CN101773560B - Method for testing quality of Nguyen supernatant pills - Google Patents
Method for testing quality of Nguyen supernatant pills Download PDFInfo
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- CN101773560B CN101773560B CN2010101017919A CN201010101791A CN101773560B CN 101773560 B CN101773560 B CN 101773560B CN 2010101017919 A CN2010101017919 A CN 2010101017919A CN 201010101791 A CN201010101791 A CN 201010101791A CN 101773560 B CN101773560 B CN 101773560B
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- 238000012360 testing method Methods 0.000 title claims abstract description 57
- 239000006187 pill Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000006228 supernatant Substances 0.000 title abstract 5
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims abstract description 49
- 235000006226 Areca catechu Nutrition 0.000 claims abstract description 34
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 claims abstract description 21
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229940116229 borneol Drugs 0.000 claims abstract description 20
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 claims abstract description 20
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000017336 Capparis spinosa Nutrition 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 14
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 claims abstract description 10
- 229930014456 matrine Natural products 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 107
- 239000000243 solution Substances 0.000 claims description 83
- 239000013558 reference substance Substances 0.000 claims description 40
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- 235000019441 ethanol Nutrition 0.000 claims description 33
- 244000235603 Acacia catechu Species 0.000 claims description 28
- 239000000047 product Substances 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 15
- 235000005487 catechin Nutrition 0.000 claims description 15
- 229950001002 cianidanol Drugs 0.000 claims description 15
- PFTAWBLQPZVEMU-ZFWWWQNUSA-N (+)-epicatechin Natural products C1([C@@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-ZFWWWQNUSA-N 0.000 claims description 12
- PFTAWBLQPZVEMU-UKRRQHHQSA-N (-)-epicatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-UKRRQHHQSA-N 0.000 claims description 12
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000004587 chromatography analysis Methods 0.000 claims description 12
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 claims description 12
- 235000012734 epicatechin Nutrition 0.000 claims description 12
- 239000000741 silica gel Substances 0.000 claims description 12
- 229910002027 silica gel Inorganic materials 0.000 claims description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 229910021538 borax Inorganic materials 0.000 claims description 11
- 239000004328 sodium tetraborate Substances 0.000 claims description 11
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 11
- 238000012850 discrimination method Methods 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 244000246386 Mentha pulegium Species 0.000 claims description 7
- 235000016257 Mentha pulegium Nutrition 0.000 claims description 7
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 7
- 235000001050 hortel pimenta Nutrition 0.000 claims description 7
- 235000015489 Emblica officinalis Nutrition 0.000 claims description 6
- 241000219784 Sophora Species 0.000 claims description 6
- 235000011517 Terminalia chebula Nutrition 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 240000001592 Amaranthus caudatus Species 0.000 claims description 4
- 235000009328 Amaranthus caudatus Nutrition 0.000 claims description 4
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 4
- 235000012735 amaranth Nutrition 0.000 claims description 4
- 239000004178 amaranth Substances 0.000 claims description 4
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Substances OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001802 infusion Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000011003 system suitability test Methods 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 239000000341 volatile oil Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 244000140995 Capparis spinosa Species 0.000 claims 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 244000277583 Terminalia catappa Species 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 239000003208 petroleum Substances 0.000 claims 1
- 241000722721 Capparis Species 0.000 abstract description 14
- 239000003814 drug Substances 0.000 abstract description 9
- 229940079593 drug Drugs 0.000 abstract description 7
- 238000003908 quality control method Methods 0.000 abstract description 7
- 230000005180 public health Effects 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000009472 formulation Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 241000873224 Capparaceae Species 0.000 abstract description 2
- 244000080767 Areca catechu Species 0.000 abstract 6
- 238000005259 measurement Methods 0.000 abstract 1
- 238000000691 measurement method Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 10
- 241000001522 Terminalia chebula Species 0.000 description 7
- 210000001124 body fluid Anatomy 0.000 description 5
- 239000010839 body fluid Substances 0.000 description 5
- 235000013372 meat Nutrition 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 206010068319 Oropharyngeal pain Diseases 0.000 description 3
- 201000007100 Pharyngitis Diseases 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 235000021374 legumes Nutrition 0.000 description 3
- 210000004072 lung Anatomy 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000035922 thirst Effects 0.000 description 3
- 241000202807 Glycyrrhiza Species 0.000 description 2
