CN110501297A - A kind of quality determining method of radix tetrastigme medicinal material - Google Patents
A kind of quality determining method of radix tetrastigme medicinal material Download PDFInfo
- Publication number
- CN110501297A CN110501297A CN201910676207.3A CN201910676207A CN110501297A CN 110501297 A CN110501297 A CN 110501297A CN 201910676207 A CN201910676207 A CN 201910676207A CN 110501297 A CN110501297 A CN 110501297A
- Authority
- CN
- China
- Prior art keywords
- radix tetrastigme
- medicinal material
- water
- solution
- methanol
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 29
- 229930003944 flavone Natural products 0.000 claims abstract description 45
- 235000011949 flavones Nutrition 0.000 claims abstract description 45
- -1 flavone glycoside Chemical class 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000605 extraction Methods 0.000 claims abstract description 38
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 36
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229930182470 glycoside Natural products 0.000 claims abstract description 29
- 239000013558 reference substance Substances 0.000 claims abstract description 22
- 229930182486 flavonoid glycoside Natural products 0.000 claims abstract description 19
- 150000007955 flavonoid glycosides Chemical class 0.000 claims abstract description 15
- 239000000284 extract Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 12
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 9
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 9
- 238000003556 assay Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 120
- 239000000243 solution Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 19
- 229930187677 Orientoside Natural products 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 14
- 238000002835 absorbance Methods 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 11
- 150000002213 flavones Chemical class 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000012074 organic phase Substances 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000012490 blank solution Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- MHYCRLGKOZWVEF-UHFFFAOYSA-N ethyl acetate;hydrate Chemical compound O.CCOC(C)=O MHYCRLGKOZWVEF-UHFFFAOYSA-N 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000012417 linear regression Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims 2
- 239000012895 dilution Substances 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 14
- 229930003935 flavonoid Natural products 0.000 abstract description 5
- 150000002215 flavonoids Chemical class 0.000 abstract description 5
- 235000017173 flavonoids Nutrition 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007812 deficiency Effects 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000013441 quality evaluation Methods 0.000 abstract description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 18
- 239000004615 ingredient Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- PLAPMLGJVGLZOV-UHFFFAOYSA-N Epi-orientin Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O PLAPMLGJVGLZOV-UHFFFAOYSA-N 0.000 description 5
- PTNJRKBWIYNFSY-UHFFFAOYSA-N Lirinin-O-methyl-ether Natural products COc1ccc-2c(CC3N(C)CCc4cc(OC)c(OC)c-2c34)c1 PTNJRKBWIYNFSY-UHFFFAOYSA-N 0.000 description 5
- RBVAFYCFAFADAG-UHFFFAOYSA-N Orientin Natural products OCC1OC(C(O)c2c(O)cc(O)c3C(=O)C=C(Oc23)c4ccc(O)c(O)c4)C(O)C1O RBVAFYCFAFADAG-UHFFFAOYSA-N 0.000 description 5
- LQSNPVIQIPKOGP-UHFFFAOYSA-N UNPD159785 Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O LQSNPVIQIPKOGP-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- PEFNSGRTCBGNAN-UHFFFAOYSA-N nephrocizin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C=C(C=3C=C(O)C(O)=CC=3)OC2=C1 PEFNSGRTCBGNAN-UHFFFAOYSA-N 0.000 description 5
- PLAPMLGJVGLZOV-VPRICQMDSA-N orientin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O PLAPMLGJVGLZOV-VPRICQMDSA-N 0.000 description 5
- 150000002338 glycosides Chemical class 0.000 description 4
- 230000000144 pharmacologic effect Effects 0.000 description 4
- 150000003648 triterpenes Chemical class 0.000 description 4
- XXLFLUJXWKXUGS-UHFFFAOYSA-N 6-methoxyquinoline-4-carboxylic acid Chemical compound N1=CC=C(C(O)=O)C2=CC(OC)=CC=C21 XXLFLUJXWKXUGS-UHFFFAOYSA-N 0.000 description 3
- 230000000259 anti-tumor effect Effects 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000003810 ethyl acetate extraction Methods 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000341 volatile oil Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 240000008663 Persicaria orientalis Species 0.000 description 2
- JMFSHKGXVSAJFY-UHFFFAOYSA-N Saponaretin Natural products OCC(O)C1OC(Oc2c(O)cc(O)c3C(=O)C=C(Oc23)c4ccc(O)cc4)C(O)C1O JMFSHKGXVSAJFY-UHFFFAOYSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 230000003110 anti-inflammatory effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 230000001568 sexual effect Effects 0.000 description 2
- 150000003431 steroids Chemical class 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 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 description 1
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 1
- RQOCXCFLRBRBCS-UHFFFAOYSA-N (22E)-cholesta-5,7,22-trien-3beta-ol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CCC(C)C)CCC33)C)C3=CC=C21 RQOCXCFLRBRBCS-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 1
- CWVRJTMFETXNAD-GMZLATJGSA-N 5-Caffeoyl quinic acid Natural products O[C@H]1C[C@](O)(C[C@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-GMZLATJGSA-N 0.000 description 1
