CN1327217C - Quality control of Jianweixiaoshi tablets for promotnig digest - Google Patents
Quality control of Jianweixiaoshi tablets for promotnig digest Download PDFInfo
- Publication number
- CN1327217C CN1327217C CNB2004100132365A CN200410013236A CN1327217C CN 1327217 C CN1327217 C CN 1327217C CN B2004100132365 A CNB2004100132365 A CN B2004100132365A CN 200410013236 A CN200410013236 A CN 200410013236A CN 1327217 C CN1327217 C CN 1327217C
- Authority
- CN
- China
- Prior art keywords
- solution
- methyl alcohol
- ethyl acetate
- medicinal material
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000003908 quality control method Methods 0.000 title claims description 16
- 239000000463 material Substances 0.000 claims abstract description 58
- 238000002360 preparation method Methods 0.000 claims abstract description 47
- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000001100 (2S)-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chroman-4-one Substances 0.000 claims abstract description 14
- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 claims abstract description 14
- APSNPMVGBGZYAJ-GLOOOPAXSA-N clematine Natural products COc1cc(ccc1O)[C@@H]2CC(=O)c3c(O)cc(O[C@@H]4O[C@H](CO[C@H]5O[C@@H](C)[C@H](O)[C@@H](O)[C@H]5O)[C@@H](O)[C@H](O)[C@H]4O)cc3O2 APSNPMVGBGZYAJ-GLOOOPAXSA-N 0.000 claims abstract description 14
- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 claims abstract description 14
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 claims abstract description 14
- 229940025878 hesperidin Drugs 0.000 claims abstract description 14
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 189
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 96
- 238000012360 testing method Methods 0.000 claims description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000003814 drug Substances 0.000 claims description 41
- XEKOWRVHYACXOJ-UHFFFAOYSA-N ethyl acetate Substances CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000706 filtrate Substances 0.000 claims description 26
- 238000004587 chromatography analysis Methods 0.000 claims description 24
- 229940079593 drug Drugs 0.000 claims description 22
- 241001092040 Crataegus Species 0.000 claims description 21
- 235000009917 Crataegus X brevipes Nutrition 0.000 claims description 20
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 claims description 20
- 235000009685 Crataegus X maligna Nutrition 0.000 claims description 20
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 claims description 20
- 235000009486 Crataegus bullatus Nutrition 0.000 claims description 20
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 claims description 20
- 235000009682 Crataegus limnophila Nutrition 0.000 claims description 20
- 235000004423 Crataegus monogyna Nutrition 0.000 claims description 20
- 235000002313 Crataegus paludosa Nutrition 0.000 claims description 20
- 235000009840 Crataegus x incaedua Nutrition 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000013558 reference substance Substances 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000010828 elution Methods 0.000 claims description 12
- 239000002024 ethyl acetate extract Substances 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 240000001811 Dioscorea oppositifolia Species 0.000 claims description 8
- 238000003556 assay Methods 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 239000000741 silica gel Substances 0.000 claims description 8
- 229910002027 silica gel Inorganic materials 0.000 claims description 8
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 8
- 235000002722 Dioscorea batatas Nutrition 0.000 claims description 7
- 235000006536 Dioscorea esculenta Nutrition 0.000 claims description 7
- 235000003416 Dioscorea oppositifolia Nutrition 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 6
- 230000004580 weight loss Effects 0.000 claims description 6
- PJWKAIDLIGVSCP-UHFFFAOYSA-N OC=O.CCOC(C)=O.C1CCCCC1 Chemical compound OC=O.CCOC(C)=O.C1CCCCC1 PJWKAIDLIGVSCP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- OAMZXMDZZWGPMH-UHFFFAOYSA-N ethyl acetate;toluene Chemical compound CCOC(C)=O.CC1=CC=CC=C1 OAMZXMDZZWGPMH-UHFFFAOYSA-N 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 238000004811 liquid chromatography Methods 0.000 claims description 3
- NOTFZGFABLVTIG-UHFFFAOYSA-N Cyclohexylethyl acetate Chemical compound CC(=O)OCCC1CCCCC1 NOTFZGFABLVTIG-UHFFFAOYSA-N 0.000 claims 1
- GXCLVBGFBYZDAG-UHFFFAOYSA-N N-[2-(1H-indol-3-yl)ethyl]-N-methylprop-2-en-1-amine Chemical compound CN(CCC1=CNC2=C1C=CC=C2)CC=C GXCLVBGFBYZDAG-UHFFFAOYSA-N 0.000 claims 1
- OJCYRKYVCZBFDK-UHFFFAOYSA-N acetic acid;cyclohexane;ethyl acetate Chemical compound CC(O)=O.CCOC(C)=O.C1CCCCC1 OJCYRKYVCZBFDK-UHFFFAOYSA-N 0.000 claims 1
- UOIFTOBIGNZZSO-UHFFFAOYSA-N acetic acid;ethyl acetate;hexane Chemical compound CC(O)=O.CCCCCC.CCOC(C)=O UOIFTOBIGNZZSO-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- RTEXIPZMMDUXMR-UHFFFAOYSA-N benzene;ethyl acetate Chemical compound CCOC(C)=O.C1=CC=CC=C1 RTEXIPZMMDUXMR-UHFFFAOYSA-N 0.000 claims 1
- MDHYEMXUFSJLGV-UHFFFAOYSA-N beta-phenethyl acetate Natural products CC(=O)OCCC1=CC=CC=C1 MDHYEMXUFSJLGV-UHFFFAOYSA-N 0.000 claims 1
- PQPKPCPUSAPERC-UHFFFAOYSA-N ethyl acetate;formic acid;hexane Chemical compound OC=O.CCCCCC.CCOC(C)=O PQPKPCPUSAPERC-UHFFFAOYSA-N 0.000 claims 1
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 claims 1