- 241000123725 Sophora tonkinensis Species 0.000 description 2
- 206010042135 Stomatitis necrotising Diseases 0.000 description 2
- 206010000269 abscess Diseases 0.000 description 2
- 208000002399 aphthous stomatitis Diseases 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 210000000936 intestine Anatomy 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
- 238000002156 mixing Methods 0.000 description 2
- 201000008585 noma Diseases 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000006020 Acacia catechu Nutrition 0.000 description 1
- 240000007124 Brassica oleracea Species 0.000 description 1
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 description 1
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- 241000722718 Capparis masaikai Species 0.000 description 1
- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 235000001878 Mentha haplocalyx Nutrition 0.000 description 1
- 244000280293 Mentha haplocalyx Species 0.000 description 1
- 244000018795 Prunus mume Species 0.000 description 1
- 241000381592 Senegalia polyacantha Species 0.000 description 1
- 241000238370 Sepia Species 0.000 description 1
- 241000566916 Tomentella Species 0.000 description 1
- 235000009508 confectionery Nutrition 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
- 239000000284 extract Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000001114 myogenic effect Effects 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
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- 210000000952 spleen Anatomy 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to a method for testing the quality of Nguyen supernatant pills, which are described in the 20th volume of 'Drug Standard of Ministry of Public Health of the People's Republic of China' (Chinese medicament formulation preparations). The method comprises microscopic identification method of catechu and caper, physical and chemical reactions, thin-layer chromatography identification method of matrine, thin-layer chromatography identification method of borneol, thin-layer chromatography identification method of the catechu and content measurement method of the catechu in the Nguyen supernatant pills. The method for testing the quality of the Nguyen supernatant pills improves the quality control standard of the Nguyen supernatant pills, creates the content measurement and testing index and a testing method of the catechu which is a main medicament of the preparation, deletes physical and chemical reaction identification without specificity, increases the microscopical identification method of the catechu and the capers and the thin-layer chromatography identification method of the borneol, the catechu and the matrine, and ensures high quality control level of the compound preparation.
Description
Technical field
The present invention relates to the quality determining method of Ruan Shi shangqing pill in the 20 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Technical background
Medicine Ruan Shi shangqing pill in the 20 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation) has heat-clearing and fire-reducing, and the effect that promotes the production of body fluid to quench thirst is mainly used in abscess of throat, the noma aphtha, and body fluid deficiency, mouth parched and tongue scorched.This compound preparation is made up of Chinese crude drug catechu 606g, caper seed 61g, peppermint 121g, dark plum (meat) 30g, borax 61g, myrobalan 30g, subprostrate sophora 30g, borneol 30.3g, Radix Glycyrrhizae 30g, and above-mentioned raw materials is made 1000g altogether.Main ingredient in the catechu side of being is the peeling branch of legume catechu Acacia catechu (L.f.) Willd., dried dry soft extracts, has hygroscopic, myogenic, holds back the effect of sore; Caper seed is the dry seed of Capparidaceae plant caper seed Cappsris masaikai Levl., has clearing heat and detoxicating effect; Peppermint is the dry aerial parts of labiate peppermint Mentha haplocalyx Briq., has the effect of dispelling wind-heat, the clear sharp head, relieve sore throat promoting eruption; Dark plum (meat) is the dry almost ripe fruit of rosaceous plant Prunus mume (Sieb.) et Zucc., have astringe the lung, puckery intestines, the effect that promotes the production of body fluid to quench thirst; 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; The myrobalan is the dry mature fruit of combretaceae plant myrobalan Terminaliachebula Retz. or fine hair myrobalan Terminalia chebula Retz.tomentella Kurt., has puckery intestines and astringes the lung, and falls the effect of fiery relieve sore throat; Subprostrate sophora is the dry root and rhizome of legume sophora tonkinensis Gapnep Sophora tonkinensis Gagnep., has effect clearing heat and detoxicating, the detumescence relieve sore throat; Borneol is a borneolum syntheticum, has the inducing resuscitation of having one's ideas straightened out, the effect of clearing away heat to and alleviating pain.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 invigorate the spleen and benefit qi, the effect of clearing heat and detoxicating, coordinating the drug actions of a prescription." Drug Standard of Ministry of Public Health of the Peoples Republic of China " the 20 quality control standard of issuing the Ruan Shi shangqing pill, but in the existing Ruan Shi shangqing pill method of quality control that the Ministry of Public Health issues, has only the physical and chemical reaction discrimination method, specificity is relatively poor, limitation is very big, is difficult to accurately control the quality of Ruan Shi shangqing 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 Ruan Shi shangqing pill is provided, to improve the quality control standard of Ruan Shi shangqing pill.
