CN101732553A - Quality inspection method of cough pills - Google Patents
Quality inspection method of cough pills Download PDFInfo
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- CN101732553A CN101732553A CN201010102153A CN201010102153A CN101732553A CN 101732553 A CN101732553 A CN 101732553A CN 201010102153 A CN201010102153 A CN 201010102153A CN 201010102153 A CN201010102153 A CN 201010102153A CN 101732553 A CN101732553 A CN 101732553A
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- 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 35
- 238000007689 inspection Methods 0.000 title abstract description 8
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 32
- 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
- 238000003908 quality control method Methods 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 81
- 238000012360 testing method Methods 0.000 claims description 64
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 22
- 229960004756 ethanol Drugs 0.000 claims description 19
- 210000000582 semen Anatomy 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
- 239000000853 adhesive Substances 0.000 claims description 16
- 230000001070 adhesive effect Effects 0.000 claims description 16
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims description 16
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 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
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 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
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- 239000012567 medical material Substances 0.000 claims description 8
- BYTORXDZJWWIKR-UHFFFAOYSA-N Hinokiol Natural products CC(C)c1cc2CCC3C(C)(CO)C(O)CCC3(C)c2cc1O BYTORXDZJWWIKR-UHFFFAOYSA-N 0.000 claims description 7
- 241001619461 Poria <basidiomycete fungus> 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
- 235000011201 Ginkgo Nutrition 0.000 claims description 6
- 235000008100 Ginkgo biloba Nutrition 0.000 claims description 6
- 238000012850 discrimination method Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
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- 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
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- 239000004816 latex Substances 0.000 claims description 4
- 229920000126 latex Polymers 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
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 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
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 4
- 235000012141 vanillin Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 241000218628 Ginkgo Species 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
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- 229940079593 drug Drugs 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000005180 public health Effects 0.000 abstract description 5
- 244000183685 Citrus aurantium Species 0.000 abstract description 4
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- 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
- 230000000694 effects Effects 0.000 description 23
- 206010062717 Increased upper airway secretion Diseases 0.000 description 12
- 208000026435 phlegm Diseases 0.000 description 12
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 description 8
- 210000004072 lung Anatomy 0.000 description 8
- 244000194101 Ginkgo biloba Species 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 208000006673 asthma Diseases 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
- 229960002179 ephedrine Drugs 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 241001673966 Magnolia officinalis Species 0.000 description 3
- 239000003172 expectorant agent Substances 0.000 description 3
- 230000003419 expectorant effect Effects 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 244000052769 pathogen Species 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
- 241001278898 Glycyrrhiza inflata Species 0.000 description 2
- 208000008454 Hyperhidrosis Diseases 0.000 description 2
- 244000124853 Perilla frutescens Species 0.000 description 2
- 235000004348 Perilla frutescens Nutrition 0.000 description 2
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- 208000013116 chronic cough Diseases 0.000 description 2
- 208000013219 diaphoresis Diseases 0.000 description 2
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- 241000125183 Crithmum maritimum Species 0.000 description 1
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- 206010012735 Diarrhoea Diseases 0.000 description 1
- 241000723281 Ephedra equisetina Species 0.000 description 1
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- 208000010201 Exanthema Diseases 0.000 description 1
- 241000628997 Flos 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
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- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
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- 244000211187 Lepidium sativum Species 0.000 description 1
- 235000007849 Lepidium sativum Nutrition 0.000 description 1