- 239000008194 pharmaceutical composition Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 230000001737 promoting effect Effects 0.000 abstract description 9
- 230000029087 digestion Effects 0.000 abstract description 8
- 210000002784 stomach Anatomy 0.000 abstract description 8
- 238000005728 strengthening Methods 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 6
- 241001038563 Pseudostellaria Species 0.000 abstract description 4
- 238000004809 thin layer chromatography Methods 0.000 abstract description 3
- 241000675108 Citrus tangerina Species 0.000 abstract 1
- 241000209140 Triticum Species 0.000 abstract 1
- 235000021307 Triticum Nutrition 0.000 abstract 1
- 230000005180 public health Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 210000000952 spleen Anatomy 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 2
- 229920001353 Dextrin Polymers 0.000 description 2
- 235000002723 Dioscorea alata Nutrition 0.000 description 2
- 235000007056 Dioscorea composita Nutrition 0.000 description 2
- 235000009723 Dioscorea convolvulacea Nutrition 0.000 description 2
- 235000005362 Dioscorea floribunda Nutrition 0.000 description 2
- 235000004868 Dioscorea macrostachya Nutrition 0.000 description 2
- 235000005361 Dioscorea nummularia Nutrition 0.000 description 2
- 235000005360 Dioscorea spiculiflora Nutrition 0.000 description 2
- 244000281702 Dioscorea villosa Species 0.000 description 2
- 235000006350 Ipomoea batatas var. batatas Nutrition 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 235000019425 dextrin Nutrition 0.000 description 2
- 235000004879 dioscorea Nutrition 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 235000019640 taste Nutrition 0.000 description 2
- 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 description 1
- 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 description 1
- WCGUUGGRBIKTOS-GPOJBZKASA-N (3beta)-3-hydroxyurs-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C WCGUUGGRBIKTOS-GPOJBZKASA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241001672694 Citrus reticulata Species 0.000 description 1
- 235000014493 Crataegus Nutrition 0.000 description 1
- 235000008440 Crataegus cuneata Nutrition 0.000 description 1
- 244000160089 Crataegus cuneata Species 0.000 description 1
- 241000657480 Crataegus pinnatifida Species 0.000 description 1
- 235000014283 Crataegus pinnatifida var major Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- OVSQVDMCBVZWGM-SJWGPRHPSA-N Hyperin Natural products O[C@H]1[C@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-SJWGPRHPSA-N 0.000 description 1
- FVQOMEDMFUMIMO-UHFFFAOYSA-N Hyperosid Natural products OC1C(O)C(O)C(CO)OC1OC1C(=O)C2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 FVQOMEDMFUMIMO-UHFFFAOYSA-N 0.000 description 1
- 244000131316 Panax pseudoginseng Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 241001038562 Pseudostellaria heterophylla Species 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- MDZKJHQSJHYOHJ-UHFFFAOYSA-N crataegolic acid Natural products C1C(O)C(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MDZKJHQSJHYOHJ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 description 1
- 235000012734 epicatechin Nutrition 0.000 description 1
- LSYBEKRLBPCVES-UHFFFAOYSA-N ethyl acetate formic acid Chemical compound C(C)(=O)OCC.C(=O)O.C(=O)O LSYBEKRLBPCVES-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- NQYPTLKGQJDGTI-FCVRJVSHSA-N hyperoside Natural products OC[C@H]1O[C@@H](OC2=C(Oc3cc(O)cc(O)c3[C@H]2O)c4ccc(O)c(O)c4)[C@H](O)[C@@H](O)[C@H]1O NQYPTLKGQJDGTI-FCVRJVSHSA-N 0.000 description 1
- MDZKJHQSJHYOHJ-LLICELPBSA-N maslinic acid Chemical compound C1[C@@H](O)[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MDZKJHQSJHYOHJ-LLICELPBSA-N 0.000 description 1
- 230000037306 mature skin Effects 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 description 1
- BBFYUPYFXSSMNV-UHFFFAOYSA-N quercetin-7-o-galactoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 BBFYUPYFXSSMNV-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 trimethyl Chemical compound 0.000 description 1
- 229940096998 ursolic acid Drugs 0.000 description 1
- PLSAJKYPRJGMHO-UHFFFAOYSA-N ursolic acid Natural products CC1CCC2(CCC3(C)C(C=CC4C5(C)CCC(O)C(C)(C)C5CCC34C)C2C1C)C(=O)O PLSAJKYPRJGMHO-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a method for detecting and controlling the quality of a compound preparation (a stomach strengthening and digestion promoting tablet) prepared from the following traditional Chinese medicinal materials: 228.6g of pseudostellaria root, 22.9g of tangerine peel, 171.4g of yam, 171.4g of (sauted) wheat germ and 114.3g of haw. The present invention is characterized in that high performance liquid chromatography is used for measuring the content of hesperidin (C28H34O15) in the stomach strengthening and digestion promoting tablet; thin layer chromatography is used for identifying the traditional Chinese medicinal materials (the pseudostellaria root and the haw) in the compound preparation. The method ensures the accuracy and the advancement of the quality detecting standard of the stomach strengthening and digestion promoting tablet, the quality of the stomach strengthening and digestion promoting tablet can be effectively controlled, and the present invention can be used as a stability index of a quality controlling and exploring process of the stomach strengthening and digestion promoting tablet.
