CN101773560A - Method for testing quality of Nguyen supernatant pills - Google Patents
Method for testing quality of Nguyen supernatant pills Download PDFInfo
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- CN101773560A CN101773560A CN201010101791A CN201010101791A CN101773560A CN 101773560 A CN101773560 A CN 101773560A CN 201010101791 A CN201010101791 A CN 201010101791A CN 201010101791 A CN201010101791 A CN 201010101791A CN 101773560 A CN101773560 A CN 101773560A
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- 238000012360 testing method Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000006187 pill Substances 0.000 title claims abstract description 46
- 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
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 26
- 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
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 241000722721 Capparis Species 0.000 claims abstract description 15
- 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
- 244000080767 Areca catechu Species 0.000 claims abstract 12
- 239000000243 solution Substances 0.000 claims description 83
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 68
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 40
- 239000013558 reference substance Substances 0.000 claims description 40
- 229960004756 ethanol Drugs 0.000 claims description 30
- 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
- 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
- 210000000582 semen Anatomy 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
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000001768 carboxy methyl cellulose Substances 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
- 239000000463 material Substances 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
- 239000002904 solvent Substances 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
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000004575 stone Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 6
- 235000013372 meat Nutrition 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
- OJHAHQJRQIOCFK-UHFFFAOYSA-N azane;chloroform;methanol Chemical compound N.OC.ClC(Cl)Cl OJHAHQJRQIOCFK-UHFFFAOYSA-N 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
- 210000004027 cell Anatomy 0.000 claims description 4
- 210000002421 cell wall Anatomy 0.000 claims description 4
- LIOIDYIXMHPGGB-UHFFFAOYSA-N chloroform;formic acid;methanol Chemical compound OC.OC=O.ClC(Cl)Cl LIOIDYIXMHPGGB-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000945 filler Substances 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
- 239000012567 medical material Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003208 petroleum Substances 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
- 239000002253 acid Substances 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 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
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 8
- 238000003908 quality control method Methods 0.000 abstract description 7
- 229940079593 drug Drugs 0.000 abstract description 6
- 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
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 abstract 2
- 235000017336 Capparis spinosa Nutrition 0.000 abstract 2
- 229940116229 borneol Drugs 0.000 abstract 2
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 abstract 2
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 abstract 2
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- 238000000691 measurement method Methods 0.000 abstract 1
- 244000235603 Acacia catechu Species 0.000 description 22
- 230000000694 effects Effects 0.000 description 11
- 210000001124 body fluid Anatomy 0.000 description 5
- 239000010839 body fluid Substances 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 231100000614 poison Toxicity 0.000 description 4
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- 206010068319 Oropharyngeal pain Diseases 0.000 description 3
- 201000007100 Pharyngitis Diseases 0.000 description 3
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- 238000004128 high performance liquid chromatography Methods 0.000 description 3
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- 206010012735 Diarrhoea Diseases 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
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- 241000001522 Terminalia chebula Species 0.000 description 2
- 235000011517 Terminalia chebula Nutrition 0.000 description 2
- 208000025865 Ulcer Diseases 0.000 description 2
- 208000002399 aphthous stomatitis Diseases 0.000 description 2
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- 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
- 206010040943 Skin Ulcer Diseases 0.000 description 1
- 241000566916 Tomentella Species 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 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
