.
The preparation of reference substance solution: extracting liquorice acid ammonium reference substance is appropriate, accurately weighed, adds 70% ethanol and makes every 1ml and contain
The solution of ammonium glycyrrhizinate 0.2mg, then dilute 10 times and get final product.
Methodology certification is tested
1. specificity examination
Draw ammonium glycyrrhizinate reference substance solution, need testing solution, each 10 μ l of negative control solution, respectively sample introduction respectively.?
In reference substance solution and need testing solution chromatogram relevant position, there are the chromatographic peak of identical retention time and feminine gender noiseless, see
Accompanying drawing 2.
2. linear relationship examination
Draw ammonium glycyrrhizinate reference substance solution (0.02mg/ml) 2 μ l, 4 μ l, 8 μ l, 12 μ l, 16 μ l respectively, inject liquid phase color
Spectrometer, measures ammonium glycyrrhizinate peak area, the results are shown in Table 15.With reference substance sample size (μ g) as abscissa, chromatographic peak peak area is
Vertical coordinate draws standard curve, and result is shown in accompanying drawing 3.
Calculating regression equation is: Y=29.514X+0.5963, R2=1, show ammonium glycyrrhizinate sample size at 0.04 μ g～
0.32 μ g range internal linear relation is good.
Table 15 ammonium glycyrrhizinate linear relationship examination experimental result (n=2)
| Sampling volume (μ l) | Sample size (μ g) | 2 pin peak area meansigma methodss |
| 2 | 0.04 | 28.9352 |
| 4 | 0.08 | 57.9603 |
| 6 | 0.12 | 88.4974 |
| 8 | 0.16 | 116.9784 |
| 10 | 0.20 | 147.3747 |
| 12 | 0.24 | 176.5220 |
| 14 | 0.28 | 206.5903 |
| 16 | 0.32 | 234.8698 |
3. precision examination
Accurate absorption need testing solution 20 μ l, continuously repeats sample introduction 6 times, measures peak area, and calculating RSD is 1.02%, knot
Fruit is shown in Table 16.Show that the method precision is good.
Table 16 precision examination result
4. the stability examination of need testing solution
Take need testing solution, respectively at 0,2,4,6,8,10,12h sample introductions, each sample introduction 20 μ l, measure in need testing solution
The chromatographic peak peak area of ammonium glycyrrhizinate.The results are shown in Table 17.Showing that need testing solution is basicly stable in 12h, RSD is 1.49%.
Table 17 stability examination result
5. replica test
Take granule (20111101 crowdes) about 1g, accurately weighed, accurate addition 70% ethanol 75ml, weigh, ultrasonic
30min, lets cool, and is re-weighed, and mends weight, shakes up, and filters, and takes subsequent filtrate as need testing solution, and operation repetitive prepares 6 parts, respectively
Sample introduction 20 μ l, measures the chromatographic peak peak area of ammonium glycyrrhizinate in need testing solution, and the average content calculating ammonium glycyrrhizinate is
0.059%, RSD are 2.14%.The results are shown in Table 18.Show that this assay method repeatability is good.
Table 18 replica test result
6. average recovery test
Take granule (content 0,059%) the about 0.5g of above-mentioned known ammonium glycyrrhizinate content, accurately weighed, accurate addition
Ammonium glycyrrhizinate reference substance solution 1.6ml of 0.2mg/ml, more accurate addition 70% ethanol 73.4ml, weigh, and ultrasonic 30min is put
Cold, it is re-weighed, mends weight, shake up, filter, take subsequent filtrate as need testing solution, operation repetitive prepares 6 parts, respectively sample introduction 20 μ l,
Measuring the chromatographic peak peak area of ammonium glycyrrhizinate in need testing solution, calculate the response rate, recording average recovery rate is 101.85%,
RSD is 2.45%, the results are shown in Table 19.Result shows that this assay method accuracy is qualified.
Table 19 average recovery result of the test
Sample determination
According to the content assaying method of above-mentioned foundation, remaining 4 batches of test sample granule is carried out ammonium glycyrrhizinate and has contained measurement
Fixed, the results are shown in Table 20.
The assay result of ammonium glycyrrhizinate in table 20 test sample granule
The content assaying method research of embodiment 4 protostermonine
Chromatographic condition is groped
The preparation of need testing solution:
Reflux extraction: take sample about 1.5g, accurately weighed, put in 100ml tool plug conical flask, accurate addition 50ml first
Alcohol, close plug, weigh, be heated to reflux 1h, after letting cool, be re-weighed, supply the weight of less loss, shake up, filter, take subsequent filtrate and i.e. obtain confession
Test sample solution.