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 1
- MQVRGDZCYDEQML-UHFFFAOYSA-N Astragalin Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(CO)O2)O)C(=O)C2=C(O)C=C(O)C=C2O1 MQVRGDZCYDEQML-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 1
- 241000345998 Calamus manan Species 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 206010007882 Cellulitis Diseases 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- 241000218202 Coptis Species 0.000 description 1
- 235000002991 Coptis groenlandica Nutrition 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- DNVPQKQSNYMLRS-NXVQYWJNSA-N Ergosterol Natural products CC(C)[C@@H](C)C=C[C@H](C)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)CC[C@]4(C)[C@@H]3CC[C@]12C DNVPQKQSNYMLRS-NXVQYWJNSA-N 0.000 description 1
- 206010017553 Furuncle Diseases 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- OVSQVDMCBVZWGM-IDRAQACASA-N Hirsutrin Natural products O([C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1)C1=C(c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O OVSQVDMCBVZWGM-IDRAQACASA-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
- 108010036012 Iodide peroxidase Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 244000062793 Sorghum vulgare Species 0.000 description 1
- 241001355168 Tetrastigma Species 0.000 description 1
- 241001557415 Tetrastigma hemsleyanum Species 0.000 description 1
- 102000014267 Thyroid peroxidases Human genes 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- MOZJVOCOKZLBQB-UHFFFAOYSA-N Vitexin Natural products OCC1OC(Oc2c(O)c(O)cc3C(=O)C=C(Oc23)c4ccc(O)cc4)C(O)C(O)C1O MOZJVOCOKZLBQB-UHFFFAOYSA-N 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- OVVGHDNPYGTYIT-ROUHPGRKSA-N alpha-L-Rhap-(1->6)-D-Glcp Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)C(O)O1 OVVGHDNPYGTYIT-ROUHPGRKSA-N 0.000 description 1
- FSLPMRQHCOLESF-SFMCKYFRSA-N alpha-amyrin Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C FSLPMRQHCOLESF-SFMCKYFRSA-N 0.000 description 1
- SJMCNAVDHDBMLL-UHFFFAOYSA-N alpha-amyrin Natural products CC1CCC2(C)CCC3(C)C(=CCC4C5(C)CCC(O)CC5CCC34C)C2C1C SJMCNAVDHDBMLL-UHFFFAOYSA-N 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003208 anti-thyroid effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 229940043671 antithyroid preparations Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AJRZXLHOVKRBQW-UHFFFAOYSA-N benzene 1,7,7-trimethylbicyclo[2.2.1]heptan-2-one Chemical compound C1=CC=CC=C1.C12(C(=O)CC(CC1)C2(C)C)C AJRZXLHOVKRBQW-UHFFFAOYSA-N 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 229960004365 benzoic acid Drugs 0.000 description 1
- QXMNTPFFZFYQAI-IMDKZJJXSA-N beta-sitosterol 3-O-beta-D-glucopyranoside Natural products CC[C@H](CC[C@@H](C)[C@H]1CC[C@H]2[C@@H]3CC=C4C[C@H](CC[C@]4(C)[C@H]3CC[C@]12C)O[C@@H]5C[C@H](CO)[C@@H](O)[C@H](O)[C@H]5O)C(C)C QXMNTPFFZFYQAI-IMDKZJJXSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- TWOWSRSKGJSZHZ-VRHDFFKNSA-N bouvardin Chemical compound C1=CC(OC)=CC=C1C[C@H](N(C)C(=O)[C@H](C)NC(=O)[C@H](C)NC(=O)[C@@H](N(C1=O)C)C2)C(=O)N[C@@H](C)C(=O)N(C)[C@H]1[C@@H](O)C(C=C1)=CC=C1OC1=CC2=CC=C1O TWOWSRSKGJSZHZ-VRHDFFKNSA-N 0.000 description 1
- BNOCDYMCAVSRBT-UHFFFAOYSA-N bouvardin Natural products COc1ccc(CC2N(C)C(=O)C(C)NC(=O)C(C)NC(=O)C3Cc4ccc(O)c(Oc5cccc(c5)C(O)C(N(C)C(=O)C(C)NC2=O)C(=O)N3C)c4)cc1 BNOCDYMCAVSRBT-UHFFFAOYSA-N 0.000 description 1
- 108010047824 bouvardin Proteins 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229940074393 chlorogenic acid Drugs 0.000 description 1
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 1
- 235000001368 chlorogenic acid Nutrition 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- NPJICTMALKLTFW-OFUAXYCQSA-N daucosterol Chemical compound O([C@@H]1CC2=CC[C@H]3[C@@H]4CC[C@@H]([C@]4(CC[C@@H]3[C@@]2(C)CC1)C)[C@H](C)CC[C@@H](CC)C(C)C)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O NPJICTMALKLTFW-OFUAXYCQSA-N 0.000 description 1
- QDFKFNAHVGPRBL-UHFFFAOYSA-N daucosterol Natural products CCC(CCC(C)C1CCC2C1CCC3C2(C)CC=C4CC(CCC34C)OC5OC(CO)C(O)C(O)C5O)C(C)C QDFKFNAHVGPRBL-UHFFFAOYSA-N 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- DNVPQKQSNYMLRS-SOWFXMKYSA-N ergosterol Chemical compound C1[C@@H](O)CC[C@]2(C)[C@H](CC[C@]3([C@H]([C@H](C)/C=C/[C@@H](C)C(C)C)CC[C@H]33)C)C3=CC=C21 DNVPQKQSNYMLRS-SOWFXMKYSA-N 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000000273 goitrogenic effect Effects 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 230000002443 hepatoprotective effect Effects 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- GXMWXESSGGEWEM-UHFFFAOYSA-N isoquercitrin Natural products OCC(O)C1OC(OC2C(Oc3cc(O)cc(O)c3C2=O)c4ccc(O)c(O)c4)C(O)C1O GXMWXESSGGEWEM-UHFFFAOYSA-N 0.000 description 1
- MYXNWGACZJSMBT-VJXVFPJBSA-N isovitexin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MYXNWGACZJSMBT-VJXVFPJBSA-N 0.000 description 1
- OYJCWTROZCNWAA-UHFFFAOYSA-N isovitexin Natural products OCC1OC(C(O)C(O)C1O)c2c(O)cc3CC(=CC(=O)c3c2O)c4ccc(O)cc4 OYJCWTROZCNWAA-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- JPUKWEQWGBDDQB-QSOFNFLRSA-N kaempferol 3-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=CC(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O JPUKWEQWGBDDQB-QSOFNFLRSA-N 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 235000019713 millet Nutrition 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- OVSQVDMCBVZWGM-QSOFNFLRSA-N quercetin 3-O-beta-D-glucopyranoside 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-QSOFNFLRSA-N 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- ZYOCVAPRXVCQQR-UHFFFAOYSA-N taraxasterone Natural products CC12CCC(=O)C(C)(C)C1CCC1(C)C2CCC2C3C(C)C(=C)CCC3(C)CCC21C ZYOCVAPRXVCQQR-UHFFFAOYSA-N 0.000 description 1