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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 resolving heat and reducing pathogenic fire, and the effect of promoting the production of body fluid to quench thirst is mainly used in laryngopharynx swelling and pain, ulcerative gingivitis aphtha, deficiency of body fluid, dry mouth and tougue.This compound preparation is made up of Chinese crude drug catechu 606g, Semen Capparis 61g, Herba Menthae 121g, Fructus Mume (meat) 30g, Borax 61g, Fructus Chebulae 30g, Radix Sophorae Tonkinensis 30g, Borneolum Syntheticum 30.3g, Radix Glycyrrhizae 30g, and above-mentioned raw materials is made 1000g altogether.Principal agent in the catechu side of being is the peeling branch of leguminous plant catechu Acacia catechu (L.f.) Willd., dried dry soft extracts, has removing dampness, granulation promoting, holds back the effect of skin ulcer; Semen Capparis is the dry seed of Capparidaceae plant Semen Capparis Cappsris masaikai Levl., has the effect of heat-clearing and toxic substances removing; Herba Menthae is the dry aerial parts of labiate Herba Menthae Mentha haplocalyx Briq., has the effect of dispelling wind-heat, the clear sharp head, sore-throat relieving rash; Fructus Mume (meat) is the dry almost ripe fruit of rosaceous plant Prunus mume (Sieb.) et Zucc., have astringe the lung, the effect of astringing intestine to stop diarrhea, promoting 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%, the effect of tool heat-clearing and toxic substances removing, removing heat from the lung and dissipating phlegm; The Fructus Chebulae is the dry mature fruit of Combretum Racemosum plant Fructus Chebulae Terminaliachebula Retz. or fine hair Fructus Chebulae Terminalia chebula Retz.tomentella Kurt., has astringing intestine to stop diarrhea and astringes the lung, the effect of pathogenic fire reducing sore-throat relieving; Radix Sophorae Tonkinensis is the dry root and rhizome of leguminous plant Sophora tonkinensis Gagnep. Sophora tonkinensis Gagnep., has the effect of heat-clearing and toxic substances removing, detumescence sore-throat relieving; Borneolum Syntheticum is a borneolum syntheticum, has the refreshment of having one's ideas straightened out, the effect of clearing away heat to alleviate pain.Radix Glycyrrhizae is the dry root and rhizome of glycyrrhizic legume Glycyrrhiza inflata Bat., Glycyrrhiza inflata Bat. Glycyrrhiza in flata Bat or Glycyrrhiza glabra L. Glycyrrhiza glabra L., has the effect of invigorating the spleen and replenishing QI, heat-clearing and toxic substances removing, coordinating the actions of various ingredients in 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 Ministry of Public Health is issued, 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, Semen Capparis 61g, and Herba Menthae 121g, Fructus Mume (meat) 30g, Borax 61g, Fructus Chebulae 30g, Radix Sophorae Tonkinensis 30g, Borneolum Syntheticum 30.3g, Radix Glycyrrhizae 30g forms; And make watered pill 1000g.
The quality determining method of Ruan Shi shangqing pill of the present invention is:
1, the microscopical identification method of catechu and Semen Capparis: get the Ruan Shi shangqing pill and put the microscopically observation: visible yellowish-brown block (microscopic features of catechu).The stone cell shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic stone cell wall thickness (microscopic features of Semen Capparis);
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 dehydrated alcohol-liquor ammoniae fortis (volume proportion 3: 2) 5ml, sealing was placed 10-20 minute, added chloroform 40-60ml heating and refluxing extraction 0.5-1.5 hour, putting cold back filters, filtrate evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds dehydrated alcohol and makes solution that every 1ml contains 2mg product solution in contrast; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-ammonia (volume proportion 10-14: 0.8-1.2: 0.1) be developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
4, the thin layer chromatography discrimination method of Borneolum Syntheticum: 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 Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (volume proportion 15-20: 2-4) be developing solvent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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;
5, the thin layer chromatography qualitative identification method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 20-40ml, and supersound process 10-20 minute, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 10-25ml, and supersound process 10-20 minute, filter, filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-formic acid (volume proportion 16-24: 4-6: 0.8-1.2) be developing solvent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle 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 filler; With acetonitrile-water (volume proportion 10: 90) is mobile 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, supersound process (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) algoscopy: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, 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; Alcoholic acid percentage ratio 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 principal agent 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 Semen Capparis, and increased the thin layer chromatography discrimination method of Borneolum Syntheticum, catechu and matrine, guaranteed this compound preparation higher quality standard level.
The specific embodiment
Embodiment:
The pharmaceutical formulation of Ruan Shi shangqing pill is by catechu 606g, Semen Capparis 61g, and Herba Menthae 121g, Fructus Mume (meat) 30g, Borax 61g, Fructus Chebulae 30g, Radix Sophorae Tonkinensis 30g, Borneolum Syntheticum 30.3g, Radix Glycyrrhizae 30g forms.
Method for making: above nine flavors, Borneolum Syntheticum, Borax grind respectively in addition, and all the other seven flavors are ground into fine powder, add Borax, Borneolum Syntheticum, mixing, with the general ball of an amount of ethanol, drying is made watered 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 Semen Capparis: get the Ruan Shi shangqing pill and put the microscopically observation: visible yellowish-brown block (microscopic features of catechu), the stone cell shape differs, pit is obvious, and what have includes the rufous material, divides dendritic stone cell wall thickness (microscopic features of Semen Capparis).