Ultrasonic extraction: resampling product about 1.5g, accurately weighed, put in 100ml tool plug conical flask, accurate addition 50ml first
Alcohol, close plug, weigh, ultrasonic 30min, after letting cool, it is re-weighed, supplies the weight of less loss, shake up, filter, take subsequent filtrate and i.e. obtain confession
Test sample solution.
The preparation of negative control solution:
The preparation of negative control solution: with reference to Application No. 201210005887.4 application for a patent for invention preparation without the Radix Stemonae
Negative thick paste, take about 1.5g in proportion, accurately weighed, test sample preparation method is pressed in other operation, prepares negative control respectively
Solution (reflux extraction) and negative control solution (ultrasonic extraction).
The preparation of reference substance solution: precision weighs protostermonine reference substance 0.0054g, puts in volumetric flask, uses methanol constant volume
To 10ml, make dissolving, shake up, more therefrom accurate absorption 1ml, dilute 10 times, obtain the protostermonine reference substance of 0.054mg/ml
Solution.
Through groping finally to select following chromatographic condition:
Chromatographic column: with octadecylsilane chemically bonded silica as filler (Hypersil ODS, 4.6mm × 250mm, 5 μm)；
Flowing phase: second eyeball-0.1% triethylamine aqueous solution (36: 64)；Detection wavelength: 305nm；Flow velocity: 1.0ml/min；Column temperature: room temperature.
Methodology certification is tested
1. specificity examination
Draw protostermonine reference substance solution, need testing solution, each 5 μ l of negative control solution, respectively sample introduction respectively.Right
According on product solution and need testing solution chromatogram relevant position, there are the chromatographic peak of identical retention time and feminine gender noiseless, result
Being shown in Table 21, chromatogram is shown in accompanying drawing 4.
Table 21 protostermonine assay specificity result of the test
2. need testing solution preparation method examination
Take granule about 0.4g prepared by Radix Stemonae, accurately weighed, put in 50ml tool plug conical flask, accurate addition 10ml first
Alcohol, close plug, weigh, be heated to reflux 1h, after letting cool, be re-weighed, supply the weight of less loss, shake up, filter, take subsequent filtrate and i.e. obtain confession
Test sample solution (reflux extraction).Take three parts of the sample of Radix Stemonae batch again, every part of about 0.4g, accurately weighed, put 50ml tool
In plug conical flask, accurate addition 10ml methanol, close plug, weigh, ultrasonic 20min, 40min, 60min, after letting cool, then claim respectively
Weight, supplies the weight of less loss, shakes up, and filters, takes subsequent filtrate and i.e. obtain three kinds of need testing solutions (ultrasonic extraction).
The preparation of reference substance solution: precision weighs protostermonine reference substance 0.00542g, puts in volumetric flask, uses methanol constant volume
To 25ml, make dissolving, shake up (0.2168mg/ml), more therefrom accurate absorption 0.5ml, with methanol dilution to 25ml, obtain 4.336 μ
G/ml reference substance solution.
The reference substance solution of different extraction times and the need testing solution of extracting method and above-mentioned new preparation sample introduction 10 μ respectively
L, calculates protostermonine content in granule, the results are shown in Table 22.Owing to ultrasonic 40min and ultrasonic 60min, backflow 1h record former hundred
The content of portion's alkali is identical, therefore selects the extracting method sample preparation of ultrasonic 40min, the most both simplified operation steps, reduces again operation
Time.
Table 22 extraction time examines or check result with method
| Extracting method | Sample weighting amount (g) | Peak area | Protostermonine content (%) |
| Ultrasonic 20min | 0.3939 | 322.02 | 0.011 |
| Ultrasonic 40min | 0.4085 | 358.70 | 0.012 |
| Ultrasonic 60min | 0.3910 | 364.72 | 0.012 |
| Cocurrent flow 1h | 0.3950 | 350.26 | 0.012 |
Through above-mentioned investigation, determine that need testing solution preparation method is as follows:
The preparation of need testing solution: take this product about 0.4g prepared by Radix Stemonae, accurately weighed, put 50ml tool plug conical flask
In, accurate addition 10ml methanol, close plug, weigh, ultrasonic 40min, let cool, be re-weighed, supply the weight of less loss, shake up, filter,
Take subsequent filtrate as need testing solution.
3. linear relationship examination
Draw above-mentioned protostermonine reference substance solution (4.336 μ g/ml) 4 μ l, 8 μ l, 12 μ l, 16 μ l, 20 μ l respectively, inject
Chromatograph of liquid, measures protostermonine reference substance peak area, the results are shown in Table 23.With reference substance sample size (μ g) as abscissa, color
Spectral peak peak area is that vertical coordinate draws standard curve, and result is shown in accompanying drawing 5.