- GGGUGZHBAOMSFJ-GADYQYKKSA-N taraxerol Chemical compound CC([C@@H]1CC2)(C)[C@@H](O)CC[C@]1(C)[C@@H]1[C@]2(C)C2=CC[C@@]3(C)CCC(C)(C)C[C@H]3[C@]2(C)CC1 GGGUGZHBAOMSFJ-GADYQYKKSA-N 0.000 description 1
- HYTFUKZLSYXRDX-UHFFFAOYSA-N taraxerol Natural products CC1CCCC2C3(C)CCC4(C)C5CC(C)(C)CCC5(C)C=CC4(C)C3C(O)CC12C HYTFUKZLSYXRDX-UHFFFAOYSA-N 0.000 description 1
- DBCAVZSSFGIHQZ-YLAYQGCQSA-N taraxerone Chemical compound CC([C@@H]1CC2)(C)C(=O)CC[C@]1(C)[C@@H]1[C@]2(C)C2=CC[C@@]3(C)CCC(C)(C)C[C@H]3[C@]2(C)CC1 DBCAVZSSFGIHQZ-YLAYQGCQSA-N 0.000 description 1
- FXOCQCYCKZXBIJ-UHFFFAOYSA-N taraxerone Natural products CC1C=C2C(C)(CCC3C4(C)CCC(=O)C(C)(C)C4CCC23C)C5CC(C)(C)CCC15 FXOCQCYCKZXBIJ-UHFFFAOYSA-N 0.000 description 1
- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical compound N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 206010044008 tonsillitis Diseases 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
- 238000004704 ultra performance liquid chromatography Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- SGEWCQFRYRRZDC-VPRICQMDSA-N vitexin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(O)C2=C1OC(C=1C=CC(O)=CC=1)=CC2=O SGEWCQFRYRRZDC-VPRICQMDSA-N 0.000 description 1
- PZKISQRTNNHUGF-UHFFFAOYSA-N vitexine Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C=C(O)C2=C1OC(C=1C=CC(O)=CC=1)=CC2=O PZKISQRTNNHUGF-UHFFFAOYSA-N 0.000 description 1
- 230000002618 waking effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of quality determining methods of radix tetrastigme medicinal material, with general flavone glycoside content in determined by ultraviolet spectrophotometry medicinal material, using the flavone c-glycosides contained in radix tetrastigme as reference substance, it is extracted using high concentration alcohol water system, it is dissolved after being evaporated extracting solution with water, polar organic solvent and water-saturated n-butanol extraction in successively using again, are evaporated the dissolution of extract liquor alcohol-water system to obtain general flavone glycoside, then carry out the assay of general flavone glycoside.This method is easy, easy, reproducible, it can definitely reflect the content of general flavone glycoside in radix tetrastigme medicinal material, the further perfect quality standard of radix tetrastigme medicinal material, it compensates in radix tetrastigme quality evaluation and lacks to using flavonoid glycoside as the deficiency of the detection method of the flavonoids characteristic component of representative, keep the quality detection technology of radix tetrastigme medicinal material more scientific, reasonable.The quality of radix tetrastigme medicinal material can be effectively controlled using detection method of the present invention, so that it is guaranteed that the safety of its clinical application, stability and validity.
Description
Technical field
The invention belongs to pharmaceutical technology fields, and in particular to a kind of quality determining method of radix tetrastigme medicinal material.
Background technique
Radix tetrastigme is Vitaceae Tetrastigma plant tetratigma hemsleyanum (Tetrastigma hemsleyanum Diels et
Gilg), alias gold thread hoist, the flat rattan of three leaves, stone mouse, hemsley rockvine root etc..Herb can be used as medicine, with underground root tuber and fruit
Medicinal effects are best, and Winter Solstice is best in quality to picking during the Waking of Insects (3rd solar term).Radix tetrastigme saves in Zhejiang, Jiangxi, Fujian, Guangxi and Sichuan etc.
Part is distributed, wherein producing the performance optimal of radix tetrastigme with Zhejiang.Radix tetrastigme is referred to as " bouvardin ", medicinal and economic valence
Value is very high, is listed in Rare plant.It is recorded according to Compendium of Material Medica, radix tetrastigme is cool in nature, nontoxic, sweet and slightly bitter taste, has heat-clearing
The effect of removing toxic substances, promoting blood circulation by removing wind.It is usually used in treating children with high fever induced convulsions, children's wind-heat, pneumonia, hepatitis etc., external application is controlled poisonous snake and stung
Wound, tonsillitis, ulcerative carbuncle malignant boil furuncle, cellulitis, traumatic injury etc..Modern pharmacological studies have shown that radix tetrastigme pharmacological action is extensive,
Have the function of antitumor, anti-inflammatory, liver protection and adjusts immune etc..
Pass through literature survey, the main pharmacological components and its feature of radix tetrastigme are as follows:
(1) flavone compound
Flavones and its glycosides compound are the most abundant ingredients of content in radix tetrastigme, are ground in current radix tetrastigme chemical component
Study carefully most element of the first species, and experiment shows it with obvious pharmacological action.
Have determined that the radix tetrastigme flavone compound of structure has more than 20 at present, including flavones and its glycoside
Close object.(Xu Wen, Fu Zhiqin, Lin Jing wait .HPLC-MS/MS method while measuring 10 kinds of flavones ingredients in radix tetrastigme Xu Wen etc.