- 244000280293 Mentha haplocalyx Species 0.000 description 1
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- 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 wind and cold and goes into lung, the cough with copious phlegm that inhibited pulmonary QI causes, dyspnea with rapid and short breath 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 Herba Ephedrae 20g, Fructus Perillae 40g, Cortex Magnoliae Officinalis (Rhizoma Zingiberis Recens is processed) 50g, Semen Lepidii (Semen Descurainiae) 20g, Bulbus Fritillariae Cirrhosae 4g, Rhizoma Pinelliae Preparatum (stir-baking with sand) 20g, Semen Ginkgo 18g, Pericarpium Papaveris 50g, Borax 6g, Fructus Aurantii (parched with bran) 40g, Pericarpium Citri Reticulatae 70g, Radix Platycodonis 30g, Radix Saposhnikoviae 40g, Poria 70g, Rhizoma Cynanchi Stauntonii 20g, Radix Peucedani 30g, Radix Glycyrrhizae 40g, Folium Mori 50g, Radix Scutellariae (wine is processed) 10g, Radix Adenophorae 60g, Herba Menthae 50g, Folium Perillae 40g.Principal agent in the Herba Ephedrae side of being, Herba Ephedrae is the dry herb stem of Ephedraceae plant plait Herba Ephedrae Ephedra sinica Stapf, epheday intermedia Ephedra intermedia Schrenk et C.A.Mey. or ephedra equisetina Ephedra equisetina Bge., tool diaphoresis cold expelling, the effect of depressed lung-energy dispersing; Fructus Perillae is the dry mature fruit of labiate Folium Perillae Perilla frutescens (L.) Britt., has the sending down the abnormal ascending QI expectorant, relievings asthma the effect of intestine moistening; Cortex Magnoliae Officinalis is dry dried bark, root bark and the branch skin of Magnoliacea plant Cortex Magnoliae Officinalis Magnoliaofficinalis Rehd.et Wils. or magnolia officinalis rehd.et wils.var.biloba rehd.et wils. Magnolia officinalis Rehd.et Wils.var.biloba Rebd.et Wils., has the effect of dampness expectorant; Semen Lepidii (Semen Descurainiae) is the dry mature seed of crucifer Lepidium sativum L. Lepidiumapetalum Willd. or descurainia sophia (l.) webb ex prantl Descurainia Sophia (L.) Webb ex Prantl, has eliminating pathogen from the lung for 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 Bulbus Fritillariae Uninbracteatae Fritillaria unibracteata Hsiao et K.C.Hsia, Gansu Bulbus Fritillariae Uninbracteatae 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 Pinelliae Preparatum is the process of preparing Chinese medicine processed goods (Rhizoma Pinelliae is the dry tuber of aroid Rhizoma Pinelliae Pinellia ternata (Thunb.) Breit.) of the Rhizoma Pinelliae, has the effect of drying dampness to eliminate phlegm; Semen Ginkgo is the dry mature seed of Ginkgoaceae plant Ginkgo biloba Ginkgo biloba L., has the effect of astringing lung QI for relieving asthma; Pericarpium Papaveris is the drying and ripening shell of bloodroot Semen Papaveris Papaver somniferum L., has and astringes the lung, astringing intestine to stop diarrhea, the effect of pain relieving; Borax is a sodium tetraborate, contains Na
2B
4O
710H
2O should be 99.0～105.0%, the effect of tool heat-clearing and toxic substances removing, removing heat from the lung and dissipating phlegm; Fructus Aurantii is the dry immature fruit of rutaceae Citrus aurantium Linn. Citrus aurantium L. and variety thereof, tool regulating the flow of QI to ease the stomach, the effect of the stagnant relieving distension of row; Pericarpium Citri Reticulatae is the dry mature skin of rutaceae orange Citrus reticulate Blanco and variety thereof, has regulating qi-flowing for strengthening spleen, the effect of drying dampness to eliminate phlegm; Radix Platycodonis is the dry root of campanulaceae Platycodon grandiflouorum Platycodongrandiflorum (Jacq.) A.DC., has lung qi dispersing, and sore-throat relieving eliminates the phlegm, the effect of evacuation of pus; Radix Saposhnikoviae is the dry root of umbelliferae Saposhnikovia divaricata Saposhnikovia divaricata (Turcz.) Schischk., the effect of tool inducing diaphoresis to dispel wind; Poria is the dry sclerotia of Polyporaceae fungus Poria Poria cocos (Schw.) Wolf, has promoting diuresis to eliminate damp pathogen, the effect of spleen invigorating mind calming; Rhizoma Cynanchi Stauntonii is dry rhizome and the root of asclepiadaceae plant rhizoma et radix cynanchi stauntoni Cynanchum stauntonii (Dec-ne.) Schltr.ex Levl. or Flos Genkwa leaf Rhizoma Cynanchi Stauntonii Cynanchum glaucescens (Dcene.) Hand.