Description
Technical field
The present invention relates to the method for quality control of digestion-promoting stomachic in the 16 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation).
Technical background
The medicine digestion-promoting stomachic that has digestion promoting effect in the 16 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation), this compound preparation is made up of Chinese crude drug radix pseudostellariae 228.6g, dried orange peel 22.9g, Chinese yam 171.4g, Fructus Hordei Germinatus (stir-fry) 171.4g, hawthorn 114.3g, and above-mentioned raw materials is made 1000 (sheets) or 1600 (small pieces) altogether.Main flavour of a drug in the radix pseudostellariae side of being, the dried root for pinkwort caryophyllaceous ginseng Pseudostellaria heterophylla (Miq.) Pax ex Pax et hoffm. has the effect that replenishes qi to invigorate the spleen; Dried orange peel is the dry mature skin of rutaceae orange Citrus reticulata Blanco and variety thereof, has the effect of regulating qi-flowing for strengthening spleen; Chinese yam is the dry rhizome of Dioscoreaceae plant Chinese yam Dioscorea opposita Thunb., has the effect of tonifying spleen nourishing the stomach.Fructus Hordei Germinatus is that the ripening fruits of grass barley Hordeum vulgare L. gets through the drying of germinateing, and has the effect of promote qi circulation digestion promoting, spleen benefiting and stimulating the appetite; Hawthorn is the dry mature fruit of rosaceous plant large-fruited Chinese hawthorn Crataegus pinnatifidaBge.Var.major N.E.Br or hawthorn Crataegus pinnatifida Bge, has food digesting stomach fortifying, the effect of the diffusing stasis of blood of promoting the circulation of qi mainly contains chemical constitutions such as crataegolic acid, epicatechin, Hyperoside, citric acid and methyl esters, dimethyl ester, trimethyl, ursolic acid; Second WS3-B-3086-98 of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " (Chinese traditional patent formulation preparation) and " Drug Standard of Ministry of Public Health of the Peoples Republic of China " the 16 quality control standard of having issued digestion-promoting stomachic, but in the existing digestion-promoting stomachic method of quality control that the Ministry of Public Health issues, have only thin layer to differentiate, limitation is very big, is difficult to accurately control the quality of digestion-promoting stomachic; The present invention overcomes the deficiencies in the prior art, improve the quality control standard of digestion-promoting stomachic, set up assay index and detection method thereof in the preparation, increase the thin-layer chromatography qualitative identification method of main ingredient radix pseudostellariae wherein and medicinal material hawthorn, guaranteed this compound preparation higher quality standard level.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, formulate the method for quality control of new digestion-promoting stomachic, utilize Determination of Hesperidin Content in this compound preparation of high effective liquid chromatography for measuring; The thin-layer chromatography that increases main ingredient radix pseudostellariae in this compound preparation and medicinal material hawthorn is differentiated, has guaranteed the accuracy and the advance of quality determining method, can control the product quality of digestion-promoting stomachic effectively.
The present invention is achieved by following technical proposals:
The quality control detection method that digestion-promoting stomachic is new, this method comprises following determination step:
1. measure stomach strengthening and digestion promoting with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000)
Aurantiamarin (C in the sheet
28H
34O
15) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; (35-45: 55-65) be moving phase, the detection wavelength is 283 ± 2nm to methyl alcohol--0.5% glacial acetic acid solution;
The preparation of b reference substance solution: precision takes by weighing the aurantiamarin reference substance 5-25mg through the phosphorus pentoxide drying, puts in the 25-250ml measuring bottle, adds in methyl alcohol or the ethanol any and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol or ethanol or moving phase and is diluted to scale, shakes up, and makes the solution that every 1ml contains 5--50 μ g;
C. the preparation of need testing solution: get this product 5-20 sheet, the accurate title, decided mixing, porphyrize is got 1--3g, and accurate the title decides, accurate any 10--50ml that adds in methyl alcohol or the ethanol claims to decide weight, puts in the water-bath backflow 0.5-2 hour, put coldly, supply with in methyl alcohol or the ethanol any and to subtract weight loss, filter, precision is measured subsequent filtrate 1-25ml and is put in the 5-25ml measuring bottle, adds in water or aqueous methanol or the hydrous ethanol any to scale, shakes up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: accurate respectively reference substance solution and each 5--20 μ l of need testing solution of drawing, inject liquid chromatograph, the mensuration Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, sheet must not be less than 0.20mg; Small pieces must not be less than 0.12mg.
2. this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000):
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 2-10g, add little the boiling of water and decocted 0.5-3 hour, decocting liquid is centrifugal, gets supernatant and passes through D
101Macroporous resin column (internal diameter 0.5-2cm, long 5-25cm), water 50-300ml successively, ethanol 50-200ml wash-out discards water elution liquid, collects ethanol eluate, and any 0.5-2ml that evaporate to dryness, residue add in methyl alcohol or the ethanol makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product 20-40 sheet (sheet) or 40-60 sheet (small pieces), porphyrize adds any 25-100ml in methyl alcohol or the ethanol, put in the water-bath reflux 15-60 minute, and filtered the filtrate evaporate to dryness, residue adds water 10-30ml makes dissolving, passes through D
101Macroporous resin column (internal diameter 0.5-2cm, long 5-25cm), water 50-300ml successively, ethanol 50-200ml wash-out discards water elution liquid, collects ethanol eluate, and any 0.5-2ml that evaporate to dryness, residue add in methyl alcohol or the ethanol makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000): draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any thin layer plate in same silica G or GF254 or H, with in toluene (or benzene, sherwood oil, normal hexane, cyclohexane)-ethyl acetate (8: 2) or (8: 1) or (9: 2) any is developping agent, launch, take out, dry, spray is with 1-5% vanillic aldehyde sulfuric acid or 5-10% ethanol solution of sulfuric acid, 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 control medicinal material chromatogram on, show the spot of same color.