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 dehydrated alcohol-liquor ammoniae fortis (volume proportion 3: 2) 5ml, sealing was placed 15 minutes, added chloroform 50ml heating and refluxing extraction 1 hour, putting cold back filters, filtrate evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds dehydrated alcohol and makes solution that every 1ml contains 2mg product solution in contrast; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-ammonia (volume proportion 12: 1: 0.1) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
4, the thin layer chromatography discrimination method of Borneolum Syntheticum: 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 Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (volume proportion 17: 3) is developing solvent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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;
5, the thin layer chromatography discrimination method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 30ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 20ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution; According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-methanol-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 speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle 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 filler; With acetonitrile-water (volume proportion 10: 90) is mobile 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, supersound process (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) algoscopy: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, 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; Alcoholic acid percentage ratio 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 Semen Capparis 61g Herba Menthae 121g
Fructus Mume (meat) 30g Borax 61g Fructus Chebulae 30g
Radix Sophorae Tonkinensis 30g Borneolum Syntheticum 30.3g Radix Glycyrrhizae 30g
[method for making] above nine flavors, Borneolum Syntheticum, Borax grind respectively in addition, and all the other seven flavors are ground into fine powder, add Borax, Borneolum Syntheticum, mixing, with the general ball of an amount of ethanol, drying is made watered pill 1000g, upper garment, polishing, promptly.
[character] this product is the watered pill of black, removes to show brown to sepia behind the coating; Bitter in the mouth cold, puckery, little sweet.
This product is got in [discriminating] (1), puts microscopically and observes: visible yellowish-brown block.The stone cell shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic stone cell 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 dehydrated alcohol-liquor ammoniae fortis (3: 2) 5ml, sealing was placed 15 minutes, added chloroform 50ml heating and refluxing extraction 1 hour, put cold back and filtered, filtrate evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets the matrine reference substance, adds dehydrated alcohol and makes solution that every 1ml contains 2mg product solution in contrast.According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-ammonia (12: 1: 0.1) is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle 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 Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (17: 3) is developing solvent, launch, take out, dry.Spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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.
(5) get this product 0.5g, porphyrize adds ethanol 30ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution.Other gets catechu control medicinal material 0.1g, adds ethanol 20ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.According to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-formic acid (20: 5: 1) is developing solvent, launch, take out, dry.Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle 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 filler with the octadecylsilane chemically bonded silica; With acetonitrile-water (10: 90) is mobile 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, supersound process (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 algoscopy inject chromatograph of liquid, 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] resolving heat and reducing pathogenic fire, promoting the production of body fluid to quench thirst.Be used for laryngopharynx swelling and pain, ulcerative gingivitis aphtha, deficiency of body fluid, dry mouth and tougue.
[usage and consumption] swallowed or buccal, a 0.5g, 2～4 times on the one.
[specification] every bottled 8g.
[storage] is airtight, protection against the tide.
[effect duration] 5 years
Annotate: Semen Capparis is the dry seed of the plant Semen Capparis 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, Semen Capparis 61g, and Herba Menthae 121g, Fructus Mume (meat) 30g, Borax 61g, Fructus Chebulae 30g, Radix Sophorae Tonkinensis 30g, Borneolum Syntheticum 30.3g, Radix Glycyrrhizae 30g forms, and makes watered 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 Semen Capparis: get the Ruan Shi shangqing pill and put microscopically and observe: visible yellowish-brown block, the stone cell shape differs, and pit is obvious, and what have includes the rufous material, divides dendritic stone cell 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 dehydrated alcohol-dense ammonia solution 5ml of 3: 2 of proportioning by volume, sealing was placed 10-20 minute, added chloroform 40-60ml heating and refluxing extraction 0.5-1.5 hour, putting cold back filters, filtrate evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution; Other gets the matrine reference substance, adds dehydrated alcohol and makes solution that every 1ml contains 2mg product solution in contrast; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-ammonia proportioning 10-14: 0.8-1.2 by volume: 0.1 as developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color;
4) the thin layer chromatography qualitative identification method of Borneolum Syntheticum: 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 Borneolum Syntheticum reference substance, adds ethyl acetate 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 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 adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate proportioning 15-20 by volume: 2-4 is as developing solvent, launch, take out, dry, spray is with 10% (g/ml) phosphomolybdic acid ethanol solution, and it is clear to be heated to the 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;
5) the thin layer chromatography discrimination method of catechu: get Ruan Shi shangqing pill 0.5g, porphyrize adds ethanol 20-40ml, and supersound process 10-20 minute, filter, filtrate evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets catechu control medicinal material 0.1g, adds ethanol 10-25ml, and supersound process 10-20 minute, filter, filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with chloroform-methanol-formic acid proportioning 16-24: 4-6 by volume: 0.8-1.2 is as developing solvent, launch, take out, dry, spray is with 10% (g/ml) ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 100-110 ℃, in the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle 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 filler; With acetonitrile-water by volume proportioning the detection wavelength was 280 ± 2nm as mobile 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, supersound process 15-45 minute, take out, put coldly, and add capacity percentage concentration 50% ethanol to scale, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: accurate respectively above-mentioned two kinds of reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, 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; Alcoholic acid percentage ratio means the ratio of capacity in the time of 20 ℃.
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