CN101732553B - Quality inspection method of cough pills - Google Patents
Quality inspection method of cough pills Download PDFInfo
- Publication number
- CN101732553B CN101732553B CN2010101021539A CN201010102153A CN101732553B CN 101732553 B CN101732553 B CN 101732553B CN 2010101021539 A CN2010101021539 A CN 2010101021539A CN 201010102153 A CN201010102153 A CN 201010102153A CN 101732553 B CN101732553 B CN 101732553B
- Authority
- CN
- China
- Prior art keywords
- solution
- thin
- add
- cough
- reference substance
- 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.)
- Active
Links
- 206010011224 Cough Diseases 0.000 title claims abstract description 51
- 239000006187 pill Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000007689 inspection Methods 0.000 title abstract description 8
- VVOAZFWZEDHOOU-UHFFFAOYSA-N magnolol Chemical compound OC1=CC=C(CC=C)C=C1C1=CC(CC=C)=CC=C1O VVOAZFWZEDHOOU-UHFFFAOYSA-N 0.000 claims abstract description 27
- BALXUFOVQVENIU-GNAZCLTHSA-N Ephedrine hydrochloride Chemical compound Cl.CN[C@@H](C)[C@H](O)C1=CC=CC=C1 BALXUFOVQVENIU-GNAZCLTHSA-N 0.000 claims abstract description 24
- 229960002534 ephedrine hydrochloride Drugs 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 81
- 238000012360 testing method Methods 0.000 claims description 63
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 61
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000013558 reference substance Substances 0.000 claims description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 16
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims description 16
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims description 16
- 238000004587 chromatography analysis Methods 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- 244000124853 Perilla frutescens Species 0.000 claims description 14
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 241001465251 Ephedra sinica Species 0.000 claims description 12
- 235000004347 Perilla Nutrition 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 240000000249 Morus alba Species 0.000 claims description 9
- 229910021538 borax Inorganic materials 0.000 claims description 9
- 239000004328 sodium tetraborate Substances 0.000 claims description 9
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 235000008708 Morus alba Nutrition 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 8
- 241001116477 Adenophora triphylla Species 0.000 claims description 7
- 244000194101 Ginkgo biloba Species 0.000 claims description 7
- BYTORXDZJWWIKR-UHFFFAOYSA-N Hinokiol Natural products CC(C)c1cc2CCC3C(C)(CO)C(O)CCC3(C)c2cc1O BYTORXDZJWWIKR-UHFFFAOYSA-N 0.000 claims description 7
- 241000218378 Magnolia Species 0.000 claims description 7
- 241000244269 Peucedanum Species 0.000 claims description 7
- 235000006753 Platycodon grandiflorum Nutrition 0.000 claims description 7
- 244000197580 Poria cocos Species 0.000 claims description 7
- 241000107360 Vincetoxicum glaucescens Species 0.000 claims description 7
- FVYXIJYOAGAUQK-UHFFFAOYSA-N honokiol Chemical compound C1=C(CC=C)C(O)=CC=C1C1=CC(CC=C)=CC=C1O FVYXIJYOAGAUQK-UHFFFAOYSA-N 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 241000801118 Lepidium Species 0.000 claims description 6
- 244000246386 Mentha pulegium Species 0.000 claims description 6
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 6
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 6
- 240000003582 Platycodon grandiflorus Species 0.000 claims description 6
- 235000008599 Poria cocos Nutrition 0.000 claims description 6
- 238000012850 discrimination method Methods 0.000 claims description 6
- 235000001050 hortel pimenta Nutrition 0.000 claims description 6
- 244000273928 Zingiber officinale Species 0.000 claims description 5
- 235000006886 Zingiber officinale Nutrition 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 235000008397 ginger Nutrition 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 235000019890 Amylum Nutrition 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000003556 assay Methods 0.000 claims description 4
- UWUZCDRVSPBFDA-UHFFFAOYSA-N benzene;chloroform;ethyl acetate Chemical compound ClC(Cl)Cl.CCOC(C)=O.C1=CC=CC=C1 UWUZCDRVSPBFDA-UHFFFAOYSA-N 0.000 claims description 4
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 4
- 210000004027 cell Anatomy 0.000 claims description 4
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 claims description 4
- 229960002327 chloral hydrate Drugs 0.000 claims description 4
- SKCNIGRBPJIUBQ-UHFFFAOYSA-N chloroform;ethyl acetate Chemical compound ClC(Cl)Cl.CCOC(C)=O SKCNIGRBPJIUBQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013530 defoamer Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- -1 each 10-20ml Substances 0.000 claims description 4
- 210000003743 erythrocyte Anatomy 0.000 claims description 4
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 239000012634 fragment Substances 0.000 claims description 4
- 239000004519 grease Substances 0.000 claims description 4
- 230000001788 irregular Effects 0.000 claims description 4
- 239000004816 latex Substances 0.000 claims description 4
- 229920000126 latex Polymers 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 210000002955 secretory cell Anatomy 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000011003 system suitability test Methods 0.000 claims description 4
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 241001522129 Pinellia Species 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 241000050051 Chelone glabra Species 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 13
- 229940079593 drug Drugs 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000003908 quality control method Methods 0.000 abstract description 6
- 230000005180 public health Effects 0.000 abstract description 5
- 244000183685 Citrus aurantium Species 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000009472 formulation Methods 0.000 abstract description 3
- 235000007716 Citrus aurantium Nutrition 0.000 abstract 2
- 230000000694 effects Effects 0.000 description 23
- 206010062717 Increased upper airway secretion Diseases 0.000 description 13
- 208000026435 phlegm Diseases 0.000 description 13
- 210000004072 lung Anatomy 0.000 description 11
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 description 8