Calculating regression equation is: Y=7545.6X+6.2048, r=0.9997.Show that protostermonine is at 0.01734 μ g
～0.08672 μ g range internal linear relation good.
Table 23 protostermonine linear relationship examination result
| Sampling volume (μ l) | Sample size (μ g) | Peak area |
| 4 | 0.01734 | 134.31 |
| 8 | 0.03469 | 268.04 |
| 12 | 0.05203 | 400.54 |
| 16 | 0.06938 | 537.03 |
| 20 | 0.08672 | 654.16 |
4. precision test
Accurate concentration of drawing is 4.336 μ g/ml protostermonine reference substance solution 10 μ l, continuously repeats sample introduction 6 times, measures former
(-)-Stemoninine chromatographic peak peak area, calculating RSD is 0.61%, the results are shown in Table 24.Show that the method precision is good.
Table 24 Precision test result
| Number of injections | Peak area | Meansigma methods | RSD (%) |
| 1 | 336.48 | ||
| 2 | 336.11 | ||
| 3 | 335.91 | 336.96 | 0.61 |
| 4 | 337.72 | ||
| 5 | 337.32 | ||
| 6 | 337.18 |
5. the stability test of need testing solution
Investigate the method determined under item according to need testing solution preparation method, taking Radix Stemonae is granule prepared by raw material
(only indicating Radix Stemonae, without lot number) prepares need testing solution, respectively at 0, within 1,2,3,4,5,6,7,8,9,10,11 hour, enters
Sample, each sample introduction 10 μ l, measure the chromatographic peak peak area of protostermonine in need testing solution.The results are shown in Table 25.Show test sample
Solution is basicly stable in 11h, and RSD is 1.72%.
Table 25 stability test result
| Time (h) | Peak area | Meansigma methods | RSD (%) |
| 0 | 359.71 | ||
| 1 | 360.24 | ||
| 2 | 360.46 | ||
| 3 | 360.29 | ||
| 4 | 360.78 | ||
| 5 | 362.48 | ||
| 6 | 364.34 | 362.31 | 1.72 |
| 7 | 362.91 | ||
| 8 | 363.97 | ||
| 9 | 363.86 | ||
| 10 | 364.47 | ||
| 11 | 364.26 |
6. replica test
Take granule (20120503 batches), investigate, according to need testing solution preparation method, the method determined under item and prepare test sample
Solution, operation repetitive is prepared 6 parts, is distinguished sample introduction 10 μ l, measures the chromatographic peak peak area of protostermonine in need testing solution, calculates
The average content of protostermonine is 0.0077%, and RSD is 1.09%.The results are shown in Table 26.Show that this assay method repeatability is good.
Table 26 replica test result (20120503 batches)
7. average recovery test
Take granule (20120503 crowdes) about 0.2g, accurately weighed, the accurate protostermonine pair adding 4.336 μ g/ml
According to product solution 3.8ml, more accurate addition methanol 6.2ml, weigh, ultrasonic 40min, let cool, be re-weighed, mend weight, shake up, filter,
Taking subsequent filtrate as need testing solution, operation repetitive prepares 6 parts, respectively sample introduction 10 μ l, measures protostermonine in need testing solution
Chromatographic peak peak area, calculate protostermonine the response rate, average recovery rate is 100.36%, and RSD is 3.63%.The results are shown in Table
27.Show that this assay method accuracy is qualified.
Table 27 average recovery result of the test
Sample determination result
According to the content assaying method of above-mentioned foundation, remaining 3 test sample granule is carried out the assay of protostermonine,
The results are shown in Table 28.