-Mazz., have sending down the abnormal ascending QI, expectorant, the effect of cough-relieving; Radix Peucedani is the dry root of samphire Peucedanum praeruptorum DUNN Peucedanum praeruptorm Dunn, has diffusing wind heat clearing away, 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 inflata Bat. Glycyrrhiza in flataBat or Glycyrrhiza glabra L. Glycyrrhiza glabra L., has invigorating the spleen and replenishing QI, heat-clearing and toxic substances removing, expelling phlegm for arresting cough, the effect of coordinating the actions of various ingredients in a prescription; Folium Mori are the dried leaves of moraceae plants Mulberry Morus alba L., have dispelling wind and heat pathogens, the effect of clearing away lung-heat and moistening for dryness; Radix Scutellariae is the dry root of labiate Radix Scutellariae Scutellaria baicalensis Georgi, has heat clearing and damp drying, the effect of eliminating fire and detoxication; Radix Adenophorae is the dry root of campanulaceae plant adenophora tetraphylla Adenophora tetraphylla (Thunb.) Fisch. or Radix Adenophorae (Radix Glehniae) Adenophora stricta Miq., has nourishing YIN and clearing away lung-heat, reduces phlegm the effect of QI invigorating; Herba Menthae is the dry aerial parts of labiate Menthahaplocalyx Briq., tool dispelling wind-heat, refresh oneself, the effect of rash; Folium Perillae is the dried leaves (or band twig) of labiate Folium Perillae Perilla frutescens (L.) Britt, has the effect of the cold expelling 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 Ministry of Public Health is issued, 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: Herba Ephedrae 20g, Fructus Perillae 40g, Cortex Magnoliae Officinalis (Rhizoma Zingiberis Recens is processed) 50g, Semen Lepidii (Semen Descurainiae) 20g, Bulbus Fritillariae Cirrhosae 4g, Rhizoma Pinelliae Preparatum (stir-baking with sand) 20g, Semen Ginkgo 18g, Pericarpium Papaveris 50g, Borax 6g, Fructus Aurantii (parched with bran) 40g, Pericarpium Citri Reticulatae 70g, Radix Platycodonis 30g, Radix Saposhnikoviae 40g, Poria 70g, Rhizoma Cynanchi Stauntonii 20g, Radix Peucedani 30g, Radix Glycyrrhizae 40g, Folium Mori 50g, Radix Scutellariae (wine is processed) 10g, Radix Adenophorae 60g, Herba Menthae 50g, Folium Perillae 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, phloem 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.Starch grain 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-dehydrated 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 liquid 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 methanol 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 methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer 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 adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide, with chloroform-methanol-strong ammonia solution (volume proportion 36-44: 6-8: 0.8-1.2) be developing solvent, launch, take out, dry, spray is with 0.5% (g/ml) ethanol solution of ninhydrin, it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle 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 active carbon 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 dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methanol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin layer 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 adhesive 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 ultra-violet lamp (365nm) and inspect; Or spray is with 1% (g/ml) vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 100-110 ℃, in the test sample chromatograph with two kinds of corresponding positions of reference substance chromatograph on, show the speckle of same color;
4, the thin layer chromatography discrimination method of Pericarpium Citri Reticulatae: get Pericarpium Citri Reticulatae control medicinal material 0.5g, with ether-dehydrated 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 methanol 1ml makes dissolving, in contrast medical material solution, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw to differentiate 1 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 adhesive with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate (volume proportion 2-3: 2-4) be developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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-dehydrated alcohol, close plug, jolting constantly, placement is spent the night, filter, the filtrate evaporate to dryness, residue adds methanol lml makes dissolving, medical material solution according to thin layer 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 1 in contrast, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (volume proportion 6-7: 3-4: 0.4-0.6) be developing solvent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 100-110 ℃, puts under the ultra-violet lamp (365nm) and inspects, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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 (appendix VID of Chinese Pharmacopoeia):
1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol-water (volume proportion 1: 1) is mobile 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, with water dissolution and be 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 methanol 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, supersound process 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 methanol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, that is, the every ball of this product contains Herba Ephedrae 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 principal agent 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 Pericarpium Citri Reticulatae, Fructus Aurantii, guaranteed cough pill compound preparation higher quality standard level.