- 208000006673 asthma Diseases 0.000 description 6
- 241000207929 Scutellaria Species 0.000 description 5
- 206010006451 bronchitis Diseases 0.000 description 4
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229960002179 ephedrine Drugs 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 210000000952 spleen Anatomy 0.000 description 3
- 206010006458 Bronchitis chronic Diseases 0.000 description 2
- 208000000059 Dyspnea Diseases 0.000 description 2
- 206010013975 Dyspnoeas Diseases 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 241000935235 Fritillaria meleagris Species 0.000 description 2
- 241000202807 Glycyrrhiza Species 0.000 description 2
- 241001673966 Magnolia officinalis Species 0.000 description 2
- 244000274050 Platycodon grandiflorum Species 0.000 description 2
- 206010036790 Productive cough Diseases 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 208000007451 chronic bronchitis Diseases 0.000 description 2
- 208000013116 chronic cough Diseases 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 208000024794 sputum Diseases 0.000 description 2
- 210000003802 sputum Anatomy 0.000 description 2
- 238000009495 sugar coating Methods 0.000 description 2
- 208000011580 syndromic disease Diseases 0.000 description 2
- 241001412627 Adenophora liliifolia Species 0.000 description 1
- 241001633574 Adenophora stricta Species 0.000 description 1
- 241000208327 Apocynaceae Species 0.000 description 1
- 240000006891 Artemisia vulgaris Species 0.000 description 1
- 241000208671 Campanulaceae Species 0.000 description 1
- 241000282461 Canis lupus Species 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 241000125183 Crithmum maritimum Species 0.000 description 1
- 244000264242 Descurainia sophia Species 0.000 description 1
- 235000017680 Descurainia sophia Nutrition 0.000 description 1
- 241000723281 Ephedra equisetina Species 0.000 description 1
- 241000723237 Ephedra intermedia Species 0.000 description 1
- 241000218670 Ephedraceae Species 0.000 description 1
- 241001547127 Fritillaria cirrhosa Species 0.000 description 1
- 241001644297 Fritillaria delavayi Species 0.000 description 1
- 241001644295 Fritillaria przewalskii Species 0.000 description 1
- 241001644290 Fritillaria unibracteata Species 0.000 description 1
- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
- 208000008454 Hyperhidrosis Diseases 0.000 description 1
- 241001657511 Lepidium apetalum Species 0.000 description 1
- 235000001878 Mentha haplocalyx Nutrition 0.000 description 1
- 244000280293 Mentha haplocalyx Species 0.000 description 1
- 206010068319 Oropharyngeal pain Diseases 0.000 description 1
- 240000001090 Papaver somniferum Species 0.000 description 1
- 201000007100 Pharyngitis Diseases 0.000 description 1
- 241001522232 Pinellia ternata Species 0.000 description 1
- 235000006751 Platycodon Nutrition 0.000 description 1
- 241000222341 Polyporaceae Species 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 235000016551 Potentilla erecta Nutrition 0.000 description 1
- 240000000103 Potentilla erecta Species 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 241001180873 Saposhnikovia divaricata Species 0.000 description 1
- 241000576755 Sclerotia Species 0.000 description 1
- 240000004534 Scutellaria baicalensis Species 0.000 description 1
- 244000297179 Syringa vulgaris Species 0.000 description 1
- 235000004338 Syringa vulgaris Nutrition 0.000 description 1
- 241000729171 Vincetoxicum stauntonii Species 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 208000013219 diaphoresis Diseases 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical group [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 230000037306 mature skin Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 229930189914 platycodon Natural products 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a quality inspection method of cough pills prescribed in Volume 11 of Drug Standard of Ministry of Public Health of the People's Republic of China (Chinese Traditional Patent Formulation Preparations). The quality inspection method comprises microscopic identification of cough pills, a thin-layer chromatography identification method of ephedrine hydrochloride, magnolol and dried orange peel, a thin-layer chromatography qualitative identification method of bitter orange and a content determination method of ephedrine hydrochloride in the cough pills. The quality inspection method raises the quality control standards of cough pills and establishes content determination inspection indexes of main drugs in a preparation and a inspection method thereof; and meanwhile, the quality inspection method deletes physical and chemical reaction identification of poor specialization and adds the thin-layer chromatography qualitative identification method of ephedrine hydrochloride, magnolol, dried orange peel and bitter orange, thereby ensuring a higher quality standard level of compound preparations of cough pills.
Description
Technical field
The present invention relates to the quality determining method of cough pill in the 11 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Background technology
Medicine cough pill (WS in the 11 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation)
3-B-2096-96), having lowering the adverse-rising QI to resolve phlegm, the effect of relieving cough and relieving asthma is used for chill and goes into lung, the coughing with a lot of sputum that Lung Qi obstruction causes, syndrome characterized by dyspnea is uncomfortable in chest, and malasia or chronic cough are more than, and old acute/chronic bronchitis.This compound preparation is made up of Chinese medicine Chinese ephedra 20g, perilla seed 40g, the bark of official magnolia (ginger is processed) 50g, lepidium seed 20g, Bulbus Fritillariae Cirrhosae 4g, rhizoma pinellinae praeparata (sand stir-fry) 20g, gingko 18g, pappy shell 50g, borax 6g, Fructus Aurantii (bran stir-fry) 40g, dried orange peel 70g, balloonflower root 30g, windproof 40g, Poria cocos 70g, Cynanchum glaucescens 20g, root of purple-flowered peucedanum 30g, Radix Glycyrrhizae 40g, mulberry leaf 50g, the root of large-flowered skullcap (wine is processed) 10g, adenophora tetraphylla 60g, peppermint 50g, perilla leaf 40g.Main ingredient in the Chinese ephedra side of being, Chinese ephedra is the dry herbaceous