The assay result of protostermonine in table 28 test sample granule
Claims (2)
1. one kind is made up of the Radix Stemonae, Radix Asteris, Radix Peucedani, Radix Platycodonis, Bombyx Batryticatus, Periostracum Cicadae, Herba Ephedrae, Semen Armeniacae Amarum, Fructus Mume, Rhizoma Phragmitis, Radix Glycyrrhizae Preparata
The detection method of compositions, it is characterised in that include the discrimination method of Radix Asteris:
Method one:
Prepared by need testing solution: take this product powder 0.50g, adds methanol 25ml, supersound process 30 minutes, filters, and filtrate volatilizes, residual
Slag adds ethyl acetate 1 ml, makes dissolving, to obtain final product；
Prepared by control medicinal material solution: take control medicinal material powder 1.00g, with above-mentioned need testing solution preparation method, makes control medicinal material molten
Liquid；
Prepared by negative control solution: take negative control powder 0.52g, with above-mentioned need testing solution preparation method, makes negative control molten
Liquid；
Chromatographic identification is carried out, with the petroleum ether-diethyl ether solution of 9:1 as developing solvent, with 10% by the thin layer chromatography of States Pharmacopoeia specifications
Ethanol solution of sulfuric acid develops the color, and 105 DEG C to be heated to spot development clear；
Method two:
The preparation of need testing solution: take this product 4g, adds methanol 25ml, supersound process 30 minutes, filters, and filtrate volatilizes, and residue adds
Ethyl acetate 1 ml, makes dissolving, to obtain final product；
Prepared by negative control solution: take negative control powder 4g, with above-mentioned need testing solution preparation method, makes negative control solution；
Prepared by control medicinal material solution: take control medicinal material powder 1.00g, with above-mentioned need testing solution preparation method, makes control medicinal material molten
Liquid；
Point sample amount: need testing solution 15 μ l, negative control 15 μ l, control medicinal material 5 μ l；
Carry out chromatographic identification by the thin layer chromatography of States Pharmacopoeia specifications, make developing solvent with the petroleum ether-diethyl ether solution of 100:1, with 10%
Ethanol solution of sulfuric acid develops the color, and 105 DEG C to be heated to spot development clear.
2. detection method described in claim 1, it is characterised in that also include Rhizoma Phragmitis, Radix Platycodonis, Fructus Mume, Semen Armeniacae Amarum, Bombyx Batryticatus and Periostracum Cicadae
Discriminating: it is characterized in that,
The discriminating of Rhizoma Phragmitis:
Method one
Method for making sample: weigh test sample 1.00g, control medicinal material 1.00g, negative control 1.00g respectively, adds methanol 25ml, ultrasonic
Processing 30 minutes, filter, filtrate volatilizes, and residue adds ethyl acetate 1 ml, makes dissolving, obtains need testing solution, control medicinal material molten
Liquid, negative control solution；
Carry out chromatographic identification by the thin layer chromatography of States Pharmacopoeia specifications, developing solvent one in the following developing solvent, with vanillin-
10% ethanol solution of sulfuric acid colour developing, 105 DEG C to be heated to spot development clear；
Developing solvent: 1. chloroform-formic acid mixed solution, volume ratio 100:1；2. petroleum ether-chloroform mixed solution, volume
Compare 1:1；3. petroleum ether-chloroform mixed solution, volume ratio 4:1；5. petroleum ether-chloroform mixed solution, volume ratio 2:
1；
Method two
Method for making sample: weigh Rhizoma Phragmitis medical material 0.50g, test sample 2.00g, negative control 2.00g respectively, adds methanol 25ml, ultrasonic
Processing 30 minutes, filter, filtrate volatilizes, and residue adds ethyl acetate 1 ml, makes dissolving, obtains control medicinal material solution, test sample molten
Liquid, negative control solution；
Carrying out chromatographic identification by the thin layer chromatography of States Pharmacopoeia specifications, developing solvent is petroleum ether-chloroform-formic acid mixed solution,
Volume ratio 4:1:0.05, develops the color with vanillin-10% ethanol solution of sulfuric acid, and 105 DEG C to be heated to spot development clear；
The discriminating of Radix Platycodonis:
Method one
Need testing solution is prepared: taking sample particle 0.56g, adding volume ratio is by thin-layer identification method under 2010 editions pharmacopeia Radix Platycodonis items
The mixed solution 20ml of the 7% sulphuric acid alcohol-water of 1:3, is heated to reflux 3h, lets cool, and shakes extraction 2 times with chloroform, every time