The pharmaceutical formulation of Ruan Shi shangqing pill is by catechu 606g, caper seed 61g, and peppermint 121g, dark plum (meat) 30g, borax 61g, myrobalan 30g, subprostrate sophora 30g, borneol 30.3g, Radix Glycyrrhizae 30g forms; And make water-bindered pill 1000g.
The quality determining method of Ruan Shi shangqing pill of the present invention is:
1, the microscopical identification method of catechu and caper seed: get the Ruan Shi shangqing pill and put the microscopically observation: visible yellowish-brown block (microscopic features of catechu).The lithocyte shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic lithocyte wall thickness (microscopic features of caper seed);
2, physical and chemical reaction: get splint and be dipped in this product infusion, make slightly painted, to be dried after, immerse the salt acido again and promptly take out and put near the baking flame, be displaing amaranth on the bar;
3, the thin-layer chromatography discrimination method of matrine: get Ruan Shi shangqing pill 8g, porphyrize, put in the tool plug conical flask, add absolute ethyl alcohol-liquor ammoniae fortis (volume proportion 3: 2) 5ml, sealing was placed 10-20 minute, added methenyl choloride 40-60ml heating and refluxing extraction 0.5-1.5 hour, putting cold back filters, filtrate evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds absolute ethyl alcohol and makes solution that every 1ml contains 2mg product solution in contrast; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 10～15 μ l, reference substance solution 15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-ammoniacal liquor (volume proportion 10-14: 0.8-1.2: 0.1) be developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
4, the thin-layer chromatography discrimination method of borneol: get Ruan Shi shangqing pill 8g, porphyrize is put in the 250ml round-bottomed bottle, add water 40-60ml,, add ethyl acetate 2-3ml according to the operation of determination of volatile oil method, be heated to boiling and kept little 1-2 of boiling hour, divide and to get ethyl acetate as need testing solution; Other gets the borneol reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 3～8 μ l, reference substance solution 10～15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with sherwood oil (60～90 ℃)-ethyl acetate (volume proportion 15-20: 2-4) be developping agent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, 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;
5, the thin-layer chromatography qualitative identification method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 20-40ml, and sonicated 10-20 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 10-25ml, and sonicated 10-20 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, in contrast medicinal material solution; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw each 1～2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-formic acid (volume proportion 16-24: 4-6: 0.8-1.2) be developping agent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 100-110 ℃, in the test sample chromatogram, with the corresponding position of control medicinal material on, show the spot of same color;
6, the content assaying method of catechu in the Ruan Shi shangqing pill: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With acetonitrile-water (volume proportion 10: 90) is moving phase, and the detection wavelength is 280 ± 2nm, and number of theoretical plate calculates by the catechin peak should be not less than 2000;
2) preparation of reference substance solution: precision takes by weighing catechin reference substance, epicatechin reference substance, adds 50% ethanol and makes the solution that every 1ml contains catechin 0.2mg, epicatechin 0.1mg respectively, promptly;
3) preparation of need testing solution: it is an amount of to get this product, and porphyrize is got about 0.1g, accurately claims surely, puts in the 50ml measuring bottle, add 50% ethanol 40-45ml, sonicated (power 160w, frequency 50KHz) 15-45 minute is taken out, and puts cold, and add 50% ethanol to scale, and shake up, filter, get subsequent filtrate, promptly;
4) determination method: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The every 1g of this product contains catechu with catechin (C
15H
14O
6) and epicatechin (C
15H
14O
6) the total amount meter, must not be less than 70mg.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; The number percent of ethanol means the ratio of capacity in the time of 20 ℃.
The quality determining method of Ruan Shi shangqing pill of the present invention, improved the quality control standard of Ruan Shi shangqing pill, the assay of setting up main ingredient catechu in the preparation detects index and detection method thereof, having deleted the physical and chemical reaction that does not have specificity differentiates, increased the microscopical identification method of catechu and caper seed, and increased the thin-layer chromatography discrimination method of borneol, catechu and matrine, guaranteed this compound preparation higher quality standard level.