[J] Acta Pharmaceutica Sinica, 2014,49 (12): 1711-1717.) establish the triple level four bars mass spectrographies surveys of ultra performance liquid chromatography series connection
Determine the content of 4 kinds of ingredients (rutin, isoquercitrin, Kaempferol rutinoside, astragalin) in radix tetrastigme.(Lin Jing's Lin Jing etc. records
Ming younger sister, Huang Zehao, wait radix tetrastigme chemical component and its anti tumor activity in vitro research [J] Chinese Pharmaceutical Journal, 2015,50
(8): 658-663.) 10 flavone compounds are identified in separation in radix tetrastigme herb, wherein apiolin, orientin and different Polygonum orientale
Elements etc. are isolated from the plant for the first time.Fujian University of Traditional Chinese Medicine has applied for the purification side of radix tetrastigme aerial part general flavone
Method (201410648201.2), but non-flavonoid glycoside；Also apply identifying or determining by RRLC-Q-TOF-MS method fast qualitative simultaneously
The patent (201611139156.3) of Main Flavonoids ingredient in amount detection radix tetrastigme leaf.
But the method for the total content of detection radix tetrastigme flavonoid glycoside ingredient is not yet had been reported that at present.For detection method,
Wherein HPLC, HPLC-MS method detect the method for single or several flavonoid glycosides it has been reported that but relatively complicated.With regard to flavonoid
For object, mainly include flavones oxygen glycosides and flavone c-glycoside, wherein flavone c-glycoside in contrast have better structural specificity and
Stability, therefore we have extensively studied the property of flavone c-glycosides, and it is total to establish a kind of determined by ultraviolet spectrophotometry
The method of flavonoid glycoside can carry out general flavone glycoside content detection to radix tetrastigme, study the quality of radix tetrastigme.
(2) phenolic acid compound
Phenolic acid is a kind of widely distributed aromatics secondary metabolite, has a variety of medicines such as anti-inflammatory, anti-oxidant, antitumor
Reason activity.More than 30 phenolic acid compounds are had been found that from radix tetrastigme at present, including phenolic acid compound 5- caffeoyl
Quininic acid, 3-caffeoylquinic acid, 1- caffeoylquinic acids, 5- are to coumaric acyl quininic acid, salicylic acid, benzoic acid, chlorogenic acid, original
Catechuic acid etc., and demonstrate in vitro with antioxidant activity.
(3) triterpene and steroid compound
Triterpenes and steroid are also this kind of life metabolite of plant.The terpene that triterpene is made of 30 carbon atoms
Compound in a free form or is combined into glycosides with sugar and exists in plant.Steroid compound all has ring penta in the structure
The steroid nucleus of the more hydrogen phenanthrene of alkane a pair of horses going side by side, it may have multiple biological activities.The triterpene and steroidal substance isolated from radix tetrastigme at present have
α-amyrin, taraxerone, alnulin, cupreol, ergosterol, 6- oxygen-benzoyl base daucosterol, Hu Luo
Foretell this 7 kinds of glycosides.
Fatty acid and volatile oil
(4) fatty acid and volatile oil are also the chemical component from radix tetrastigme.It can be carried out effectively using GC-MS technology
Identification.The radix tetrastigme fatty acid and volatile oil compositions being reported include: linoleic acid, palmitinic acid, myristic acid, camphor benzene etc..
(5) other compounds
In addition to above-mentioned four classes compound, there are also the ingredients such as polysaccharide, amino acid and microelement in radix tetrastigme.Wherein
Polysaccharide is primarily present in radix tetrastigme root tuber part；Amino acid is present in aerial part more；Micronutrient levels is higher have magnesium,
Iron, manganese, zinc.
In conclusion the flavonoid glycoside characteristic component that the present invention contains in radix tetrastigme, carries out the content of general flavone glycoside
Detection method research.
Radix tetrastigme flavones ingredient is based on flavonoid glycoside, studies have shown that flavonoid glycoside compound also has good pharmacology
Activity, for example, isorientin has significant hepatoprotective effect [30] under the dosage of 15mg/kg, orientin, isorientin have aobvious
Antioxidation (Budzianowski J, Pakulski G, the Robak J.Studies on antioxidative of work
activity of some C-glycosylflavones[J].J Pharmacol Pharm,1991,43(5):395.).It is different
Orientin, orientin, Vitexin have inhibit thyroid peroxidase activity etc. (Gaitan E, Lindsay RH,
Reichert RD,et al.Antithyroid and goitrogenic effects of millet:role of C-
glycosylflavones[J].J Clin Endocrinol Metab,1989,68(4):707.).Flavonoid glycoside, it is especially yellow
Ketone carbon glycosides is the important component that radix tetrastigme plays drug effect.Therefore, we establish using the flavone c-glycoside in radix tetrastigme as standard items
The method of measurement radix tetrastigme general flavone glycoside content will provide important evidence for the control of radix tetrastigme quality.
Summary of the invention
The purpose of the present invention is to provide a kind of detection method of content of general flavone glycoside in radix tetrastigme medicinal material, can be effectively controlled
The quality of radix tetrastigme medicinal material, so that it is guaranteed that the safety of its clinical application, stability and validity.
To achieve the above object, the invention provides the following technical scheme:
A kind of quality determining method of radix tetrastigme medicinal material, with general flavone glycoside content in determined by ultraviolet spectrophotometry medicinal material,
Step includes: flavone c-glycosides to contain in radix tetrastigme as reference substance, is extracted, is evaporated using high concentration alcohol water system
It is dissolved after extracting solution with water, then successively polar organic solvent and water-saturated n-butanol extraction in use, is evaporated extract liquor alcohol water body
Then system's dissolution carries out the assay of general flavone glycoside to obtain general flavone glycoside with direct measuring method at maximum wavelength.
The quality determining method of the radix tetrastigme medicinal material, specific detecting step are as follows:
1) radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, 25mL high concentration alcohol water system is added and returns
Stream extracts 10-60min.After the completion of extraction, filtering is diluted to 25mL with former Extraction solvent.It shakes up, as extracting solution.