20ml, merges chloroform liquid, and add water washing 2 times, and each 30ml discards washing liquid, chloroform liquid anhydrous sodium sulfate dehydration,
Filtering, filtrate is evaporated, and residue adds methanol 1ml makes dissolving, obtains need testing solution, then takes control medicinal material 1.06g, negative right respectively
According to 0.55g, with the preparation method of need testing solution, prepare control medicinal material solution, negative control solution respectively, and by three kinds of solution
Put respectively on same silica gel g thin-layer plate, select a kind of expansion in following developing solvent, develop the color with 10% ethanol solution of sulfuric acid,
It is heated to spot development clear at 105 DEG C；
1. developing solvent: chloroform-ether mixed solution, volume ratio 2: 1；
2. developing solvent: chloroform-ether mixed solution, volume ratio 1: 1；
3. developing solvent: chloroform-petroleum ether mixed solution, volume ratio 1: 5；
4. developing solvent: chloroform-petroleum ether mixed solution, volume ratio 1: 1；
Method two
Extracting directly saponin component prepares need testing solution: take sample particle 0.50g, adds 15ml water, and ultrasonic 10min, with just
Butanol, before immunoassay 2 times, each 15ml, take n-butanol layer, heating is concentrated into 5ml, obtains need testing solution；Take negative control 0.50g,
With need testing solution preparation method, prepare negative control solution；Take Radix Platycodonis control medicinal material 1.0g again, be ground into powder, add 30ml water,
Decoct 30min, filter, obtain filtrate, cooling, with n-butanol extraction 2 times, each 20ml, take n-butanol layer, heating is concentrated into 5ml,
Obtain control medicinal material solution；And three kinds of solution are put on same silica gel g thin-layer plate respectively, select in following developing solvent
Plant and launch, with 10% ethanol solution of sulfuric acid colour developing, be heated to spot development at 105 DEG C clear；
1. developing solvent: n-butyl alcohol-ethyl acetate-water mixed solution, volume ratio 4:1:5, upper strata；
2. developing solvent: n-butyl alcohol-ethyl acetate-water mixed solution, volume ratio 1:4:5, upper strata；
3. developing solvent: chloroform-methanol-water mixed solution, volume ratio 13:7:2, lower floor；
4. developing solvent: chloroform-methanol-water mixed solution, volume ratio 15:5:2, lower floor；
5. developing solvent: chloroform-methanol-water mixed solution, volume ratio 9:1:1, lower floor；
The discriminating of Fructus Mume:
Method one
Taking sample particle 1.00g, add methanol 25ml, supersound process 30min, filter, filtrate is evaporated, and residue adds ethyl acetate 1ml,
Make dissolving, as need testing solution；Take negative control 1.00g again, take Fructus Mume control medicinal material 1.00g, pound and fragmentate, same to test sample
The preparation method of solution, prepares negative control solution, control medicinal material solution respectively；And three kinds of solution are put respectively in same silicon
On glue G lamellae, select a kind of expansion in following developing solvent, with vanillin-concentrated sulfuric acid solution colour developing, be heated at 105 DEG C
Spot development is clear；
1. developing solvent: chloroform-acetone-formic acid mixed solution, volume ratio 5:2:0.8；
2. developing solvent: cyclohexane-ethyl acetate-glacial acetic acid mixed solution, volume ratio 4:1:0.1；
3. developing solvent: chloroform-acetone-formic acid mixed solution, volume ratio 9:0.5:0.5；
4. developing solvent: chloroform；
5. developing solvent: chloroform-acetone mixed solution, volume ratio 50:1；
6. developing solvent: chloroform-formic acid mixed solution, volume ratio 100:1；
Method two
Method by extracting organic acid: take test sample 1.00g, negative control 1.04g, control medicinal material 1.06g respectively, be ground into powder
End, adds dilute hydrochloric acid 20ml, supersound process 30min, takes supernatant, and add diethyl ether extraction 2 times, and each 15ml merges ether solution, volatilizes
Solvent, residue adds dehydrated alcohol 1ml, makes dissolving, prepares need testing solution, negative control solution, control medicinal material solution the most respectively；
And three kinds of solution are put on same silica gel g thin-layer plate respectively, select a kind of expansion in following developing solvent, and develop the color, see
Examine；
1. developing solvent: hexamethylene-dichloromethane-glacial acetic acid mixed solution, volume ratio 8:8:1；
Colour developing: 1% ferric chloride ethanol solution and 1% potassium ferricyanide solution mixed in equal amounts, now joins, it is seen that light is inspected；
2. developing solvent: hexamethylene-chloroform mixed solution, volume ratio 1:10, colour developing: vanillin-concentrated sulfuric acid solution, 105