Optimized technical scheme of the present invention can be:
The method of quality control of digestion-promoting stomachic also comprises the following steps:
3. this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000):
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 1-5g, boiling 0.5-2 hour, decocting liquid filters, and filtrate is concentrated into 10-50ml, with any adjusting pH value to 1～3 in hydrochloric acid or the watery hydrochloric acid, extract 1-3 time with ethyl acetate, each 10-50ml merges the ethyl acetate extract, evaporate to dryness, any 0.5-2ml that residue adds in methyl alcohol or the ethanol makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product 20-40 sheet (sheet) or 40-60 sheet (small pieces), porphyrize adds any 25-100ml in methyl alcohol or the ethanol, put in the water-bath reflux 15-60 minute, filter, filtrate evaporate to dryness, residue add water 10-50ml makes dissolving, extract 1-3 time with ethyl acetate, each 10-50ml merges the ethyl acetate extract, evaporate to dryness, any 0.5-2ml that residue adds in methyl alcohol or the ethanol makes dissolving, as need testing solution;
C. test according to thin-layered chromatography (appendix VIB): draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on any thin layer plate in same silica G or GF254 or H, so that cyclohexane (or normal hexane, sherwood oil)-(19-20: 19-21: any 0.2-1.5) is developping agent to ethyl acetate-formic acid (or acetate), launch, take out, dry, spray is with 1-5% ferric trichloride ethanolic solution, and 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 chromatogram on, show the principal spot of same color.
More preferably technical scheme comprises following determination step:
1. measure aurantiamarin (C in the digestion-promoting stomachic with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000)
28H
34O
15) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; Methyl alcohol--0.5% glacial acetic acid solution (40: 60) is a moving phase, and the detection wavelength is 283nm;
The preparation of b reference substance solution: precision takes by weighing through dry 48 hours aurantiamarin reference substance 12.5mg of phosphorus pentoxide, puts in the 100ml measuring bottle, adds methyl alcohol and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol and is diluted to scale, shakes up, and makes the solution that every 1ml contains 15 μ g;
C. the preparation of need testing solution: get 10 of this product, the accurate title, decided porphyrize, get 2g, the accurate title, decide, the accurate methyl alcohol 20ml that adds, claim to decide weight, reflux 1 hour is put cold, weight decided in title again, supplies with methyl alcohol to subtract weight loss, filters, precision is measured subsequent filtrate 5ml and is put in the 10ml measuring bottle, adds water to scale, shakes up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, inject liquid chromatograph, the mensuration Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, sheet must not be less than 0.20mg; Small pieces must not be less than 0.12mg.
2. this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000):
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 5g, add little the boiling of water and decocted 2 hours, decocting liquid is centrifugal, gets supernatant and passes through D
101Macroporous resin column (internal diameter 1.2cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 of this product (sheet) or 48 (small pieces), porphyrize adds methyl alcohol 50ml, puts in the water-bath reflux 30 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, passes through D
101Macroporous resin column (internal diameter 1.2cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000): draw each 20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (8: 2) is developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid, and 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 chromatogram on, show the spot of same color.
The method of quality control of preferred digestion-promoting stomachic also comprises the following steps: in the above-mentioned more preferably technical scheme steps
3. this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000)
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 2g, boiling 1 hour, decocting liquid filters, and filtrate is concentrated into 20ml, regulates pH value to 1～2 with watery hydrochloric acid, from " extract 2 times with ethyl acetate; each 20ml merges the ethyl acetate extract, evaporate to dryness; residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 of this product (sheet) or 48 (small pieces), porphyrize adds methyl alcohol 50ml, put in the water-bath reflux 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with ethyl acetate, each 20ml merges the ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
C. test according to thin-layered chromatography (appendix VIB): draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-formic acid (20: 20: 1) is developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution, and 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 chromatogram on, show the principal spot of same color;
Digestion-promoting stomachic among second WS3-B-3086-98 of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " of the present invention (Chinese traditional patent formulation preparation) and the 16, every sheet weight 0.8g or 0.5g.
The TCL that the invention provides radix pseudostellariae and hawthorn differentiates that having selected the higher aurantiamarin of content is the assay index, has set up the HPLC content assaying method of digestion-promoting stomachic; Through revision test repeatedly, confirmation method is easy, the result is accurate, can be used as the digestion-promoting stomachic quality control and investigates the index of the stability of technology.