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water.With middle polar organic solvent extract 3 times, every time
10mL discards organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase.It is evaporated butanol extraction liquid, is used
80% methanol is redissolved into 10mL volumetric flask, is made into test liquid.
Said extracted with high concentration alcohol water system include but is not limited to concentration be 60%-95% methanol aqueous solution system,
Ethanol water system；Polar organic solvent includes but is not limited to chloroform, methylene chloride, ethyl acetate in above-mentioned extraction use
And their binary mixture.
2) preparation of reference substance solution: precision weighs the flavonoid glycoside compound standard reference material contained in radix tetrastigme, adds
Solution is made in the dissolution of 80% methanol；
Above-mentioned flavonoid glycoside compound standard items including but not limited to contain in the radix tetrastigmes such as orientoside, Lutonaretin
Flavone c-glycosides.
3) measuring method: precision measures 2mL test liquid into 5mL volumetric flask, is sky with 80% methanol with 80% methanol constant volume
White reference solvent；Using ultraviolet spectrophotometry, the absorbance at 336nm wavelength is tested, blank solution is noiseless；Use standard
Curve method calculates content.
As the further refinement scheme of the present invention: specific detecting step is as follows:
1) radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, 80% methanol of 25mL is added, reflux mentions
Take 30min.After the completion of extraction, filtering is diluted to 25mL with former Extraction solvent.It shakes up, as extracting solution.
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water.It is saturated with water ethyl acetate extraction 3 times, every time
10mL discards organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase.It is evaporated butanol extraction liquid, is used
80% methanol is redissolved into 10mL volumetric flask, is made into test liquid.
2) preparation of reference substance solution: precision weighs orientoside reference substance 0.0016g, is diluted to 80% methanol (50mL)
The solution of 0.032mg/mL；Precision measures orientoside reference substance solution 1,1.5,2,2.5,3,3.5mL, is separately added into 5mL capacity
In bottle, constant volume measures standard curve to get reference substance solution.
3) measuring method: precision measures 2mL test liquid into 5mL volumetric flask, is sky with 80% methanol with 80% methanol constant volume
White reference solvent；Using ultraviolet spectrophotometry, the absorbance at 336nm wavelength is tested, blank solution is noiseless；Use standard
Curve method calculates content, and using absorbance as ordinate Y, orientoside concentration is that abscissa X carries out linear regression, acquires regression equation
Formula is y=37.277x-0.002, and coefficient R 2=0.9985, concentration is in 0.0064mg/mL-0.0224mg/mL range interior lines
Sexual intercourse is good.
The flavone c-glycosides reference substance contained in radix tetrastigme described in the method for the present invention includes but is not limited to Polygonum orientale
The flavone c-glycoside contained in glycosides, Lutonaretin radix tetrastigme.The extraction includes but is not limited to that concentration is with high concentration alcohol water system
The methanol aqueous solution system and ethanol water system of 60%-95%；The middle polar organic solvent includes but is not limited to trichlorine
Methane, methylene chloride, ethyl acetate.
Detection method learns verifying by the methods of precision, repeatability, sample-adding recycling, it was demonstrated that is a kind of easy
Measure the effective ways of general flavone glycoside in radix tetrastigme.Compared with prior art, the beneficial effects of the present invention are: it is easy, easy, again
Renaturation is good, can definitely reflect radix tetrastigme quality of medicinal material, and the further perfect quality standard of radix tetrastigme medicinal material compensates for three leaves
Lack in green quality evaluation to using flavonoid glycoside as the deficiency of the detection method of the characteristic component of representative, makes the quality of radix tetrastigme medicinal material
Detection technique is more scientific, reasonable；The quality of radix tetrastigme medicinal material can be effectively controlled, so that it is guaranteed that the safety of its clinical application, steady
Qualitative and validity.
Detailed description of the invention
Fig. 1 is orientoside canonical plotting.
Specific embodiment
Below in conjunction with drawings and examples, technical solution of the present invention is clearly and completely described, it is clear that retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those of ordinary skill every other embodiment obtained without making creative work, belongs to the present invention
The range of protection.
Embodiment 1: extracting method is investigated to be investigated with coloration method
Radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, 25mL solvent is added.Solvent is respectively
Two kinds of 80% methanol, water.Extracting method is respectively that ultrasound 30min, reflux 30min extract two kinds.4 kinds of samples of total preparation.Tool
Body solvent and extracting method distribution are shown in Table 1,2.After the completion of extraction, filtering is diluted to 25mL with former Extraction solvent, is extracted
Liquid.
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water.It is saturated with water ethyl acetate extraction 3 times, every time
10mL discards organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase.It is evaporated butanol extraction liquid, is used
80% methanol is redissolved into 10mL volumetric flask, is made into test liquid.
The direct method of measurement: scanning measures under the absorbing wavelength after obtaining maximum absorption wavelength.
Triethylamine set process: taking reference substance solution 0.5mL, is placed in 5mL volumetric flask, adds Extraction solvent 2mL, with 1% triethylamine
Constant volume shakes up.Using reagent blank as reference, absorbance is measured in 400nm.
Result is extracted as shown in table 1,2
1 direct measuring method of table measures Different Extraction Method flavonoid glycoside content
2 triethylamine set process of table measures Different Extraction Method flavonoid glycoside content
Triethylamine set process and direct measuring method result compare, and show: the result of two kinds of measuring methods is illustrated as flowing back
It extracts compared with ultrasonic extraction, flavonoid glycoside content obtained by refluxing extraction is higher；Compared with water, water is as solvent extraction for 80% methanol
Gained flavonoid glycoside content is higher.