The specific embodiment
Embodiment:
The pharmaceutical formulation of cough pill is: Herba Ephedrae 20g, Fructus Perillae 40g, Cortex Magnoliae Officinalis (Rhizoma Zingiberis Recens is processed) 50g, Semen Lepidii (Semen Descurainiae) 20g, Bulbus Fritillariae Cirrhosae 4g, Rhizoma Pinelliae Preparatum (stir-baking with sand) 20g, Semen Ginkgo 18g, Pericarpium Papaveris 50g, Borax 6g, Fructus Aurantii (parched with bran) 40g, Pericarpium Citri Reticulatae 70g, Radix Platycodonis 30g, Radix Saposhnikoviae 40g, Poria 70g, Rhizoma Cynanchi Stauntonii 20g, Radix Peucedani 30g, Radix Glycyrrhizae 40g, Folium Mori 50g, Radix Scutellariae (wine is processed) 10g, Radix Adenophorae 60g, Herba Menthae 50g, Folium Perillae 40g.Method for making: above 22 flavors, Folium Mori, Pericarpium Papaveris, Radix Glycyrrhizae are decocted with water 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.Character: this product is the sugar-coat concentrated pill, removes to show yellowish-brown behind the sugar-coat; Bitter in the mouth, 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, phloem 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.Starch grain 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-dehydrated 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 liquid 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 methanol 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 methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer 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 adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide, with chloroform-methanol-strong ammonia solution (volume proportion 40: 7: 1) is developing solvent, launch, take out, dry, spray is with 0.5% (g/ml) ethanol solution of ninhydrin, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle 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 active carbon 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 dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methanol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin layer 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 adhesive 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 ultra-violet lamp (365nm) and inspect; Or spray is with 1% (g/ml) vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 100 ℃, in the test sample chromatograph with two kinds of corresponding positions of reference substance chromatograph on, show the speckle of same color;
4, the thin layer chromatography qualitative identification method of Pericarpium Citri Reticulatae: get Pericarpium Citri Reticulatae control medicinal material 0.5g, with ether-dehydrated alcohol (volume proportion 8: 2) mixed liquor 20ml, close plug, jolting constantly, placement is spent the night, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2～5 μ l of need testing solution under above-mentioned 1 and above-mentioned control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution, be developing solvent with normal hexane-ethyl acetate (volume proportion 2: 3), launch, take out, dry, under ultra-violet lamp (365nm), inspect, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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-dehydrated alcohol, close plug, jolting constantly, placement is spent the night, filter, the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, medical material solution according to thin layer 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 1 in contrast, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (volume proportion 6.5: 3.5: 0.5) is developing solvent, 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 speckle colour developing in 105 ℃, puts under the ultra-violet lamp (365nm) and inspects, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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 (appendix VID of Chinese Pharmacopoeia):
1) chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol-water (volume proportion 1: 1) is mobile 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, with water dissolution and be 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 methanol 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 filial 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, supersound process 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 methanol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, that is, the every ball of this product contains Herba Ephedrae 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 standard
Cough pill
zhike?Wan
[prescription] Herba Ephedrae 20g, Fructus Perillae 40g, Cortex Magnoliae Officinalis (Rhizoma Zingiberis Recens is processed) 50g, Semen Lepidii (Semen Descurainiae) 20g, Bulbus Fritillariae Cirrhosae 4g, Rhizoma Pinelliae Preparatum (stir-baking with sand) 20g, Semen Ginkgo 18g, Pericarpium Papaveris 50g, Borax 6g, Fructus Aurantii (parched with bran) 40g, Pericarpium Citri Reticulatae 70g, Radix Platycodonis 30g, Radix Saposhnikoviae 40g, Poria 70g, Rhizoma Cynanchi Stauntonii 20g, Radix Peucedani 30g, Radix Glycyrrhizae 40g, Folium Mori 50g, Radix Scutellariae (wine is processed) 10g, Radix Adenophorae 60g, Herba Menthae 50g, Folium Perillae 40g.
[method for making] above 22 flavors decoct with water secondary with Folium Mori, Pericarpium Papaveris, Radix Glycyrrhizae, and 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.
[character] this product is the sugar-coat concentrated pill, removes to show yellowish-brown behind the sugar-coat; Bitter in the mouth, 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, phloem 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.Starch grain 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-dehydrated 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 liquid and filtrate merge, add ethanol solution hydrochloride (1 → 20) 2ml, shake up, steam in water-bath near and do, residue adds methanol 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 methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer 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 adhesive with the carboxymethylcellulose sodium solution that contains 1% sodium hydroxide, be developing solvent 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 speckle colour developing at 105 ℃.In the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) it is an amount of to get this product, removes sugar-coat, grinds.Get powder 10g, add active carbon 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 dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets magnolol and honokiol reference substance, adds methanol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution.Test according to thin layer 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 adhesive 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 ultra-violet lamp (365nm) and inspect; Or spray is with 1% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 100 ℃.In the test sample chromatograph with two kinds of corresponding positions of reference substance chromatograph on, show the speckle of same color.
(4) get Pericarpium Citri Reticulatae control medicinal material 0.5g, with ether-dehydrated alcohol (8: 2) mixed liquor 20ml, close plug, jolting constantly, placement is spent the night, and filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer 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 adhesive with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate (2: 3) is developing solvent, open up to 9cm, take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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-dehydrated alcohol, close plug, jolting constantly, placement is spent the night, and filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer 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 adhesive with the carboxymethylcellulose sodium solution, with toluene-ethyl acetate-formic acid (6.5: 3.5: 0.5) is developing solvent, 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 speckle colour developing in 105 ℃, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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 filler with octadecylsilane chemically bonded silica; Methanol-water (1: 1) is mobile 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, with water dissolution and be 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 methanol 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, supersound process 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 algoscopy inject chromatograph of liquid, measure, promptly.