Embodiment
Embodiment 1: get Chinese crude drug radix pseudostellariae 228.6g, dried orange peel 22.9g, Chinese yam 171.4g, Fructus Hordei Germinatus (stir-fry) 171.4g, hawthorn 114.3g, the above-mentioned raw materials five tastes, yam flour is broken into fine powder, four flavor boiling secondaries such as all the other radix pseudostellariaes, each 2 hours, collecting decoction, filter, filtrate cryoconcentration to relative density is the clear cream of 1.08～1.12 (65 ℃), spray drying, it is an amount of to add above-mentioned Chinese yam fine powder, Icing Sugar and dextrin, mixing is made particle, drying, be pressed into 1000 (sheets), every heavy 0.8g; The method of quality control of this medicine comprises the following steps:
(1), measures aurantiamarin (C in this medicine with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000)
28H
34O
15) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; Methyl alcohol--0.5% glacial acetic acid solution (40: 60) is a moving phase, and the detection wavelength is 283nm;
The preparation of b reference substance solution: precision takes by weighing through 48 hours dry aurantiamarin reference substance 12.5mg of phosphorus pentoxide, puts in the 100ml measuring bottle, adds methyl alcohol and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol and is diluted to scale, makes the solution that every 1ml contains 15 μ g;
C. the preparation of need testing solution: get 10 of this product, the accurate title, decided mixing, porphyrize is got 2g, and accurate the title decides, the accurate methyl alcohol 20ml that adds claims to decide weight, puts in the water-bath and refluxes 1 hour, put coldly, claim again to decide weight, supply with methyl alcohol and subtract weight loss, filter, precision is measured subsequent filtrate 5ml and is put in the 10ml measuring bottle, adds water to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, inject liquid chromatograph, the mensuration Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 0.20mg;
(2), this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000):
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 5g, add little the boiling of water and decocted 2 hours, decocting liquid is centrifugal, gets supernatant and passes through D
101Macroporous resin column (internal diameter 1.2cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 of this product, porphyrize adds methyl alcohol 50ml, puts in the water-bath reflux 30 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, passes through D
101Macroporous resin column (internal diameter 1.5cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000): draw each 20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (8: 2) is developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and 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 chromatogram on, show the spot of same color.
(3), this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000)
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 2g, boiling 1 hour, decocting liquid filters, and filtrate is concentrated into 20ml, regulates pH value to 1～2 with watery hydrochloric acid, from " extract 2 times with ethyl acetate; each 20ml merges the ethyl acetate extract, evaporate to dryness; residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 of this product, porphyrize adds methyl alcohol 50ml, put in the water-bath reflux 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with ethyl acetate, each 20ml merges the ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
C. test according to thin-layered chromatography (appendix VIB): draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-formic acid (20: 20: 1) is developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution, and 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 chromatogram on, show the principal spot of same color.
Embodiment 2: get Chinese crude drug radix pseudostellariae 228.6g, dried orange peel 22.9g, Chinese yam 171.4g, Fructus Hordei Germinatus (stir-fry) 171.4g, hawthorn 114.3g, and the above-mentioned raw materials five tastes, yam flour is broken into fine powder, four flavor boiling secondaries such as all the other radix pseudostellariaes, each 2 hours, collecting decoction, filter, filtrate cryoconcentration to relative density is the clear cream of 1.08～1.12 (65 ℃), spray drying, it is an amount of to add above-mentioned Chinese yam fine powder, Icing Sugar and dextrin, mixing is made particle, drying, be pressed into 1600, every heavy 0.5g; The method of quality control of this medicine comprises the following steps:
(1), measures aurantiamarin (C in this medicine with high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000)
28H
34O
15) content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; Methyl alcohol--0.5% glacial acetic acid solution (40: 60) is a moving phase, and the detection wavelength is 283nm;
The preparation of b reference substance solution: precision takes by weighing through 48 hours dry aurantiamarin reference substance 12.5mg of phosphorus pentoxide, puts in the 100ml measuring bottle, adds methyl alcohol and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol and is diluted to scale, makes the solution that every 1ml contains 15 μ g;
C. the preparation of need testing solution: get 10 of this product, the accurate title, decided mixing, porphyrize is got 2g, and accurate the title decides, the accurate methyl alcohol 20ml that adds claims to decide weight, puts in the water-bath and refluxes 1 hour, put coldly, claim again to decide weight, supply with methyl alcohol and subtract weight loss, filter, precision is measured subsequent filtrate 5ml and is put in the 10ml measuring bottle, adds water to scale, shake up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: accurate respectively each the 20 μ l of reference substance solution and need testing solution that draw, inject liquid chromatograph, the mensuration Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin (C
28H
34O
15) meter, must not be less than 0.12mg;
(2), this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000):
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 5g, add little the boiling of water and decocted 2 hours, decocting liquid is centrifugal, gets supernatant and passes through D
101Macroporous resin column (internal diameter 1.2cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 48 of this product, porphyrize adds methyl alcohol 50ml, puts in the water-bath reflux 30 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, passes through D
101Macroporous resin column (internal diameter 1.5cm, long 15cm), water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000): draw each 20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (8: 2) is developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid solution, and 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 chromatogram on, show the spot of same color;
(3), this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000)
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 2g, boiling 1 hour, decocting liquid filters, and filtrate is concentrated into 20ml, regulates pH value to 1～2 with watery hydrochloric acid, from " extract 2 times with ethyl acetate; each 20ml merges the ethyl acetate extract, evaporate to dryness; residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product 48, porphyrize adds methyl alcohol 50ml, put in the water-bath reflux 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with ethyl acetate, each 20ml merges the ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
C. test according to thin-layered chromatography (appendix VIB): draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-formic acid (20: 20: 1) is developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution, and 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 chromatogram on, show the principal spot of same color.