stem stem of Ephedraceae plant plait Chinese ephedra Ephedra sinica Stapf, epheday intermedia Ephedra intermedia Schrenk et C.A.Mey. or ephedra equisetina Ephedra equisetina Bge., the tool Pulvis Diaphoreticus is cold, the effect of freeinging lung and relieving asthma; Perilla seed is the dry mature fruit of labiate purple perilla Perilla frutescens (L.) Britt., has the sending down abnormally ascending dissolving phlegm, relievings asthma the effect of ease constipation; The bark of official magnolia is dry dry hide, Gen Pi and the branch skin of Magnoliacea plant bark of official magnolia Magnolia officinalis Rehd.et Wils. or Magnolia bilola Magnolia officinalis Rehd.et Wils.var.biloba Rebd.et Wils., has the effect of eliminating dampness dissolving phlegm; Lepidium seed is crucifer Lepidium apetalum Lepidium apetalum Willd. or the dry mature seed of broadcasting ma wormwood artemisia Descurainia Sophia (L.) Webb ex Prantl, has removing heat from lung and relieving asthma, the effect of line water detumescence; Bulbus Fritillariae Cirrhosae is the dry bulb of liliaceous plant Bulbus Fritillariae Cirrhosae Fritillaria cirrhosa D.Don, dark violet bulb of fritillary Fritillaria unibracteata Hsiao et K.C.Hsia, Gansu bulb of fritillary Fritillaria przewalskii Maxim. or Bulbus Fritillariae cirrhosae Fritillaria delavayi Franch., have clearing heat and moistening lung, the effect of preventing phlegm from forming and stopping coughing; Rhizoma pinellinae praeparata is the process of preparing Chinese medicine processed goods (tuber of pinellia is the dry tuber of aroid tuber of pinellia Pinellia ternata (Thunb.) Breit.) of the tuber of pinellia, has eliminating dampness and eliminating phlegm effect; Gingko is the dry mature seed of Ginkgoaceae plant Ginkgo biloba Ginkgo biloba L., has the effect of astringing lung for relieving asthma; Pappy shell is the drying and ripening shell of bloodroot opium poppy Papaver somniferum L., has and astringes the lung, puckery intestines, the effect of pain relieving; Borax is a sodium tetraborate, contains Na
2B
4O
710H
2O should be 99.0～105.0%, and tool is clearing heat and detoxicating, the effect of clearing lung and eliminating phlegm; Fructus Aurantii is the dry immature fruit of rutaceae bitter orange Citrus aurantium L. and variety thereof, tool regulating the flow of QI to ease the stomach, the effect of the stagnant dissipate-swelling of row; Dried orange peel is the dry mature skin of rutaceae orange Citrus reticulate Blanco and variety thereof, has regulating qi-flowing for strengthening spleen, eliminating dampness and eliminating phlegm effect; Balloonflower root is the dry root of Campanulaceae Platycodon grandiflouorum Platycodon grandiflorum (Jacq.) A.DC., has a surname's lung, and relieve sore throat eliminates the phlegm, the effect of apocenosis; Windproof is the dry root of umbelliferae Saposhnikovia divaricata Saposhnikovia divaricata (Turcz.) Schischk., the effect of tool inducing diaphoresis to dispel wind; Poria cocos is the dry sclerotia of Polyporaceae fungi Poria cocos Poria cocos (Schw.) Wolf, has clearing damp and promoting diuresis, the effect of the peaceful heart of invigorating the spleen; Cynanchum glaucescens is dry rhizome and the root of Asclepiadaceae plant rhizoma et radix cynanchi stauntoni Cynanchum stauntonii (Dec-ne.) Schltr.ex Levl. or lilac daphne leaf Cynanchum glaucescens Cynanchum glaucescens (Dcene.) Hand.-Mazz., have sending down abnormally ascending, dissolving phlegm, the effect of cough-relieving; The root of purple-flowered peucedanum is the dry root of samphire RADIX PEUCEDANI Peucedanum praeruptorm Dunn, has diffusing wind heat-clearing, the effect of lowering the adverse-rising QI to resolve phlegm; Radix Glycyrrhizae is the dry root and rhizome of glycyrrhizic legume Glycyrrhiza inflata Bat., glycyrrhiza inflate bat Glycyrrhiza in flata Bat or glycyrrhiza glabra Glycyrrhiza glabra L., have and invigorate the spleen and benefit qi, clearing heat and detoxicating, expelling phlegm and arresting coughing, the effect of coordinating the drug actions of a prescription; Mulberry leaf are the dried leaves of moraceae plants mulberry Morus alba L., have dispelling wind and heat from the body, the effect of clearing away the lungheat and moisturizing; The root of large-flowered skullcap is the dry root of labiate root of large-flowered skullcap Scutellaria baicalensis Georgi, has heat-clearing and damp-drying drug, the effect of purging intense heat and detonicating; Adenophora tetraphylla is the dry root of Campanulaceae plant adenophora tetraphylla Adenophora tetraphylla (Thunb.) Fisch. or the root of straight ladybell Adenophora stricta Miq., has nourishiing yin to clear away the lung-heat, reduces phlegm the effect of beneficial gas; Peppermint is the dry aerial parts of labiate Mentha haplocalyx Briq., tool dispelling wind-heat, refresh oneself, the effect of promoting eruption; Perilla leaf is the dried leaves (or band spray) of labiate purple perilla Perilla frutescens (L.) Britt, has the cold effect of loosing of inducing sweat." Drug Standard of Ministry of Public Health of the Peoples Republic of China " the ten quality control standard (WS who has issued cough pill
3-B-2096-96), but in the existing cough pill method of quality control that the Ministry of Public Health issues, have only microscopical identification and physical and chemical reaction to differentiate that limitation is very big, is difficult to accurately control the quality of cough pill.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of quality determining method of cough pill is provided, to improve the quality control standard of cough pill.
The pharmaceutical formulation of cough pill is: Chinese ephedra 20g, perilla seed 40g, the bark of official magnolia (ginger is processed) 50g, lepidium seed 20g, Bulbus Fritillariae Cirrhosae 4g, rhizoma pinellinae praeparata (sand stir-fry) 20g, gingko 18g, pappy shell 50g, borax 6g, Fructus Aurantii (bran stir-fry) 40g, dried orange peel 70g, balloonflower root 30g, windproof 40g, Poria cocos 70g, Cynanchum glaucescens 20g, root of purple-flowered peucedanum 30g, Radix Glycyrrhizae 40g, mulberry leaf 50g, the root of large-flowered skullcap (wine is processed) 10g, adenophora tetraphylla 60g, peppermint 50g, perilla leaf 40g.