Embodiment
Embodiment:
The pharmaceutical formulation of Ruan Shi shangqing pill is by catechu 606g, caper seed 61g, and peppermint 121g, dark plum (meat) 30g, borax 61g, myrobalan 30g, subprostrate sophora 30g, borneol 30.3g, Radix Glycyrrhizae 30g forms.
Method for making: above nine flavors, borneol, borax grind respectively in addition, and all the other seven flavors are ground into fine powder, add borax, borneol, mixing, with the general ball of an amount of ethanol, drying is made water-bindered pill 1000g, upper garment, polishing, promptly.
The quality determining method of Ruan Shi shangqing pill of the present invention:
1, the microscopical identification method of catechu and caper seed: get the Ruan Shi shangqing pill and put the microscopically observation: visible yellowish-brown block (microscopic features of catechu), the lithocyte shape differs, pit is obvious, and what have includes the rufous material, divides dendritic lithocyte wall thickness (microscopic features of caper seed).
2, physical and chemical reaction: get splint and be dipped in this product infusion, make slightly painted, to be dried after, immerse the salt acido again and promptly take out and put near the baking flame, be displaing amaranth on the bar.
3, the thin-layer chromatography discrimination method of matrine: get Ruan Shi shangqing pill 8g, porphyrize, put in the tool plug conical flask, add absolute ethyl alcohol-liquor ammoniae fortis (volume proportion 3: 2) 5ml, sealing was placed 15 minutes, added methenyl choloride 50ml heating and refluxing extraction 1 hour, putting cold back filters, filtrate evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds absolute ethyl alcohol and makes solution that every 1ml contains 2mg product solution in contrast; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 10～15 μ l, reference substance solution 15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-ammoniacal liquor (volume proportion 12: 1: 0.1) is developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
4, the thin-layer chromatography discrimination method of borneol: get Ruan Shi shangqing pill 8g, porphyrize is put in the 250ml round-bottomed bottle, adds water 50ml, according to the operation of determination of volatile oil method, adds ethyl acetate 3ml, is heated to boiling and keeps little and boiled 1 hour, divides and gets ethyl acetate as need testing solution; Other gets the borneol reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 3～8 μ l, reference substance solution 10～15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with sherwood oil (60～90 ℃)-ethyl acetate (volume proportion 17: 3) is developping agent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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;
5, the thin-layer chromatography discrimination method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 30ml, and sonicated 15 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 20ml, and sonicated 15 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, in contrast medicinal material solution; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw each 1～2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with methenyl choloride-methyl alcohol-formic acid (volume proportion 20: 5: 1), launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, in the test sample chromatogram, with the corresponding position of control medicinal material on, show the spot of same color;
6, the content assaying method of catechu in the Ruan Shi shangqing pill: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With acetonitrile-water (volume proportion 10: 90) is moving phase, and the detection wavelength is 280nm, and number of theoretical plate calculates by the catechin peak should be not less than 2000;
2) preparation of reference substance solution: precision takes by weighing catechin reference substance, epicatechin reference substance, adds 50% ethanol and makes the solution that every 1ml contains catechin 0.2mg, epicatechin 0.1mg respectively, promptly;
3) preparation of need testing solution: it is an amount of to get this product, and porphyrize is got about 0.1g, accurately claims surely, puts in the 50ml measuring bottle, add 50% ethanol 40ml, sonicated (power 160w, frequency 50KHz) 30 minutes is taken out, and puts cold, and add 50% ethanol to scale, and shake up, filter, get subsequent filtrate, promptly;
4) determination method: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The every 1g of this product contains catechu with catechin (C
15H
14O
6) and epicatechin (C
15H
14O
6) the total amount meter, must not be less than 70mg.
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; The number percent of ethanol means the ratio of capacity in the time of 20 ℃.