Two methods comparison, triethylamine set process are not necessarily to complicated pre-treatment, extracting solution almost free of losses；And direct measuring method needs
The pre-treatment steps such as extraction, may cause content during the experiment has loss.But measurement result, the content of direct measuring method
Measurement result is above triethylamine set process.General flavone glycoside assay is carried out using direct measuring method so determining.
In an experiment it has also been found that, when solvent is water, no matter refluxing extraction or ultrasonic extraction, the stickiness of extracting solution all compares
Greatly.Supposition may be to have polysaccharide component to extract in extraction process.It will do it relatively slowly in filter process in this way, also have one
A little losses, cause the general flavone glycoside content finally measured and actual value relatively low.When solvent is aqueous methanol, extracting solution was easy to
Filter is solvent compared to water, and loss can be smaller, and the content value of measurement is also relatively accurate.
Embodiment 2: the selection of wavelength is measured
By full wavelength scanner, a length of 341nm of maximum absorption wave of orientoside reference substance is obtained, four kinds of extracting methods obtain
The maximum absorption wavelength of test liquid be followed successively by 325nm, 331nm, 336nm, 340nm.By inspection information, obtain in radix tetrastigme
The maximum absorption wavelength of some flavonoid glycosides, if a length of 336nm of the maximum absorption wave of Vitexina, Saponaretin is (in the Chinese Academy of Sciences
Extra large institute of materia medica's fitochemical studies room Beijing flavonoids identification handbook [M]: Science Press, 1981:399-
401.).Therefore select wavelength of the 336nm as measurement content when.
Embodiment 3: the selection of extractant
According to Literature Consult, discovery extracts flavones and water-saturated n-butanol is used to carry out depth extraction to flavones aqueous solution mostly
To obtain the higher flavones of purity.Removal oil-soluble impurities such as aglycon generally has ethyl acetate, chloroform, methylene chloride etc..Cause
This, polar organic solvent extracts in, discards organic phase；It is saturated with water extracting n-butyl alcohol again, discards water phase, is evaporated extract liquor use
Alcohol-water system is dissolved to obtain general flavone glycoside.
The TLC of three kinds of different solvents extraction is observed as a result, display can remove the low organic interference of polarity in most
Ingredient.
Extraction times are equally probed into, and will be extracted obtained organic layer and directly be put on silica gel plate, are developed the color, observation
Whether contain Flavonoid substances, if so, then continuing to extract, determines that extraction times are 3 times.
Embodiment 4: methodological study
4.1 Precision Experiment
Accurately weighed radix tetrastigme sample 1g extracts 30min with 80% methanol eddy of 25mL.Extracting solution is accurate by processing
2mL is pipetted into 5mL volumetric flask, with 80% methanol constant volume, using 80% methanol as reference, the duplicate measurements absorbance at 336nm
Value 6 times, general flavone glycoside content is calculated, calculated result is as shown in table 3, calculates to obtain relative standard deviation=0.26%, shows instrument essence
Density is good.
3 direct measuring method instrument precision experimental result of table
4.2 repeated experiment
5 parts of radix tetrastigme sample are taken, every part of 1g is accurately weighed.30min is extracted with 80% methanol eddy of 25mL.Extracting solution warp
Processing is crossed, precision pipettes 2mL into 5mL volumetric flask, is measured at 336nm with 80% methanol constant volume using 80% methanol as reference
Absorbance value, calculates general flavone glycoside content, and calculated result is as shown in table 4.In the method for extracting 30min using 80% methanol eddy
When extraction, the average content of radix tetrastigme general flavone glycoside is 0.747mg/g, RSD=1.24%, illustrates that the repeatability of this method is good
It is good.
4 repetitive test result of table
4.3 stability experiment
Accurately weighed radix tetrastigme sample 1g extracts 30min with 80% methanol eddy of 25mL.Extracting solution is accurate by processing
2mL is pipetted into 5mL volumetric flask, with 80% methanol constant volume, using 80% methanol as reference, at 336nm respectively 0,0.5,1,2,
Absorbance is measured when 3h, calculates general flavone glycoside content, and calculated result is shown in Table 5.RSD=0.52% illustrates good in 3h internal stability
It is good.
5 stability experiment result of table
4.4 sample-adding recovery experiments
6 parts of radix tetrastigme sample are taken, every part of 1g is accurately weighed, and it is appropriate to be separately added into orientin standard substance.With 80% first of 25mL
Alcohol reflux extracts 30min.After extracting solution is handled, precision pipettes 1mL into 5mL volumetric flask, with 80% methanol constant volume, with
80% methanol is reference, measures absorbance at 336nm, calculates general flavone glycoside content.It the results are shown in Table 6.Sample recovery rate average value
For 100.3%, RSD=2.98%.
Table 6 is loaded recovery test
Embodiment 5: content assaying method
1) radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, 80% methanol of 25mL is added, reflux mentions
Take 30min.After the completion of extraction, filtering is diluted to 25mL with former Extraction solvent.It shakes up, as extracting solution.
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water.It is saturated with water ethyl acetate extraction 3 times, every time
10mL discards organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase.It is evaporated butanol extraction liquid, is used
80% methanol is redissolved into 10mL volumetric flask, is made into test liquid.
2) preparation of reference substance solution: precision weighs orientoside reference substance 0.0016g, is diluted to 80% methanol (50mL)
The solution of 0.032mg/mL；Precision measures orientoside reference substance solution 1,1.5,2,2.5,3,3.5mL, is separately added into 5mL capacity
In bottle, constant volume measures standard curve to get reference substance solution.
3) measuring method: precision measures 2mL test liquid into 5mL volumetric flask, is sky with 80% methanol with 80% methanol constant volume
White reference solvent；Using ultraviolet spectrophotometry, the absorbance at 336nm wavelength is tested, blank solution is noiseless；Use standard
Curve method calculates content, and using absorbance as ordinate Y, orientoside concentration is that abscissa X carries out linear regression, acquires regression equation
Formula is y=37.277x-0.002, and coefficient R 2=0.9985, concentration is in 0.0064mg/mL-0.0224mg/mL range interior lines
Sexual intercourse is good.