Claims (3)
1. the method for quality control of a digestion-promoting stomachic, wherein said pharmaceutical formulation is made up of Chinese crude drug radix pseudostellariae 228.6g, dried orange peel 22.9g, Chinese yam 171.4g, coloured malt 171.4g, hawthorn 114.3g, above-mentioned raw materials is made 1000 or 1600 altogether, it is characterized in that this method comprises the following steps:
(1), with aurantiamarin C in this medicine of high effective liquid chromatography for measuring
28H
34O
15Content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; Proportioning is the methyl alcohol of 35-45: 55-65--0.5% glacial acetic acid solution is a moving phase, and the detection wavelength is 283 ± 2nm;
The preparation of b reference substance solution: precision takes by weighing the aurantiamarin reference substance 5-25mg through the phosphorus pentoxide drying, puts in the 25-250ml measuring bottle, adds in methyl alcohol or the ethanol any and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol or ethanol or moving phase and is diluted to scale, shakes up, and makes the solution that every 1ml contains 5--50 μ g;
C. the preparation of need testing solution: get this product 5-20 sheet, the accurate title, decided mixing, porphyrize is got 1--3g, and accurate the title decides, accurate any 10--50ml that adds in methyl alcohol or the ethanol claims to decide weight, puts in the water-bath backflow 0.5-2 hour, put coldly, supply with in methyl alcohol or the ethanol any and to subtract weight loss, filter, precision is measured subsequent filtrate 1-25ml and is put in the 5-25ml measuring bottle, adds water or aqueous methanol or hydrous ethanol to scale, shakes up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: accurate respectively reference substance solution and each 5--20 μ l of need testing solution of drawing, inject liquid chromatograph, the mensuration Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin C
28H
34O
15Meter, sheet must not be less than 0.20mg; Small pieces must not be less than 0.12mg;
(2), this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 2-10g, add little the boiling of water and decocted 0.5-3 hour, decocting liquid is centrifugal, gets the D of supernatant by internal diameter 0.5-2cm, long 5-25cm
101Macroporous resin column, water 50-300ml successively, ethanol 50-200ml wash-out discards water elution liquid, collects ethanol eluate, and any 0.5-2ml that evaporate to dryness, residue add in methyl alcohol or the ethanol makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product 20-40 sheet sheet or 40-60 sheet small pieces, porphyrize adds any 25-100ml in methyl alcohol or the ethanol, put in the water-bath reflux 15-60 minute, and filtered the filtrate evaporate to dryness, residue adds water 10-30ml makes dissolving, by the D of internal diameter 0.5-2cm, long 5-25cm
101Macroporous resin column, water 50-300ml successively, ethanol 50-200ml wash-out discards water elution liquid, collects ethanol eluate, and any 0.5-2ml that evaporate to dryness, residue add in methyl alcohol or the ethanol makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography: draw each 5-20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on any thin layer plate in same silica G or GF254 or H, with toluene-ethyl acetate, benzene-ethyl acetate, sherwood oil-ethyl acetate, in normal hexane-ethyl acetate or the cyclohexane-ethyl acetate any is developping agent, the proportioning of two components is 8: 2 or 8: 1 or 9: 2, launch, take out, dry, spray is with 1-5% vanillic aldehyde sulfuric acid or 5-10% 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 chromatogram on, show the spot of same color;
(3), this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 1-5g, boiling 0.5-2 hour, decocting liquid filters, and filtrate is concentrated into 10-50ml, with salt acid for adjusting pH value to 1～3, extract 1-3 time with ethyl acetate, each 10-50ml merges the ethyl acetate extract, evaporate to dryness, any 0.5-2ml that residue adds in methyl alcohol or the ethanol makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get this product 20-40 sheet sheet or 40-60 sheet small pieces, porphyrize adds any 25-100ml in methyl alcohol or the ethanol, put in the water-bath reflux 15-60 minute, filter, filtrate evaporate to dryness, residue add water 10-50ml makes dissolving, extract 1-3 time with ethyl acetate, each 10-50ml merges the ethyl acetate extract, evaporate to dryness, any 0.5-2ml that residue adds in methyl alcohol or the ethanol makes dissolving, as need testing solution;
D. test according to thin-layered chromatography: draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively on any thin layer plate in same silica G or GF254 or H, with cyclohexane-ethyl acetate-formic acid, normal hexane-ethyl acetate-formic acid, sherwood oil-ethyl acetate-formic acid, cyclohexane-ethyl acetate-acetate, normal hexane-ethyl acetate-acetate, in sherwood oil-ethyl acetate-acetate any is developping agent, the proportioning of three components is 19-20: 19-21: 0.2-1.5, launch, take out, dry, spray is with 1-5% ferric trichloride ethanolic 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 control medicinal material chromatogram on, show the principal spot of same color.
2. the method for quality control of digestion-promoting stomachic according to claim 1, it is characterized in that: hydrochloric acid is watery hydrochloric acid or concentrated hydrochloric acid.