It is clear DEG C to be heated to spot development；
3. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:5:5；
4. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:5:5 ,+2 formic acid；
5. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:2:2 ,+2 formic acid；
6. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:2:4 ,+4 formic acid；
7. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:1:1 ,+4 formic acid；
8. developing solvent: hexamethylene-dichloromethane-ethyl acetate-formic acid mixed solution, volume ratio 4:1:1:0.1；
When selecting 3.-8. described developing solvent to launch, with 5% vanillin-concentrated sulfuric acid solution colour developing, it is heated to speckle at 105 DEG C and shows
Color is clear；
Method three
By official method: take test sample 4.00g, negative control 4.00g, control medicinal material 1.00g respectively, be ground into powder, add methanol
30ml, supersound process 30min, filter, take filtrate, be evaporated, residue adds 20ml water, dissolves, then the extraction 2 times that adds diethyl ether, every time
20ml, merges ether solution, is evaporated, and residue petroleum ether soaks 2 times, and each 15ml, incline petroleum ether, the anhydrous second of residue 2ml
Alcohol dissolves, and prepares need testing solution, negative control solution, control medicinal material solution the most respectively, and is put respectively by three kinds of solution in same
On one piece of silica gel g thin-layer plate, select a kind of expansion in following developing solvent, with 10% ethanol solution of sulfuric acid colour developing, add at 105 DEG C
Heat is clear to spot development；
1. developing solvent: hexamethylene-dichloromethane-ethyl acetate-formic acid mixed solution, volume ratio 20:5:8:0.1；
2. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:1:1 ,+1 formic acid；
3. developing solvent: hexamethylene-dichloromethane-ethyl acetate mixed solution, volume ratio 1:3:3 ,+2 formic acid；
Amygdalate discriminating:
By official method sample preparation: separately sampled product 5.51g, control medicinal material 1.03g, negative control 5.35g, put apparatus,Soxhlet's
In, adding 50ml dichloromethane, be heated to reflux 2h, discard dichloromethane solution, medicinal residues volatilize, then add methanol 50ml, are heated to reflux
40min, lets cool, and filters, obtains filtrate, reclaims methanol, is concentrated into 15ml, obtains three kinds of solution, and three kinds of solution are put respectively in
On same silica gel g thin-layer plate, if selecting a kind of expansion in the developing solvent of following (1)-(6), with 15% sulphuric acid of 0.8% phosphomolybdic acid
Ethanol solution leaching plate colour developing, 105 DEG C to be heated to spot development clear；If selecting developing solvent (7) to launch, show with vanillin concentrated sulphuric acid
Color, 105 DEG C to be heated to spot development clear；
(1) chloroform-acetate-methanol-water mixed solution, volume ratio 15:40:22:10, lower floor, place 12 for 5～10 DEG C
h；
(2) chloroform-acetate-methanol-water mixed solution, volume ratio 2:4:1:1, lower floor；
(3) chloroform-acetate-methanol-water mixed solution, volume ratio 4:1:1:1, lower floor；
(4) chloroform-acetate-methanol-water mixed solution, volume ratio 8:1:0.5:1, lower floor；
(5) chloroform；
(6) chloroform-methanol mixed solution, volume ratio 1:1；
(7) chloroform-methanol mixed solution, volume ratio 1: 5；
Bombyx Batryticatus and the discriminating of Periostracum Cicadae
Bombyx Batryticatus, the preparation of the double-negative contrast solution of Periostracum Cicadae: weigh Radix Stemonae 16.59g, Radix Peucedani 12.52g, Herba Ephedrae 6.24g, Semen Armeniacae Amarum
9.38g, 70% alcohol reflux 3 times, united extraction liquid, filter, decompression filtrate recycling ethanol is concentrated into paste, and thick paste is standby；
Weigh Radix Asteris 12.50g, Radix Platycodonis 12.48g, Radix Glycyrrhizae 6.25g, Rhizoma Phragmitis 12..52g, Fructus Mume 6.21g, soak by water 2 times, merge
Decocting liquid, filters, and it is 1.03～1.05 that filtrate is concentrated into 50 DEG C of relative densities, adds ethanol and makes alcohol content reach 60%, stands
24h, takes supernatant and filters, and decompression filtrate recycling ethanol is concentrated into paste, and thick paste is standby；
By two kinds of thick paste mixings, obtain negative thick paste；Weigh negative thick paste 1.28g, put in tool plug conical flask, accurate addition 70% second
Alcohol 5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product；
The preparation of need testing solution: weigh sample particle 3.19g, puts in tool plug conical flask, and the accurate 70% ethanol 5ml that adds is close
Plug, supersound process 30min, filter, take subsequent filtrate and get final product；