The quality determining method of cough pill of the present invention is:
1, get cough pill and put the microscopically observation: the dendritic agglomerate of irregular branch is colourless, meets chloral hydrate liquid and dissolves; Hyphae colorless or light brown, diameter 4～6 μ m.Grease chamber's fragment contains the volatilization oil droplet, and is faint yellow, and secretory cell includes the yellowish-brown thing; The corner place of part similar round or elliptical erythrocyte often thickens; Connect latex dust and include small faint yellow granular substance; The fiber bunchy, faint yellow, bast fiber is more rare, fusiformis, wall thickness.The conduit scalariform, reticulate pattern is more sees that bordered pit is rare, and test-tube baby is tiny; Needle-like calcium oxalate crystal is dispersed in more, prismatic crystal multiaspect shape.Nonglandular hair is often broken, and one to several cells compositions.Amylum body similar round, oval, omphalion slit-like, starlike, point-like and herringbone shape;
2, the thin-layer chromatography discrimination method of ephedrine hydrochloride: it is an amount of to get cough pill, remove sugar-coat, grind, get powder 20g, (volume proportion 8: 2) the mixed liquor 70-90ml that adds diethyl ether-absolute ethyl alcohol adds strong ammonia solution 2-3ml again, close plug, jolting constantly, placement is spent the night, and filters, residue washs at twice with ether 10-20ml, washing lotion and filtrate merge, and add ethanol solution hydrochloride (1 → 20) (referring to that 1ml hydrochloric acid adds ethanol and makes into 20ml solution) 2-3ml, shake up, in water-bath, steam near and do, residue adds methyl alcohol 2ml and stirs and to make moltenly, and with a little absorbent cotton filtration, filtrate is as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin-layered chromatography test (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned need testing solution 5～10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 1% (g/ml) NaOH, with chloroform-methanol-strong ammonia solution (volume proportion 36-44: 6-8: 0.8-1.2) be developping agent, launch, take out, dry, spray is with 0.5% (g/ml) ethanol solution of ninhydrin, it is clear to be heated to spot colour developing at 100-110 ℃, in the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
3, the thin-layer chromatography discrimination method of honokiol, magnolol, it is an amount of to get cough pill, removes sugar-coat, grinds, get powder 10g, add activated charcoal 2-4g, ethanol 40-60ml, backflow 20-40 minute, put coldly, filter, filtrate is steamed near and is done, and residue adds that water 15-25ml is warm to make dissolving, put cold, with chloroform extraction twice, each 10-20ml, combined chloroform liquid washes twice again with water, each 10-20ml, chloroform solution is evaporate to dryness in water-bath, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 2～5 μ l, two kinds of each 5 μ l of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, open up to 3-4cm with chloroform-benzene-ethyl acetate (volume proportion 5: 4: 1) earlier, take out, dry, again with chloroform-ethyl acetate (volume proportion 20: 1), the ammonia vapo(u)rous is opened up down to about 8-10cm, take out, dry, put under the ultraviolet lamp (365nm) and inspect; Or spray is with 1% (g/ml) vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing in 100-110 ℃, in the test sample chromatogram with two kinds of corresponding positions of reference substance chromatogram on, show the spot of same color;
4, the thin-layer chromatography discrimination method of dried orange peel: get dried orange peel control medicinal material 0.5g, with ether-absolute ethyl alcohol (volume proportion 8: 2) mixed liquor 15-25ml, close plug, jolting constantly, placement is spent the night, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, in contrast medicinal material solution, test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw to differentiate 2 need testing solution and above-mentioned control medicinal material solution 2～5 μ l respectively down, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate (volume proportion 2-3: 2-4) be developping agent, launch, take out, dry, under ultraviolet lamp (365nm), inspect, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
5, the thin-layer chromatography qualitative identification method of Fructus Aurantii: get Fructus Aurantii control medicinal material 0.5g, (volume proportion 8: 2) mixed liquor 15-25ml adds diethyl ether-absolute ethyl alcohol, close plug, jolting constantly, placement is spent the night, filter, the filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, medicinal material solution according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, is drawn need testing solution and each 5 μ l of above-mentioned control medicinal material solution under above-mentioned 2 in contrast, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (volume proportion 6-7: 3-4: 0.4-0.6) be developping agent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing in 100-110 ℃, puts under the ultraviolet lamp (365nm) and inspects, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
6, Determination of Ephedrine Hydrochloride assay method in the cough pill, measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia D):
1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; Methanol-water (volume proportion 1: 1) is a moving phase; The detection wavelength is 254 ± 2nm, and number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000;
2) preparation of reference substance solution: precision takes by weighing ephedrine hydrochloride reference substance 12.5mg, put in the 100ml measuring bottle, the water dissolving also is diluted to scale, shake up, precision is measured 15ml, puts in the 100ml measuring bottle, be diluted with water to scale, shake up, precision is measured 10ml, puts in the 25ml measuring bottle, add periodic acid solution (0.25g → 10ml) (refer to that the 0.25g periodic acid adds water and makes into 10ml solution) 1ml, 0.25mol/L sodium hydroxide solution 2.5ml shakes up, and places 30 minutes, regulate PH to neutral with the 0.5mol/L hydrochloric acid solution, add methyl alcohol to scale, shake up, promptly get (hydrochloric ephedrine 7.5 μ g among every 1ml);
3) preparation of need testing solution: it is an amount of to get cough pill, removes sugar-coat, gets 50 balls, porphyrize, put in the round-bottomed flask of 500ml, add sodium chloride 7.5g, add defoamer 1g again, add 5mol/L sodium hydroxide solution 120ml, shake diffusingly, sonicated 10 minutes is shaken diffusing again, distillation, collect the nearly 95ml of distillate with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance, add water to scale, shake up, precision is measured 10ml, put in the 25ml measuring bottle, add periodic acid solution (0.25g → 10ml) (refer to that the 0.25g periodic acid adds water and makes into 10ml solution) 1ml, 0.25mol/L sodium hydroxide solution 2.5ml, shake up, placed 30 minutes, and regulated PH to neutral, add methyl alcohol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
4) determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, that is, the every ball of this product contains Chinese ephedra with ephedrine hydrochloride (C
10H
15NOHCI) meter must not be less than 25 μ g.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution.
The quality determining method of cough pill of the present invention, improved the quality control standard of cough pill, the assay of setting up main ingredient in the preparation detects index and detection method thereof, having deleted the physical and chemical reaction of specificity difference differentiates, increase the thin-layer chromatography qualitative identification method of ephedrine hydrochloride, honokiol, magnolol and dried orange peel, Fructus Aurantii, guaranteed cough pill compound preparation higher quality standard level.
Embodiment
Embodiment:
The pharmaceutical formulation of cough pill is: Chinese ephedra 20g, perilla seed 40g, the bark of official magnolia (ginger is processed) 50g, lepidium seed 20g, Bulbus Fritillariae Cirrhosae 4g, rhizoma pinellinae praeparata (sand stir-fry) 20g, gingko 18g, pappy shell 50g, borax 6g, Fructus Aurantii (bran stir-fry) 40g, dried orange peel 70g, balloonflower root 30g, windproof 40g, Poria cocos 70g, Cynanchum glaucescens 20g, root of purple-flowered peucedanum 30g, Radix Glycyrrhizae 40g, mulberry leaf 50g, the root of large-flowered skullcap (wine is processed) 10g, adenophora tetraphylla 60g, peppermint 50g, perilla leaf 40g.Method for making: above 22 flavors, with mulberry leaf, pappy shell, Radix Glycyrrhizae boiling secondary, each 2 hours, collecting decoction filtered, and filtrate is concentrated in right amount, adds the borax dissolving; 18 flavors such as all the other Bulbus Fritillariae Cirrhosaes are ground into fine powder, sieve, and mixing, with the general ball of above-mentioned concentrated medicament, drying, sugar coating, promptly.Proterties: this product is the sugar-coat condensed pill, removes to show tawny behind the sugar-coat; Bitter, little puckery.