The every ball of this product contains Herba Ephedrae 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 wind and cold and go into lung, the cough with copious phlegm that inhibited pulmonary QI causes, dyspnea with rapid and short breath 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 method for quality control of a cough pill, the pharmaceutical formulation of cough pill is: Herba Ephedrae 20g, Fructus Perillae 40g, Cortex Magnoliae Officinalis (Rhizoma Zingiberis Recens is processed) 50g, Semen Lepidii (Semen Descurainiae) 20g, Bulbus Fritillariae Cirrhosae 4g, Rhizoma Pinelliae Preparatum (stir-baking with sand) 20g, Semen Ginkgo 18g, Pericarpium Papaveris 50g, Borax 6g, Fructus Aurantii (parched with bran) 40g, Pericarpium Citri Reticulatae 70g, Radix Platycodonis 30g, Radix Saposhnikoviae 40g, Poria 70g, Rhizoma Cynanchi Stauntonii 20g, Radix Peucedani 30g, Radix Glycyrrhizae 40g, Folium Mori 50g, Radix Scutellariae (wine is processed) 10g, Radix Adenophorae 60g, Herba Menthae 50g, Folium Perillae 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, phloem 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, starch grain 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-dehydrated 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 liquid 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 methanol 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 methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer 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 adhesive with the carboxymethylcellulose sodium solution that contains 1% (g/ml) sodium hydroxide, with chloroform-methanol-strong ammonia solution proportioning 36-44: 6-8 by volume: 0.8-1.2 is as developing solvent, launch, take out, dry, spray is with 0.5% (g/ml) ethanol solution of ninhydrin, it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle 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 active carbon 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 dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets magnolol and honokiol reference substance, adds methanol respectively and makes the solution that every 1ml contains 1mg, as two kinds of reference substance solution; Test according to thin layer 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 adhesive 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 ultra-violet lamp and inspect; Or spray is with 1% (g/ml) vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing in 100-110 ℃, in the test sample chromatograph with two kinds of corresponding positions of reference substance chromatograph on, show the speckle of same color;
4) the thin layer chromatography discrimination method of Pericarpium Citri Reticulatae: get Pericarpium Citri Reticulatae control medicinal material 0.5g, with ether-dehydrated 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 methanol 1ml makes dissolving, in contrast medical material solution, test according to thin layer chromatography, draw above-mentioned 1) 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 adhesive with the carboxymethylcellulose sodium solution, with normal hexane-ethyl acetate proportioning 2-3 by volume: 2-4 is as developing solvent, launch, take out, dry, under ultra-violet lamp, inspect, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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-dehydrated 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 methanol 1ml makes dissolving, medical material solution in contrast according to the thin layer chromatography test, draws above-mentioned 1) 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 adhesive with the carboxymethylcellulose sodium solution, by volume proportioning 6-7: 3-4: 0.4-0.6 is as developing solvent with toluene-ethyl acetate-formic acid, and expansion is taken out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 100-110 ℃, puts under the ultra-violet lamp and inspects, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph 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 filler; Methanol-water by volume proportioning the detection wavelength was 254 ± 2nm as mobile 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, with water dissolution and be 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 methanol 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, supersound process 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 methanol to scale with the 0.5mol/L hydrochloric acid solution, shake up, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, that is, the every ball of this product contains Herba Ephedrae 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.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278582A (en) * | 2013-06-08 | 2013-09-04 | 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 |
| CN110376326A (en) * | 2019-07-25 | 2019-10-25 | 河北中医学院 | A kind of multizone thin layer identification differentiating method of dried orange peel and Fructus Aurantii Immaturus |
| WO2022036795A1 (en) * | 2020-08-19 | 2022-02-24 | 广东一方制药有限公司 | Method for identifying composition for dispelling dampness and detoxicating |
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2010
- 2010-01-28 CN CN2010101021539A patent/CN101732553B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278582A (en) * | 2013-06-08 | 2013-09-04 | 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 |
| 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 |
| CN110376326A (en) * | 2019-07-25 | 2019-10-25 | 河北中医学院 | A kind of multizone thin layer identification differentiating method of dried orange peel and Fructus Aurantii Immaturus |
| WO2022036795A1 (en) * | 2020-08-19 | 2022-02-24 | 广东一方制药有限公司 | Method for identifying composition for dispelling dampness and detoxicating |
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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 |
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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 |
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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 |
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