The present invention is easy, easy, reproducible, can definitely reflect radix tetrastigme quality of medicinal material, further perfect three leaves
The quality standard of green medicinal material compensates for the detection lacked in radix tetrastigme quality evaluation to the ingredient characterized by flavonoid glycoside compound
The deficiency of method keeps the quality detection technology of radix tetrastigme medicinal material more scientific, reasonable；The quality of radix tetrastigme medicinal material can be effectively controlled,
So that it is guaranteed that the safety of its clinical application, stability and validity.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (5)
1. a kind of quality determining method of radix tetrastigme medicinal material, which is characterized in that ultraviolet spectrophotometry is used, to contain in radix tetrastigme
Some flavone c-glycosides are reference substance, are extracted using high concentration alcohol water system, are dissolved after being evaporated extracting solution with water, then according to
Polar organic solvent and water-saturated n-butanol extraction, are evaporated butanol extraction liquid in secondary use, are dissolved with alcohol-water system total to obtain
Then flavonoid glycoside carries out the assay of radix tetrastigme medicinal material general flavone glycoside with direct measuring method at maximum wavelength.
2. a kind of quality determining method of radix tetrastigme medicinal material according to claim 1, which is characterized in that specific detecting step
It is as follows:
1) radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, the reflux of 25mL high concentration alcohol water system is added and mentions
10-60min is taken, after the completion of extraction, filtering is diluted to 25mL with former Extraction solvent, shakes up, as extracting solution；
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water, and polar organic solvent extracts 3 times, each 10mL in, abandons
Go organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase.It is evaporated butanol extraction liquid, with 80% first
Alcohol is redissolved into 10mL volumetric flask, is made into test liquid；
2) preparation of reference substance solution: precision weighs orientoside reference substance 0.0016g, with 80% methanol dilution at 0.032mg/mL
Solution；
3) measuring method: precision measures 2mL test liquid into 5mL volumetric flask, with 80% methanol constant volume, joins by blank of 80% methanol
Compare solvent；Using ultraviolet spectrophotometry, the absorbance at 336nm wavelength is tested, blank solution is noiseless；Use standard curve
Method calculates content.
3. a kind of quality determining method of radix tetrastigme medicinal material according to claim 2, which is characterized in that specifically detect
Steps are as follows:
1) radix tetrastigme root tuber drying and crushing is taken, 60 meshes is crossed, takes 1g accurately weighed, 25mL80% methanol, refluxing extraction is added
30min, after the completion of extraction, filtering is diluted to 25mL with former Extraction solvent, shakes up, as extracting solution；
Precision measures 10mL extracting solution, is evaporated, and is redissolved with 10mL water.It is saturated with water ethyl acetate to extract 3 times, each 10mL, abandon
Go organic phase；It is saturated with water again extracting n-butyl alcohol 3 times, each 10mL discards water phase, is evaporated butanol extraction liquid, with 80% first
Alcohol is redissolved into 10mL volumetric flask, is made into test liquid；
2) preparation of reference substance solution: precision weighs orientoside reference substance 0.0016g, with 50mL80% methanol dilution at
The solution of 0.032mg/mL；Precision measures orientoside reference substance solution 1,1.5,2,2.5,3,3.5mL, is separately added into 5mL capacity
In bottle, constant volume measures standard curve to get reference substance solution；
3) measuring method: precision measures 2mL test liquid into 5mL volumetric flask, with 80% methanol constant volume, joins by blank of 80% methanol
Compare solvent；Using ultraviolet spectrophotometry, the absorbance at 336nm wavelength is tested, blank solution is noiseless；Use standard curve
Method calculates content, and using absorbance as ordinate Y, orientoside concentration is that abscissa X carries out linear regression, and acquiring regression equation is
Y=37.277x-0.002, coefficient R2=0.9985, concentration is linearly closed within the scope of 0.0064mg/mL-0.0224mg/mL
System is good.
4. a kind of quality determining method of radix tetrastigme medicinal material according to claims 1 and 2, which is characterized in that three leaf
The flavones that the flavone c-glycosides reference substance contained in blueness includes but is not limited to orientoside, is contained in Lutonaretin radix tetrastigme
Carbon glycosides.