The quality determining method of cough pill of the present invention is:
1, get cough pill and put the microscopically observation: the dendritic agglomerate of irregular branch is colourless, meets chloral hydrate liquid and dissolves; Hyphae colorless or light brown, diameter 4～6 μ m; Grease chamber's fragment contains the volatilization oil droplet, and is faint yellow, and secretory cell includes the yellowish-brown thing; The corner place of part similar round or elliptical erythrocyte often thickens; Connect latex dust and include small faint yellow granular substance.The fiber bunchy, faint yellow, bast fiber is more rare, fusiformis, wall thickness; The conduit scalariform, reticulate pattern is more sees that bordered pit is rare, and test-tube baby is tiny.Needle-like calcium oxalate crystal is dispersed in more, prismatic crystal multiaspect shape.Nonglandular hair is often broken, and one to several cells compositions.Amylum body similar round, oval, omphalion slit-like, starlike, point-like and herringbone shape;
2, the thin-layer chromatography qualitative identification method of ephedrine hydrochloride: it is an amount of to get cough pill, remove sugar-coat, grind, get powder 20g, (volume proportion 8: 2) the mixed liquor 80ml that adds diethyl ether-absolute ethyl alcohol adds strong ammonia solution 2ml again, close plug, jolting constantly, placement is spent the night, and filters, residue washs at twice with ether 15ml, washing lotion and filtrate merge, and add ethanol solution hydrochloride (1 → 20) (referring to that 1ml hydrochloric acid adds ethanol and makes into 20ml solution) 2ml, shake up, in water-bath, steam near and do, residue adds methyl alcohol 2ml and stirs and to make moltenly, and with a little absorbent cotton filtration, filtrate is as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned need testing solution 5～10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 1% (g/ml) NaOH, with chloroform-methanol-strong ammonia solution (volume proportion 40: 7: 1) is developping agent, launch, take out, dry, spray is with 0.5% (g/ml) ethanol solution of ninhydrin, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
3, the thin-layer chromatography qualitative identification method of magnolol: it is an amount of to get cough pill, removes sugar-coat, grinds, and gets powder 10g, add activated charcoal 3g, ethanol 50ml refluxed 30 minutes, put cold, filter, filtrate is steamed near and is done, and residue adds that water 20ml is warm to make dissolving, put cold, with chloroform extraction twice, each 15ml, combined chloroform liquid washes twice again with water, each 15ml, chloroform solution is evaporate to dryness in water-bath, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 2～5 μ l, two kinds of each 5 μ l of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, open up to 3cm with chloroform-benzene-ethyl acetate (volume proportion 5: 4: 1) earlier, take out, dry, again with chloroform-ethyl acetate (volume proportion 20: 1), the ammonia vapo(u)rous is opened up down to about 9cm, take out, dry, put under the ultraviolet lamp (365nm) and inspect; Or spray is with 1% (g/ml) vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing in 100 ℃, in the test sample chromatogram with two kinds of corresponding positions of reference substance chromatogram on, show the spot of same color;
4, the thin-layer chromatography qualitative identification method of dried orange peel: get dried orange peel control medicinal material 0.5g, with ether-absolute ethyl alcohol (volume proportion 8: 2) mixed liquor 20ml, close plug, jolting constantly, placement is spent the night, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, in contrast medicinal material solution, test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2～5 μ l of need testing solution under above-mentioned 2 and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, be developping agent with normal hexane-ethyl acetate (volume proportion 2: 3), launch, take out, dry, under ultraviolet lamp (365nm), inspect, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
5, the thin-layer chromatography qualitative identification method of Fructus Aurantii: get Fructus Aurantii control medicinal material 0.5g, (volume proportion 8: 2) mixed liquor 20ml adds diethyl ether-absolute ethyl alcohol, close plug, jolting constantly, placement is spent the night, filter, the filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, medicinal material solution according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, is drawn need testing solution and each 5 μ l of above-mentioned control medicinal material solution under differentiating 2 in contrast, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (volume proportion 6.5: 3.5: 0.5) is developping agent, launches, and takes out, dry, spray is with the ethanol solution of sulfuric acid of 10% (g/ml), and it is clear to be heated to the spot colour developing in 105 ℃, puts under the ultraviolet lamp (365nm) and inspects, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
6, the content assaying method of the hydrochloric ephedrine of cough pill, measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia D):
1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; Methanol-water (volume proportion 1: 1) is a moving phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000.
2) preparation of reference substance solution: precision takes by weighing ephedrine hydrochloride reference substance 12.5mg, put in the 100ml measuring bottle, the water dissolving also is diluted to scale, shake up, precision is measured 15ml, puts in the 100ml measuring bottle, be diluted with water to scale, shake up, precision is measured 10ml, puts in the 25ml measuring bottle, add periodic acid solution (0.25g → 10ml) (refer to that the 0.25g periodic acid adds water and makes into 10ml solution) 1ml, 0.25mol/L sodium hydroxide solution 2.5ml shakes up, and places 30 minutes, regulate PH to neutral with the 0.5mol/L hydrochloric acid solution, add methyl alcohol to scale, shake up, promptly get (hydrochloric ephedrine 7.5 μ g among every 1ml);
3) preparation of need testing solution: it is an amount of to get cough pill, remove sugar-coat, get 50 balls, porphyrize is put in the round-bottomed flask of 500ml, add sodium chloride 7.5g, (steep king-edible defoaming agent second generation extremely, Wujin, Jiangsu Province city river Fine Chemical Works is made, standard code: Q/320482XJH001-1999) to add defoamer 1g again, add 5mol/L sodium hydroxide solution 120ml, shake diffusingly, sonicated 10 minutes is shaken diffusing again, distillation, collect the nearly 95ml of distillate with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance, add water to scale, shake up, precision is measured 10ml, put in the 25ml measuring bottle, add periodic acid solution (0.25g → 10ml) (refer to that the 0.25g periodic acid adds water and makes into 10ml solution) 1ml, 0.25mol/L sodium hydroxide solution 2.5ml, shake up, placed 30 minutes, and regulated PH to neutral, add methyl alcohol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
4) determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, that is, the every ball of this product contains Chinese ephedra with ephedrine hydrochloride (C
10H
15NOHCI) meter must not be less than 25 μ g.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution.