The quality control standard of the Ruan Shi shangqing pill after the improvement is as follows:
Ruan Shi shangqing pill quality standard
The Ruan Shi shangqing pill
Ruanshi?Shangqing?Wan
[prescription] catechu 606g caper seed 61g peppermint 121g
Dark plum (meat) 30g borax 61g myrobalan 30g
Subprostrate sophora 30g borneol 30.3g Radix Glycyrrhizae 30g
[method for making] above nine flavors, borneol, borax grind respectively in addition, and all the other seven flavors are ground into fine powder, add borax, borneol, mixing, with the general ball of an amount of ethanol, drying is made water-bindered pill 1000g, upper garment, polishing, promptly.
[proterties] this product is the water-bindered pill of black, removes to show brown to sepia behind the dressing; Bitter cold, puckery, little sweet.
This product is got in [discriminating] (1), puts microscopically and observes: visible yellowish-brown block.The lithocyte shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic lithocyte wall thickness.
(2) get splint and be dipped in this product infusion, make slightly painted, to be dried after, immerse the salt acido again and promptly take out and put near the baking flame, be displaing amaranth on the bar.
(3) get this product 8g, porphyrize is put in the tool plug conical flask, adds absolute ethyl alcohol-liquor ammoniae fortis (3: 2) 5ml, sealing was placed 15 minutes, added methenyl choloride 50ml heating and refluxing extraction 1 hour, put cold back and filtered, filtrate evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the matrine reference substance, adds absolute ethyl alcohol and makes solution that every 1ml contains 2mg product solution in contrast.According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 10～15 μ l, reference substance solution 15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-ammoniacal liquor (12: 1: 0.1) is developping agent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
(4) get this product 8g, porphyrize is put in the 250ml round-bottomed bottle, adds water 50ml, according to the operation of determination of volatile oil method, adds ethyl acetate 3ml, is heated to boiling and keeps little and boiled 1 hour, divides and gets ethyl acetate as need testing solution.Other gets the borneol reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw above-mentioned need testing solution 3～8 μ l, reference substance solution 10～15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with sherwood oil (60～90 ℃)-ethyl acetate (17: 3) is developping agent, launch, take out, dry.Spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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.
(5) get this product 0.5g, porphyrize adds ethanol 30ml, and sonicated 15 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, as need testing solution.Other gets catechu control medicinal material 0.1g, adds ethanol 20ml, and sonicated 15 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, in contrast medicinal material solution.According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia B) test, draw each 1～2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-formic acid (20: 5: 1) is developping agent, launch, take out, dry.Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing at 105 ℃.In the test sample chromatogram, with the corresponding position of control medicinal material on, show the spot of same color.
[inspection] should meet every regulation relevant under the pill item (appendix IA of Chinese Pharmacopoeia version in 2005).
[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 the octadecylsilane chemically bonded silica; With acetonitrile-water (10: 90) is moving phase, and the detection wavelength is 280nm.Number of theoretical plate calculates by the catechin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing catechin reference substance, epicatechin reference substance, adds 50% ethanol and makes the solution that every 1ml contains catechin 0.2mg, epicatechin 0.1mg respectively, promptly.
It is an amount of that this product is got in the preparation of need testing solution, and porphyrize is got about 0.1g, and accurate the title decides, and puts in the 50ml measuring bottle, add 50% ethanol 40ml, sonicated (power 160w, frequency 50KHz) 30 minutes is taken out, and puts cold, and add 50% ethanol to scale, and shake up, filter, get subsequent filtrate, promptly.
Accurate respectively above-mentioned two kinds of 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 1g of this product contains catechu with catechin (C
15H
14O
6) and epicatechin (C
15H
14O
6) the total amount meter, must not be less than 70mg.
[function with cure mainly] heat-clearing and fire-reducing promotes the production of body fluid to quench thirst.Be used for abscess of throat, the noma aphtha, body fluid deficiency, mouth parched and tongue scorched.
[usage and consumption] swallowed or contained clothes, a 0.5g, 2～4 times on the one.
[specification] every bottled 8g.
[storage] is airtight, protection against the tide.
[term of validity] 5 years
Annotate: caper seed is the dry seed of the plant caper seed Capparis masaikai Levl. of cabbage rolls section.