3. the method for quality control of digestion-promoting stomachic according to claim 1 is characterized in that this method comprises the following steps:
(1), with aurantiamarin C in this medicine of high effective liquid chromatography for measuring
28H
34O
15Content:
A. chromatographic condition: with octadecylsilane chemically bonded silica is filling agent; Proportioning is 40: 60 a methyl alcohol--0.5% glacial acetic acid solution is a moving phase, and the detection wavelength is 283nm;
B. the preparation of reference substance solution: precision takes by weighing through dry 48 hours aurantiamarin reference substance 12.5mg of phosphorus pentoxide, puts in the 100ml measuring bottle, adds methyl alcohol and makes dissolving and be diluted to scale, shakes up; Accurate amount 3ml puts in the 25ml measuring bottle, adds 50% methyl alcohol and is diluted to scale, shakes up, and makes the solution that every 1ml contains 15 μ g;
C. the preparation of need testing solution: get 10 of this product, the accurate title, decided porphyrize, get 2g, the accurate title, decide, the accurate methyl alcohol 20ml that adds, claim to decide weight, reflux 1 hour is put cold, weight decided in title again, supplies with methyl alcohol to subtract weight loss, filters, precision is measured subsequent filtrate 5ml and is put in the 10ml measuring bottle, adds water to scale, shakes up, filter with 0.45 μ m filter membrane, promptly;
D. Determination of Hesperidin Content assay method: precision is measured reference substance solution and each 20 μ l of need testing solution respectively, injects liquid chromatograph, measures Determination of Hesperidin Content;
E. every contains dried orange peel with aurantiamarin C
28H
34O
15Meter, sheet must not be less than 0.20mg; Small pieces must not be less than 0.12mg;
(2), this medicine Chinese crude drug radix pseudostellariae is differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution: take by weighing radix pseudostellariae control medicinal material 5g, add little the boiling of water and decocted 2 hours, decocting liquid is centrifugal, gets the D of supernatant by internal diameter 1.2cm, long 15cm
101Macroporous resin column, water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 sheets of this product or 48 small pieces, porphyrize adds methyl alcohol 50ml, puts in the water-bath reflux 30 minutes, filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, by the D of internal diameter 1.2cm, long 15cm
101Macroporous resin column, water 200ml successively, ethanol 100ml wash-out discards water elution liquid, collects ethanol eluate, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, makes need testing solution;
C. test according to thin-layered chromatography: draw each 20 μ l of two kinds of solution of above-mentioned control medicinal material and test sample, put respectively on same silica gel g thin-layer plate, with proportioning is that 8: 2 toluene-ethyl acetate is a developping agent, launch, take out, dry, spray is with 1% vanillic aldehyde sulfuric acid, and 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 chromatogram on, show the spot of same color;
(3), this medicine Chinese crude drug hawthorn is differentiated with thin-layered chromatography:
A. the preparation of control medicinal material solution: get hawthorn control medicinal material 2g, boiling 1 hour, decocting liquid filters, and filtrate is concentrated into 20ml, regulates pH value to 1～2 with watery hydrochloric acid, extract 2 times with ethyl acetate, each 20ml merges the ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, makes control medicinal material solution;
B. the preparation of need testing solution: get 30 sheets of this product or 48 small pieces, porphyrize adds methyl alcohol 50ml, put in the water-bath reflux 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with ethyl acetate, each 20ml merges the ethyl acetate extract, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution;
C. test according to thin-layered chromatography: draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with proportioning is that cyclohexane-ethyl acetate-formic acid of 20: 20: 1 is developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution, and 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 chromatogram on, show the principal spot of same color.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100132365A CN1327217C (en) | 2004-05-26 | 2004-05-26 | Quality control of Jianweixiaoshi tablets for promotnig digest |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100132365A CN1327217C (en) | 2004-05-26 | 2004-05-26 | Quality control of Jianweixiaoshi tablets for promotnig digest |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1584586A CN1584586A (en) | 2005-02-23 |
| CN1327217C true CN1327217C (en) | 2007-07-18 |
Family
ID=34600381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100132365A Expired - Lifetime CN1327217C (en) | 2004-05-26 | 2004-05-26 | Quality control of Jianweixiaoshi tablets for promotnig digest |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1327217C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718220B (en) * | 2005-04-26 | 2010-05-12 | 江中药业股份有限公司 | method for discerning tablets of tonifying stomach and promoting digestion |
| CN1830472B (en) * | 2005-12-30 | 2011-02-16 | 江中药业股份有限公司 | Finger print atlas determination method of Chinese medicinal material tangerine peel water extraction |
| CN101396458B (en) * | 2007-09-28 | 2011-06-08 | 北京康仁堂药业有限公司 | Tangerine peel dispensing granule, and preparation method and quality control method thereof |
| CN103055128A (en) * | 2013-02-01 | 2013-04-24 | 山东华信制药集团股份有限公司 | Preparation process of stomach invigorating and digestion helping tablet |
| CN105929056A (en) * | 2016-04-21 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for detecting hesperidin in throat-clearing granule through combination of macroporous resin and HPLC |