The quality control standard of the cough pill after the improvement is as follows:
The cough pill drug standards
Cough pill
zhike?Wan
[prescription] Chinese ephedra 20g, perilla seed 40g, the bark of official magnolia (ginger is processed) 50g, lepidium seed 20g, Bulbus Fritillariae Cirrhosae 4g, rhizoma pinellinae praeparata (sand stir-fry) 20g, gingko 18g, pappy shell 50g, borax 6g, Fructus Aurantii (bran stir-fry) 40g, dried orange peel 70g, balloonflower root 30g, windproof 40g, Poria cocos 70g, Cynanchum glaucescens 20g, root of purple-flowered peucedanum 30g, Radix Glycyrrhizae 40g, mulberry leaf 50g, the root of large-flowered skullcap (wine is processed) 10g, adenophora tetraphylla 60g, peppermint 50g, perilla leaf 40g.
[method for making] above 22 flavors, with mulberry leaf, pappy shell, Radix Glycyrrhizae boiling secondary, each 2 hours, collecting decoction filtered, and filtrate is concentrated in right amount, adds the borax dissolving; 18 flavors such as all the other Bulbus Fritillariae Cirrhosaes are ground into fine powder, sieve, and mixing, with the general ball of above-mentioned concentrated medicament, drying, sugar coating, promptly.
[proterties] this product is the sugar-coat condensed pill, removes to show tawny behind the sugar-coat; Bitter, little puckery.
This product is got in [discriminating] (1), and put microscopically and observe: the dendritic agglomerate of irregular branch is colourless, meets chloral hydrate liquid and dissolves; Hyphae colorless or light brown, diameter 4～6 μ m.Grease chamber's fragment contains the volatilization oil droplet, and is faint yellow, and secretory cell includes the yellowish-brown thing.The corner place of part similar round or elliptical erythrocyte often thickens.Connect latex dust and include small faint yellow granular substance.The fiber bunchy, faint yellow, bast fiber is more rare, fusiformis, wall thickness.The conduit scalariform, reticulate pattern is more sees that bordered pit is rare, and test-tube baby is tiny.Needle-like calcium oxalate crystal is dispersed in more, prismatic crystal multiaspect shape.Nonglandular hair is often broken, and one to several cells compositions.Amylum body similar round, oval, omphalion slit-like, starlike, point-like and herringbone shape.
(2) it is an amount of to get this product, removes sugar-coat, grinds.Get powder 20g, (8: 2) the mixed liquor 80ml that adds diethyl ether-absolute ethyl alcohol adds strong ammonia solution 2ml again, close plug, jolting constantly, placement is spent the night, filter, residue washs at twice with ether 15ml, and washing lotion and filtrate merge, add ethanol solution hydrochloride (1 → 20) 2ml, shake up, steam in water-bath near and do, residue adds methyl alcohol 2ml stirring to be made molten, filter with a little absorbent cotton, filtrate is as need testing solution.Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned need testing solution 5～10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 1% NaOH, be developping agent with chloroform-methanol-strong ammonia solution (40: 7: 1), launch, take out, dry, spray is with 0.5% ethanol solution of ninhydrin, and it is clear to be heated to spot colour developing at 105 ℃.In the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) it is an amount of to get this product, removes sugar-coat, grinds.Get powder 10g, add activated charcoal 3g, ethanol 50ml refluxed 30 minutes, put cold, filter, filtrate is steamed near and is done, and residue adds that water 20ml is warm to make dissolving, put cold, with twice of chloroform extraction, each 15ml, combined chloroform liquid washes twice again with water, each 15ml, chloroform solution is evaporate to dryness in water-bath.Residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets magnolol and honokiol reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 2～5 μ l, two kinds of each 5 μ l of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, open up to 3cm with chloroform-benzene-ethyl acetate (5: 4: 1) earlier, take out, dry, again with chloroform-ethyl acetate (20: 1), the ammonia vapo(u)rous is opened up down to about 9cm, take out, dry, put under the ultraviolet lamp (365nm) and inspect; Or spray is with 1% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing in 100 ℃.In the test sample chromatogram with two kinds of corresponding positions of reference substance chromatogram on, show the spot of same color.
(4) get dried orange peel control medicinal material 0.5g, with ether-absolute ethyl alcohol (8: 2) mixed liquor 20ml, close plug, jolting constantly, placement is spent the night, and filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution and each 2～5 μ l of above-mentioned control medicinal material solution of differentiating under (2) item, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate (2: 3) is developping agent, open up to 9cm, take out, dry, under ultraviolet lamp (365nm), inspect.In the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color.
(5) get Fructus Aurantii control medicinal material 0.5g, (8: 2) the mixed liquor 20ml that adds diethyl ether-absolute ethyl alcohol, close plug, jolting constantly, placement is spent the night, and filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution and each 5 μ l of above-mentioned control medicinal material solution of differentiating under (2) item, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (6.5: 3.5: 0.5) is developping agent, and exhibition is taken out to about 9cm, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing in 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color.
[inspection] should meet every regulation relevant under the pill item (an appendix I of Chinese Pharmacopoeia version in 2005 A).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; Methanol-water (1: 1) is a moving phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000.
The preparation precision of reference substance solution takes by weighing ephedrine hydrochloride reference substance 12.5mg, put in the 100ml measuring bottle, the water dissolving also is diluted to scale, shake up, precision is measured 15ml, puts in the 100ml measuring bottle, be diluted with water to scale, shake up, precision is measured 10ml, puts in the 25ml measuring bottle, add the periodic acid solution (1ml of 0.25g → 10ml), 0.25mol/L sodium hydroxide solution 2.5ml shakes up, and places 30 minutes, regulate PH to neutral with the 0.5mol/L hydrochloric acid solution, add methyl alcohol to scale, shake up, promptly get (hydrochloric ephedrine 7.5 μ g among every 1ml).