5. a kind of quality determining method of radix tetrastigme medicinal material according to claims 1 and 2, which is characterized in that the extraction
It include but is not limited to the methanol aqueous solution system and ethanol water system that concentration is 60%-95% with high concentration alcohol water system；
The middle polar organic solvent includes but is not limited to chloroform, methylene chloride, ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910676207.3A CN110501297A (en) | 2019-07-25 | 2019-07-25 | A kind of quality determining method of radix tetrastigme medicinal material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910676207.3A CN110501297A (en) | 2019-07-25 | 2019-07-25 | A kind of quality determining method of radix tetrastigme medicinal material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110501297A true CN110501297A (en) | 2019-11-26 |
Family
ID=68586983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910676207.3A Pending CN110501297A (en) | 2019-07-25 | 2019-07-25 | A kind of quality determining method of radix tetrastigme medicinal material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110501297A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466224A (en) * | 2021-06-30 | 2021-10-01 | 中国科学院宁波材料技术与工程研究所慈溪生物医学工程研究所 | Array sensor for identifying radix tetrastigme producing area and preparation method and application thereof |
| CN113720931A (en) * | 2021-08-19 | 2021-11-30 | 遂昌县森林王中药材专业合作社 | Quality evaluation method of radix tetrastigme medicinal material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001051482A1 (en) * | 2000-01-11 | 2001-07-19 | Biorex Health Limited | Extraction of flavonoids |
| CN101732392A (en) * | 2009-12-21 | 2010-06-16 | 中国科学院长春应用化学研究所 | Method for inspecting quality of indigowoad leaf Chinese medicament |
| CN104237151A (en) * | 2014-10-14 | 2014-12-24 | 宁波枫康生物科技有限公司 | Mass detection method for dendrobium officinale medicine |
| CN104458627A (en) * | 2014-12-08 | 2015-03-25 | 敖云霞 | Method for determining content of total flavones in polygonum oriental extract |
| CN104922196A (en) * | 2015-06-30 | 2015-09-23 | 广西壮族自治区中医药研究院 | General ohwia flavone extract preparation method and general ohwia flavone extract quality detecting method |
| CN110044832A (en) * | 2019-03-11 | 2019-07-23 | 广西中医药大学 | The measuring method of general flavone content in a kind of semen litchi |
-
2019
- 2019-07-25 CN CN201910676207.3A patent/CN110501297A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001051482A1 (en) * | 2000-01-11 | 2001-07-19 | Biorex Health Limited | Extraction of flavonoids |
| CN101732392A (en) * | 2009-12-21 | 2010-06-16 | 中国科学院长春应用化学研究所 | Method for inspecting quality of indigowoad leaf Chinese medicament |
| CN104237151A (en) * | 2014-10-14 | 2014-12-24 | 宁波枫康生物科技有限公司 | Mass detection method for dendrobium officinale medicine |
| CN104458627A (en) * | 2014-12-08 | 2015-03-25 | 敖云霞 | Method for determining content of total flavones in polygonum oriental extract |
| CN104922196A (en) * | 2015-06-30 | 2015-09-23 | 广西壮族自治区中医药研究院 | General ohwia flavone extract preparation method and general ohwia flavone extract quality detecting method |
| CN110044832A (en) * | 2019-03-11 | 2019-07-23 | 广西中医药大学 | The measuring method of general flavone content in a kind of semen litchi |
Non-Patent Citations (2)
| Title |
|---|
| 范世明等: "三叶青叶化学成分鉴定及其总黄酮含量测定研究", 《药物分析杂志》 * |
| 郭力等: "《中药化学 供中药学、药学及相关专业使用》", 31 August 2015 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113466224A (en) * | 2021-06-30 | 2021-10-01 | 中国科学院宁波材料技术与工程研究所慈溪生物医学工程研究所 | Array sensor for identifying radix tetrastigme producing area and preparation method and application thereof |
| CN113466224B (en) * | 2021-06-30 | 2024-05-14 | 宁波慈溪生物医学工程研究所 | Array sensor for identifying origin of radix tetrastigme, and preparation method and application thereof |
| CN113720931A (en) * | 2021-08-19 | 2021-11-30 | 遂昌县森林王中药材专业合作社 | Quality evaluation method of radix tetrastigme medicinal material |
| CN113720931B (en) * | 2021-08-19 | 2023-10-20 | 遂昌县森林王中药材专业合作社 | Quality evaluation method of radix tetrastigme medicinal material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105467059B (en) | A kind of quality determining method for the Chinese medicine composition for treating blood urine | |
| CN107843677A (en) | Radix paeoniae rubrathe reference extract and its preparation method and application | |
| Panichayupakarananta et al. | Antioxidant assay-guided purification and LC determination of ellagic acid in pomegranate peel | |
| CN107505405B (en) | Method for efficiently and rapidly extracting and measuring flavonoid pigment in Chinese rose petals | |
| Abourashed et al. | High-speed extraction and HPLC fingerprinting of medicinal plants–I. Application to Passiflora flavonoids | |
| CN109239224B (en) | Method for simultaneously and quantitatively measuring 9 blood-entering components in spina date seed water extract | |
| CN107607649B (en) | Method for detecting periploca forrestii schltr | |
| CN104922196B (en) | The preparation of small pagodatree flower general flavone extract and quality determining method | |
| Zheng et al. | Identification of acetylcholinesterase inhibitors from seeds of plants of genus Peganum by thin-layer chromatography-bioautography | |
| CN110501297A (en) | A kind of quality determining method of radix tetrastigme medicinal material | |
| CN107843657A (en) | The quality determining method of TONGXIAO BIYAN PIAN | |
| CN109444290A (en) | The construction method and detection method of Asiatic plantain medicinal material UPLC characteristic spectrum | |
| Wei et al. | An ultra high performance liquid chromatography with tandem mass spectrometry method for simultaneous determination of thirteen components extracted from Radix Puerariae in rat plasma and tissues: Application to pharmacokinetic and tissue distribution study | |
| Wen et al. | A validated UV-HPLC method for determination of chlorogenic acid in Lepidogrammitis drymoglossoides (Baker) Ching, Polypodiaceae | |
| CN110231412A (en) | The detection method of saponin content in gynostemma pentaphylla | |
| CN110361346A (en) | A kind of quality determining method of dendrobium candidum medicinal material | |
| Yue et al. | Determination of gallic acid and salidroside in Rhodiola and its preparation by capillary electrophoresis | |
| CN115575541A (en) | Method for simultaneously determining multiple active ingredients in Yinhuang Erchen mixture | |
| CN110687219B (en) | Detection method of suhuang cough-relieving capsule fingerprint and application thereof | |
| CN102495168B (en) | Day lily flower and method for detecting day lily flower preparation | |
| Niu et al. | Development of a method to screen and isolate xanthine oxidase inhibitors from black bean in a single step: Hyphenation of semipreparative liquid chromatography and stepwise flow rate countercurrent chromatography | |
| Niu et al. | Simultaneous analysis of eight phenolic compounds in Phyllanthus simplex Retz by HPLC-DAD-ESI/MS | |
| Chen et al. | Determination of flavonoids in the flowers of Paulownia tomentosa by high-performance liquid chromatography | |
| Sun et al. | The overall quality control of Radix scutellariae by capillary electrophoresis fingerprint | |
| Liu et al. | Determination of flavonoids in Tibetan herbal medicine of Pyrethrum tatsienense by HPLC with photodiode array detection |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20191126 |