Claims (1)
1. the quality determining method of a Ruan Shi shangqing pill, the pharmaceutical formulation of Ruan Shi shangqing pill be by catechu 606g, caper seed 61g, and peppermint 121g, Fructus Mume 30g, borax 61g, myrobalan 30g, subprostrate sophora 30g, borneol 30.3g, Radix Glycyrrhizae 30g forms, and makes water-bindered pill 1000g; The quality determining method that it is characterized in that the Ruan Shi shangqing pill is as follows:
1) the microscopical identification method of catechu and caper seed: get the Ruan Shi shangqing pill and put microscopically and observe: visible yellowish-brown block, the lithocyte shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic lithocyte wall thickness;
2) physical and chemical reaction: get splint and be dipped in this product infusion, make slightly painted, to be dried after, immerse the salt acido again and promptly take out and put near the baking flame, be displaing amaranth on the bar;
3) the thin-layer chromatography discrimination method of matrine: get Ruan Shi shangqing pill 8g, porphyrize, put in the tool plug conical flask, add absolute ethyl alcohol-dense ammonia solution 5ml of 3: 2 of proportioning by volume, sealing was placed 10-20 minute, added methenyl choloride 40-60ml heating and refluxing extraction 0.5-1.5 hour, putting cold back filters, filtrate evaporate to dryness, residue add absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds absolute ethyl alcohol and makes solution that every 1ml contains 2mg product solution in contrast; Test according to thin-layered chromatography, draw above-mentioned need testing solution 10～15 μ l, reference substance solution 15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-ammoniacal liquor proportioning 10-14: 0.8-1.2 by volume: 0.1 as developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
4) the thin-layer chromatography qualitative identification method of borneol: get Ruan Shi shangqing pill 8g, porphyrize is put in the 250ml round-bottomed bottle, add water 40-60ml,, add ethyl acetate 2-3ml according to the operation of determination of volatile oil method, be heated to boiling and kept little 1-2 of boiling hour, divide and to get ethyl acetate as need testing solution; Other gets the borneol reference substance, adds ethyl acetate 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 3～8 μ l, reference substance solution 10～15 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with 60～90 ℃ of petroleum ether-ethyl acetates proportioning 15-20 by volume: 2-4 is as developping agent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, 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;
5) the thin-layer chromatography discrimination method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 20-40ml, and sonicated 10-20 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 10-25ml, and sonicated 10-20 minute, filter, filtrate evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, in contrast medicinal material solution; Test according to thin-layered chromatography, draw each 1～2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methyl alcohol-formic acid proportioning 16-24: 4-6 by volume: 0.8-1.2 is as developping agent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 100-110 ℃, in the test sample chromatogram, with the corresponding position of control medicinal material on, show the spot of same color;
6) content assaying method of catechu in the Ruan Shi shangqing pill: according to high effective liquid chromatography for measuring
(1) chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; With acetonitrile-water by volume proportioning the detection wavelength was 280 ± 2nm as moving phase in 10: 90;
(2) preparation of reference substance solution: precision takes by weighing catechin reference substance, epicatechin reference substance, adds capacity percentage concentration 50% ethanol and makes the solution that every 1ml contains catechin 0.2mg, epicatechin 0.1mg respectively, promptly;
(3) preparation of need testing solution: it is an amount of to get this product, and porphyrize is got about 0.1g, the accurate title, decide, and puts in the 50ml measuring bottle, adds capacity percentage concentration 50% ethanol 40-45ml, sonicated 15-45 minute, take out, put coldly, and add capacity percentage concentration 50% ethanol to scale, shake up, filter, get subsequent filtrate, promptly;
(4) determination method: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly; The every 1g of this product contains the total amount of catechu in catechin and epicatechin, must not be less than 70mg;
Wherein, contain the some grams of solute among the every 100ml of " % (g/ml) " expression solution; The number percent of ethanol means the ratio of capacity in the time of 20 ℃.
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| CN103852554B (en) * | 2012-11-30 | 2015-11-18 | 山东金诃药物研究开发有限公司 | A kind of Tibetan medicinal composition whin disappears the quality determining method of preparation of itching |
| CN104155240A (en) * | 2014-08-28 | 2014-11-19 | 山西振东开元制药有限公司 | Quality control method of Shangqing pills |
| CN105012360B (en) * | 2015-07-14 | 2018-11-09 | 昆明理工大学 | A kind of buccal tablet for clearing and moistening throat |
| CN104965046A (en) * | 2015-07-17 | 2015-10-07 | 江苏天晟药业有限公司 | Quality control method for cosmetics containing traditional Chinese medicinal ingredients |
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