Prepared by Bombyx Batryticatus control medicinal material solution: take Bombyx Batryticatus control medicinal material 0.64g, puts in tool plug conical flask, accurate addition 70% ethanol
5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product；
Prepared by Periostracum Cicadae control medicinal material solution: take Periostracum Cicadae control medicinal material 0.40g, puts in tool plug conical flask, accurate addition 70% ethanol
5ml, close plug, supersound process 30min, filter, take subsequent filtrate and get final product；
Chromatographic identification is carried out by the thin layer chromatography of States Pharmacopoeia specifications, developing solvent one in following developing solvent, use 2.04mg/
The ethanol solution of ninhydrin colour developing of ml；
1. developing solvent: n-butyl alcohol-glacial acetic acid-water mixed solution, volume ratio 8:3:3；
2. developing solvent: n-butyl alcohol-glacial acetic acid-water mixed solution, volume ratio 3:1:1.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210549017.3A CN103869041B (en) | 2012-12-08 | 2012-12-08 | A kind of detection method of cough-relieving combination of oral medication |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210549017.3A CN103869041B (en) | 2012-12-08 | 2012-12-08 | A kind of detection method of cough-relieving combination of oral medication |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103869041A CN103869041A (en) | 2014-06-18 |
| CN103869041B true CN103869041B (en) | 2016-08-24 |
Family
ID=50907802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210549017.3A Expired - Fee Related CN103869041B (en) | 2012-12-08 | 2012-12-08 | A kind of detection method of cough-relieving combination of oral medication |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103869041B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849369B (en) * | 2015-05-13 | 2016-07-13 | 济南康众医药科技开发有限公司 | The attached sweet drug quality detection method of a kind of fiber crops |
| CN106124686A (en) * | 2016-08-31 | 2016-11-16 | 天津中新药业研究中心 | A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine |
| CN107817313B (en) * | 2017-10-18 | 2019-10-25 | 广州白云山敬修堂药业股份有限公司 | The scattered quality determining method of a kind of day yellow bezoar from monkeys |
| CN108426955A (en) * | 2018-03-11 | 2018-08-21 | 安徽省食品药品检验研究院 | The discrimination method of tuber of stemona genunie medicinal materials |
| CN110082471B (en) * | 2019-05-09 | 2021-04-27 | 四川逢春制药有限公司 | Detection method of platycodon grandiflorum and winter flower tablets |
| CN110082470B (en) * | 2019-05-09 | 2021-03-16 | 四川逢春制药有限公司 | Detection method of san Tan Ning syrup |
| CN112763643A (en) * | 2021-01-19 | 2021-05-07 | 世达标准检测技术服务(深圳)有限公司 | TLC identification method for radix stemonae in compound fructus momordicae cough relieving granules |
| CN113189261B (en) * | 2021-04-30 | 2022-08-16 | 广州白云山中一药业有限公司 | Platycodon grandiflorum detection method based on thin-layer chromatography |
| CN113295817A (en) * | 2021-06-30 | 2021-08-24 | 江西农业大学 | Preparation, separation and identification method of phoenix-tail fern bacteriostatic component |
| CN114674953B (en) * | 2022-03-24 | 2023-06-06 | 天津中医药大学 | Method for measuring content of chemical components in dark plums |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515272A (en) * | 2003-01-08 | 2004-07-28 | 江苏康缘药业股份有限公司 | Chinese medicine composition for curing cough, its preparation method and quality control method |
| CN1557432A (en) * | 2004-02-02 | 2004-12-29 | 四川省仁德制药有限公司 | Preparing process of medicinal composition for treating acute and chronic bronchitis |
| CN1840118A (en) * | 2005-03-30 | 2006-10-04 | 张友生 | Compound preparation for treating bronchitis, its preparation method and quality control method |
| CN101062294A (en) * | 2007-06-08 | 2007-10-31 | 江苏南星药业有限责任公司 | Method for detecting the quality of the medicine combination for treating cerebral apoplexy and vasculitis |
| CN101190282A (en) * | 2006-11-22 | 2008-06-04 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Sugar-free compound traditional Chinese medicinal preparation for treating upper respiratory tract infection and quality control method thereof |
| CN101780146A (en) * | 2009-01-19 | 2010-07-21 | 天津达仁堂京万红药业有限公司 | Quality control method of Biqi capsules |
| CN102526568A (en) * | 2012-01-03 | 2012-07-04 | 迪沙药业集团山东迪沙药业有限公司 | Traditional Chinese medicine compound composition |
| CN102590431A (en) * | 2012-02-10 | 2012-07-18 | 济南康众医药科技开发有限公司 | Quality standard detection method for Chinese medicinal composition for treating cough |
-
2012
- 2012-12-08 CN CN201210549017.3A patent/CN103869041B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515272A (en) * | 2003-01-08 | 2004-07-28 | 江苏康缘药业股份有限公司 | Chinese medicine composition for curing cough, its preparation method and quality control method |