| CN110487951A (en) * | 2019-09-20 | 2019-11-22 | 南昌济顺制药有限公司 | A kind of quality determining method of Hedan tablet |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4877744A (en) * | 1987-07-27 | 1989-10-31 | The University Of Kentucky Research Foundation | Qualitative metabolism assessment using high performance thin layer chromatography |
| DE4037686A1 (en) * | 1990-11-27 | 1991-05-16 | Droeschel Stefan Dipl Ing Fh | Quantitative determn. of cocaine and its main metabolites - by thin layer chromatography followed by conversion to a fluorescing prod. by heating |
| CN1419124A (en) * | 2002-12-23 | 2003-05-21 | 北京采瑞医药有限公司 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
| CN1437982A (en) * | 2003-01-29 | 2003-08-27 | 黑龙江省中医研究院 | Medicinal composition for treating mycoplasma pneumonia and preparation method and quality-control method |
| WO2003084945A1 (en) * | 2002-04-10 | 2003-10-16 | Jilin Tianyao Science And Technology Co. Ltd. | An antispastic, analgetic pharmaceutical composition and the preparation method thereof as well as the quality control technique therefor |
-
2004
- 2004-05-26 CN CNB2004100132365A patent/CN1327217C/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4877744A (en) * | 1987-07-27 | 1989-10-31 | The University Of Kentucky Research Foundation | Qualitative metabolism assessment using high performance thin layer chromatography |
| DE4037686A1 (en) * | 1990-11-27 | 1991-05-16 | Droeschel Stefan Dipl Ing Fh | Quantitative determn. of cocaine and its main metabolites - by thin layer chromatography followed by conversion to a fluorescing prod. by heating |
| WO2003084945A1 (en) * | 2002-04-10 | 2003-10-16 | Jilin Tianyao Science And Technology Co. Ltd. | An antispastic, analgetic pharmaceutical composition and the preparation method thereof as well as the quality control technique therefor |
| CN1419124A (en) * | 2002-12-23 | 2003-05-21 | 北京采瑞医药有限公司 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
| CN1437982A (en) * | 2003-01-29 | 2003-08-27 | 黑龙江省中医研究院 | Medicinal composition for treating mycoplasma pneumonia and preparation method and quality-control method |
Non-Patent Citations (6)
| Title |
|---|
| HPLC测定健胃消食片中橙皮苷的含量 田宏等，基层中药杂志，第16卷第6期 2002 * |
| HPLC测定健胃消食片中橙皮苷的含量 田宏等，基层中药杂志，第16卷第6期 2002;对健胃消食片质量标准的补充建议 刘文京，首都医药，第6卷第9期 1999;健胃消食片质量标准的研究 潘翠花，医学理论与实践，第16卷第12期 2003;健胃消食片中橙皮苷，陈皮，山楂的薄层色谱鉴别 朱正顺等，山东医学工业，第19卷第5期 2000;中华人民共和国药典一部 国家药典编委会编，23-24，50，148-149，化学工业出版社 2000 * |
| 中华人民共和国药典一部 国家药典编委会编，23-24，50，148-149，化学工业出版社 2000 * |
| 健胃消食片中橙皮苷，陈皮，山楂的薄层色谱鉴别 朱正顺等，山东医学工业，第19卷第5期 2000 * |
| 健胃消食片质量标准的研究 潘翠花，医学理论与实践，第16卷第12期 2003 * |
| 对健胃消食片质量标准的补充建议 刘文京，首都医药，第6卷第9期 1999 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1584586A (en) | 2005-02-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dashora et al. | Antitumor activity of Dendrophthoe falcata against ehrlich ascites carcinoma in swiss albino mice | |
| CN105477166B (en) | A kind of preparation method and its method of quality control of duhuo jisheng decoction granule | |
| Gao et al. | The flower of Edgeworthia gardneri (wall.) Meisn. suppresses adipogenesis through modulation of the AMPK pathway in 3T3-L1 adipocytes | |
| CN102749401B (en) | Inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation | |
| CN104758515A (en) | Traditional Chinese medicinal composition for treating nephropathy as well as preparation method and detection method thereof | |
| CN1327217C (en) | Quality control of Jianweixiaoshi tablets for promotnig digest | |
| CN114533811A (en) | Traditional Chinese medicine composition with blood sugar reducing effect and preparation method and application thereof | |
| CN104007222A (en) | Method for detecting ephedra-perilla leaf cough relieving capsule | |
| CN114689780A (en) | Multi-component quality detection method for Baoyin decoction extract | |
| CN103412059A (en) | Method for controlling mass of Fuyankang dispersible tablet | |
| CN110441407A (en) | A kind of pool art tablet quality control method | |
| CN101732527B (en) | Quality detection method for liver-soothing granules | |
| CN107102093A (en) | The detection method of compound pellet mattress cream | |
| CN101716270B (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN101793656B (en) | Method for testing decocting rate of traditional Chinese medicine decoction | |
| CN101601821B (en) | Active component content measurement and authentication method for shenfukang tablets | |
| CN101091763B (en) | Method for detection of tonic tablet for essence and blood | |
| CN104950068B (en) | The kidney invigorating is dispeled the wind the quality determining method of climacteric mixture | |
| CN101607037B (en) | Detecting method of lanzhi brain-tranquilizing capsule | |
| CN103487548A (en) | Method for detecting Jinma Gantai preparation for treating hepatitis | |
| CN113759056B (en) | Characteristic spectrum of Chinese lobelia and preparation thereof and construction method thereof | |
| CN101711834A (en) | Method for preparing medicine composition preparation of refined tuber fleeceflower preparation | |
| CN100448476C (en) | Quality control method of Xiaoer Xishi Tablet for improving children appetite | |
| CN107865944A (en) | A kind of clarification process and method of quality control with the pharmaceutical composition for repairing skin barrier effect | |
| CN107669751A (en) | A kind of clarification process and method of quality control of the pharmaceutical composition that there is treatment red blood trace on face to act on |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 330096 Nanchang high tech Zone, Jiangxi Torch Road, No. 788 Patentee after: JIANGZHONG PHARMACEUTICAL Co.,Ltd. Address before: 330077 No. 347, Fuzhou Road, Jiangxi, Nanchang Patentee before: Jiangxi Jiangzhong Pharmaceutical Co.,Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20070718 |
|
| CX01 | Expiry of patent term |