It is an amount of that this product is got in the preparation of need testing solution, removes sugar-coat, gets 50 balls, porphyrize.Put in the round-bottomed flask of 500ml, add sodium chloride 7.5g, add defoamer 1g again, add 5mol/L sodium hydroxide solution 120ml, shake diffusing, sonicated 10 minutes, shake diffusingly again, distillation is collected the nearly 95ml of distillate with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance, add water to scale, shake up.Precision is measured 10ml, puts in the 25ml measuring bottle, and according to the method under the reference substance solution preparation, from " adding periodic acid solution ", operation in accordance with the law, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
The every ball of this product contains Chinese ephedra with ephedrine hydrochloride (C
10H
15NOHCI) meter must not be less than 25 μ g.
[function cures mainly] lowering the adverse-rising QI to resolve phlegm, relieving cough and relieving asthma.Be used for chill and go into lung, the coughing with a lot of sputum that Lung Qi obstruction causes, syndrome characterized by dyspnea is uncomfortable in chest, and malasia or chronic cough are more than, and old acute/chronic bronchitis.
[usage and dosage] is oral, one time 6 ball, 2 times on the one.
The heavy 3g of [specification] per 18 balls.
[storage] sealing.
Claims (1)
1. the quality determining method of a cough pill, the pharmaceutical formulation of cough pill is: Chinese ephedra 20g, perilla seed 40g, ginger is processed bark of official magnolia 50g, lepidium seed 20g, Bulbus Fritillariae Cirrhosae 4g, boiling-on-grain tuber of pinellia 20g, gingko 18g, pappy shell 50g, borax 6g, stir-baked FRUCTUS AURANTII in bran 40g, dried orange peel 70g, balloonflower root 30g, windproof 40g, Poria cocos 70g, Cynanchum glaucescens 20g, root of purple-flowered peucedanum 30g, Radix Glycyrrhizae 40g, mulberry leaf 50g, wine process root of large-flowered skullcap 10g, adenophora tetraphylla 60g, peppermint 50g, perilla leaf 40g; The quality determining method that it is characterized in that cough pill is:
1) get cough pill and put the microscopically observation: the dendritic agglomerate of irregular branch is colourless, meets chloral hydrate liquid and dissolves; Hyphae colorless or light brown, diameter 4～6 μ m; Grease chamber's fragment contains the volatilization oil droplet, and is faint yellow, and secretory cell includes the yellowish-brown thing, and the corner place of part similar round or elliptical erythrocyte often thickens, and connect latex dust and include small faint yellow granular substance, the fiber bunchy, faint yellow, bast fiber is more rare, fusiformis, wall thickness; The conduit scalariform, reticulate pattern is more sees that bordered pit is rare, and test-tube baby is tiny, and needle-like calcium oxalate crystal is dispersed in more, prismatic crystal multiaspect shape, and nonglandular hair is often broken, and one forms to several cells, amylum body similar round, oval, omphalion slit-like, starlike, point-like and herringbone shape;
2) the thin-layer chromatography discrimination method of ephedrine hydrochloride: it is an amount of to get cough pill, remove sugar-coat, grind, get powder 20g, add diethyl ether-absolute ethyl alcohol 8: 2 mixed liquor 70-90ml of proportioning by volume, add strong ammonia solution 2-3ml again, close plug, jolting constantly, placement is spent the night, and filters, residue washs at twice with ether 10-20ml, washing lotion and filtrate merge, and add ethanol solution hydrochloride 1 → 20 and refer to that promptly 1ml hydrochloric acid adds ethanol and makes into 20ml solution 2-3ml, shake up, in water-bath, steam near and do, residue adds methyl alcohol 2ml and stirs and to make moltenly, and with a little absorbent cotton filtration, filtrate is as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned need testing solution 5～10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 1% (g/ml) NaOH, with chloroform-methanol-strong ammonia solution proportioning 36-44: 6-8 by volume: 0.8-1.2 is as developping agent, launch, take out, dry, spray is with 0.5%, the g/ml ethanol solution of ninhydrin, and it is clear to be heated to the spot colour developing at 100-110 ℃, in the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
3) the thin-layer chromatography discrimination method of honokiol, magnolol: it is an amount of to get cough pill, removes sugar-coat, grinds, and gets powder 10g, add activated charcoal 2-4g, ethanol 40-60ml backflow 20-40 minute, is put cold, filter, filtrate is steamed near and is done, and residue adds that water 15-25ml is warm to make dissolving, put cold, with chloroform extraction twice, each 10-20ml, combined chloroform liquid washes twice again with water, each 10-20ml, chloroform solution is evaporate to dryness in water-bath, and residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin-layered chromatography, draw need testing solution 2～5 μ l, two kinds of each 5 μ l of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, open up to 3-4cm with the proportioning mixing in 5: 4: 1 by volume of chloroform-benzene-ethyl acetate earlier, take out, dry, again with the proportioning mixing in 20: 1 by volume of chloroform-ethyl acetate, the ammonia vapo(u)rous is opened up down to about 8-10cm, take out, dry, put under the ultraviolet lamp and inspect; Or spray is with 1%, g/ml vanillic aldehyde sulfuric acid solution, it is clear to be heated to spot colour developing in 100-110 ℃, in the test sample chromatogram with two kinds of corresponding positions of reference substance chromatogram on, show the spot of same color;
4) the thin-layer chromatography discrimination method of dried orange peel: get dried orange peel control medicinal material 0.5g, with ether-absolute ethyl alcohol mixed liquor 15-25ml of 8: 2 of proportioning by volume, close plug, jolting constantly, placement is spent the night, filter, filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, in contrast medicinal material solution, test according to thin-layered chromatography, draw above-mentioned 2) following need testing solution and above-mentioned control medicinal material solution 2～5 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate proportioning 2-3 by volume: 2-4 is as developping agent, launch, take out, dry, under ultraviolet lamp, inspect, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
5) the thin-layer chromatography qualitative identification method of Fructus Aurantii: get Fructus Aurantii control medicinal material 0.5g, add diethyl ether-absolute ethyl alcohol 8: 2 mixed liquor 15-25ml of proportioning by volume, close plug, jolting constantly, placement is spent the night, filter, the filtrate evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, and medicinal material solution is tested according to thin-layered chromatography in contrast, draw above-mentioned 2) following need testing solution and above-mentioned control medicinal material solution 5 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid by volume proportioning 6-7: 3-4: 0.4-0.6 launch as developping agent, take out, dry, spray with 10% the g/ml ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing in 100-110 ℃, put under the ultraviolet lamp and inspect, in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the fluorescence principal spot of same color;
6) Determination of Ephedrine Hydrochloride assay method in the cough pill, shine high effective liquid chromatography for measuring:
(1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; Methanol-water by volume proportioning the detection wavelength was 254 ± 2nm as moving phase in 1: 1
(2) preparation of reference substance solution: precision takes by weighing ephedrine hydrochloride reference substance 12.5mg, put in the 100ml measuring bottle, the water dissolving also is diluted to scale, shake up, precision is measured 15ml, puts in the 100ml measuring bottle, be diluted with water to scale, shake up, precision is measured 10ml, puts in the 25ml measuring bottle, add periodic acid solution 0.25g → 10ml and refer to that promptly the 0.25g periodic acid adds water and makes into 10ml solution 1ml, 0.25mol/L sodium hydroxide solution 2.5ml shakes up, and places 30 minutes, regulate PH to neutral with the 0.5mol/L hydrochloric acid solution, add methyl alcohol to scale, shake up, promptly;
(3) preparation of need testing solution: it is an amount of to get cough pill, removes sugar-coat, gets 50 balls, porphyrize, put in the round-bottomed flask of 500ml, add sodium chloride 7.5g, add defoamer 1g again, add 5mol/L sodium hydroxide solution 120ml, shake diffusingly, sonicated 10 minutes is shaken diffusing again, distillation, collect the nearly 95ml of distillate with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance, add water to scale, shake up, precision is measured 10ml, put in the 25ml measuring bottle, add periodic acid solution 0.25g → 10ml and refer to that promptly the 0.25g periodic acid adds water and makes into 10ml solution 1ml, 0.25mol/L sodium hydroxide solution 2.5ml, shake up, placed 30 minutes, and regulated PH to neutral, add methyl alcohol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
(4) determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, that is, the every ball of this product contains Chinese ephedra in ephedrine hydrochloride, must not be less than 25 μ g;
Wherein, contain the some grams of solute among the every 100ml of " %, g/ml " expression solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101021539A CN101732553B (en) | 2010-01-28 | 2010-01-28 | Quality inspection method of cough pills |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101021539A CN101732553B (en) | 2010-01-28 | 2010-01-28 | Quality inspection method of cough pills |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101732553A CN101732553A (en) | 2010-06-16 |
| CN101732553B true CN101732553B (en) | 2011-08-17 |
Family
ID=42456921
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101021539A Active CN101732553B (en) | 2010-01-28 | 2010-01-28 | Quality inspection method of cough pills |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101732553B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278582B (en) * | 2013-06-08 | 2014-12-10 | 广西盈康药业有限责任公司 | Method for detecting quality of ephedrine hydrochloride in three-ingredient traditional Chinese medicinal preparation containing Herbal Ephedrae |
| CN105954086A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting ephedrine hydrochloride in lung regulating pill |
| CN110376326B (en) * | 2019-07-25 | 2021-05-28 | 河北中医学院 | Multi-region thin layer identification and distinguishing method for pericarpium citri reticulatae and immature bitter orange medicinal materials |
| CN112067738A (en) * | 2020-08-19 | 2020-12-11 | 广东一方制药有限公司 | Method for identifying dampness-resolving toxin-vanquishing composition |
-
2010
- 2010-01-28 CN CN2010101021539A patent/CN101732553B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 中华人民共和国卫生部药典委员会.止咳丸.《中华人民共和国卫生部药品标准中药成方制剂第十一册》.1996,29. * |
| 范之枫等.HPLC法测定止咳丸中盐酸麻黄碱的含量.《解放军药学学报》.2005,第21卷(第5期),381-382. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101732553A (en) | 2010-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102048941B (en) | Quality control method of children-welfare tablets serving as Chinese medicinal preparation | |
| CN102038897A (en) | Quality control method of traditional Chinese medical preparation | |
| CN102688431A (en) | Kidney-reinforcing oral liquid and preparation method thereof | |
| CN102028859B (en) | Detection method for Chinese medicinal preparation for treating asthma | |
| CN101732463B (en) | Quality detection method for Jinhuaxiaocuo pills | |
| CN102749401B (en) | Inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation | |
| CN101732553B (en) | Quality inspection method of cough pills | |
| CN100543469C (en) | The detection method of tonic semifluid extract of ten ingredients | |
| CN102038908B (en) | Detection method of tambac depression-alleviating pill as traditional Chinese medical preparation | |
| CN102091168A (en) | Quality control method for Chinese medicine preparation Xuefuzhuyu capsule | |
| CN102068600A (en) | Quality control method of venation relaxing and heart-nourishing pill as Chinese herbal preparation | |
| CN105301168B (en) | The detection method of dredging collateral resolving sputum capsule | |
| CN102579734A (en) | Traditional Chinese medicine composition of bone healing medicine, preparing method thereof and detecting method thereof | |
| CN101890087A (en) | Composition containing coptis root, rhubarb and baikal skullcap root | |
| CN102068649B (en) | Quality control method for gastric condition-regulating pill as traditional Chinese preparation | |
| CN101773560A (en) | Method for testing quality of Nguyen supernatant pills | |
| CN101732552B (en) | Method for detecting quality of lung clearing and phlegm eliminating pill | |
| CN102038785B (en) | Detection method for traditional Chinese medicinal preparation of children eyesight pills | |
| CN102038789B (en) | Detection method of Chinese herbal preparation-cannabis fruit spleen-enriching pill for treating constipation | |
| CN102048864B (en) | Detection method of children lung clearing pills of Chinese medicinal preparation | |
| CN102078474B (en) | Nano-dispersible tablet for four-season common cold and preparation method thereof | |
| CN101732527A (en) | Quality detection method for liver-soothing granules | |
| CN102038869B (en) | Quality control method of traditional Chinese medical preparation | |
| CN100515476C (en) | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method | |
| CN102028839B (en) | Quality control method of Chinese medicinal preparation for regulating menstruation in Department of Obstetrics and Gynecology |
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 | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Quality inspection method of cough pills Effective date of registration: 20140609 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming Dianchi road subbranch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2014990000447 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20160426 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming Dianchi road subbranch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2014990000447 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Quality inspection method of cough pills Effective date of registration: 20160426 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2016990000339 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20170519 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2016990000339 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Quality inspection method of cough pills Effective date of registration: 20170519 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2017990000427 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20190716 Granted publication date: 20110817 Pledgee: China Merchants Bank, Limited by Share Ltd, Kunming branch Pledgor: Kunming Chinese Medicine Factory Co., Ltd. Registration number: 2017990000427 |