| CN1557432A (en) * | 2004-02-02 | 2004-12-29 | 四川省仁德制药有限公司 | Preparing process of medicinal composition for treating acute and chronic bronchitis |
| CN1840118A (en) * | 2005-03-30 | 2006-10-04 | 张友生 | Compound preparation for treating bronchitis, its preparation method and quality control method |
| CN101190282A (en) * | 2006-11-22 | 2008-06-04 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Sugar-free compound traditional Chinese medicinal preparation for treating upper respiratory tract infection and quality control method thereof |
| CN101062294A (en) * | 2007-06-08 | 2007-10-31 | 江苏南星药业有限责任公司 | Method for detecting the quality of the medicine combination for treating cerebral apoplexy and vasculitis |
| CN101780146A (en) * | 2009-01-19 | 2010-07-21 | 天津达仁堂京万红药业有限公司 | Quality control method of Biqi capsules |
| CN102526568A (en) * | 2012-01-03 | 2012-07-04 | 迪沙药业集团山东迪沙药业有限公司 | Traditional Chinese medicine compound composition |
| CN102590431A (en) * | 2012-02-10 | 2012-07-18 | 济南康众医药科技开发有限公司 | Quality standard detection method for Chinese medicinal composition for treating cough |
Non-Patent Citations (4)
| Title |
|---|
| 中药复方制剂质量控制的研究;杨胜 等;《中国医药生物技术》;20101010;第5卷(第5期);第387页左栏第4段 * |
| 中药百部中原百部碱的分离及含量测定;张彤 等;《中国药学杂志》;20070608;第42卷(第11期);第813-814页"2.3 原百部碱的HPLC测定方法的建立"小节 * |
| 康视明合剂质量标准研究;吴樱 等;《中国药房》;20080930;第19卷(第27期);第2135页"3.2 甘草酸铵的含量测定"小节 * |
| 高效液相色谱法测定利肺止咳颗粒中盐酸麻黄碱的含量;翟贰明 等;《中国医院药学杂志》;20110730;第31卷(第14期);第1221页"2 方法与结果"小节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103869041A (en) | 2014-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103869041B (en) | A kind of detection method of cough-relieving combination of oral medication | |
| CN107367562B (en) | Analysis and detection method and application of polymyxin B sulfate | |
| CN104398642A (en) | Preparation and quality detection method of compound prescription cortex phellodendri chinensis fluid | |
| CN104502518B (en) | A kind of detection method for the treatment of the Chinese medicine preparation of baby anorexia | |
| CN101618119A (en) | Quality standard of Sinopanax formosanus pills | |
| CN101444604A (en) | Chinese medicine granular formulation to therapy children anorexia and preparation method thereof and detection method | |
| CN114689775A (en) | Peony and licorice root decoction fingerprint spectrum, construction method thereof and detection method of peony and licorice root decoction product | |
| CN109085285B (en) | Quality control method of changyanning granules | |
| CN101264226B (en) | Quality detecting method of diabetes treating medicine | |
| CN101181589A (en) | Method for detecting the mass of tsunematsu 8-flavour agilawood tambac tablet | |
| CN101703610A (en) | Quality detection method of Qingnao antihypertensive tablet | |
| CN101703583B (en) | Method for detecting quality of Xinning capsule | |
| CN108037200B (en) | Quality detection method of kidney nourishing and tranquilizing pills | |
| CN108037234B (en) | Quality detection method of abrus herb hepatitis granules | |
| CN104345108B (en) | Qualitative quantitative determination method for liver-heat-clearing tablet | |
| CN101987115A (en) | Jade screen oral preparation as well as preparation method and detection method thereof | |
| CN113759057B (en) | Characteristic spectrum of allium macrostemon white water extract and preparation thereof and construction method thereof | |
| CN105616946A (en) | Preparation for treating cough, preparation method and quality control method thereof | |
| CN101112422A (en) | Quality control method of particles for eliminating phlegm and stopping cough for children | |
| CN101028474B (en) | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions | |
| CN110857939B (en) | Detection method of traditional Chinese medicine composition with sleep improvement function | |
| CN112946129A (en) | Quality detection method of antidiarrheal syrup | |
| CN109507356B (en) | Quality detection method of 'Hui Tongbiang' capsule | |
| CN101912522A (en) | Detection method of Liuweisheng tablets | |
| CN110487950A (en) | A kind of detection method of eight taste ball of heat-clearing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160831 Address after: 264205 No. 1 South Qingdao Road, Weihai economic and technological development, Shandong Patentee after: Disha Pharmaceutical Industry Group Corp., Ltd. Patentee after: Weihai Disu Pharmaceutical Co., Ltd. Address before: 264205 No. 1 South Qingdao Road, Weihai economic and technological development, Shandong Patentee before: Disha Pharmaceutical Industry Group Corp., Ltd. Patentee before: Disha Pharmaceutical Group Shandong Disha Pharmaceutical Co., Ltd. Patentee before: Weihai Disu Pharmaceutical Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160824 Termination date: 20201208 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |