CN115266955A - Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method - Google Patents
Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method Download PDFInfo
- Publication number
- CN115266955A CN115266955A CN202110474978.1A CN202110474978A CN115266955A CN 115266955 A CN115266955 A CN 115266955A CN 202110474978 A CN202110474978 A CN 202110474978A CN 115266955 A CN115266955 A CN 115266955A
- Authority
- CN
- China
- Prior art keywords
- deafness
- capsule
- baicalin
- baicalein
- wogonin
- 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
- 239000002775 capsule Substances 0.000 title claims abstract description 49
- 206010011878 Deafness Diseases 0.000 title claims abstract description 46
- 231100000895 deafness Toxicity 0.000 title claims abstract description 42
- 208000016354 hearing loss disease Diseases 0.000 title claims abstract description 42
- 238000011156 evaluation Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000004615 ingredient Substances 0.000 title description 3
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 claims abstract description 39
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims abstract description 39
- 229960003321 baicalin Drugs 0.000 claims abstract description 39
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- DUAGQYUORDTXOR-GPQRQXLASA-N Gentiopicrin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@H](C=C)C2=CCOC(=O)C2=CO1 DUAGQYUORDTXOR-GPQRQXLASA-N 0.000 claims abstract description 37
- DUAGQYUORDTXOR-WULZUDSJSA-N Gentiopicrin Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1[C@@H](C=C)C=2C(C(=O)OCC=2)=CO1 DUAGQYUORDTXOR-WULZUDSJSA-N 0.000 claims abstract description 37
- 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 claims abstract description 36
- FXNFHKRTJBSTCS-UHFFFAOYSA-N Baicalein Natural products C=1C(=O)C=2C(O)=C(O)C(O)=CC=2OC=1C1=CC=CC=C1 FXNFHKRTJBSTCS-UHFFFAOYSA-N 0.000 claims abstract description 36
- 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 claims abstract description 36
- 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 claims abstract description 36
- HIMJIPRMECETLJ-UHFFFAOYSA-N Wogonin Natural products COc1cc(O)c(O)c2C(=O)C=C(Oc12)c3ccccc3 HIMJIPRMECETLJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- UDFLTIRFTXWNJO-UHFFFAOYSA-N baicalein Chemical compound O1C2=CC(=O)C(O)=C(O)C2=C(O)C=C1C1=CC=CC=C1 UDFLTIRFTXWNJO-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229940015301 baicalein Drugs 0.000 claims abstract description 36
- 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 claims abstract description 36
- 235000001368 chlorogenic acid Nutrition 0.000 claims abstract description 36
- 229940074393 chlorogenic acid Drugs 0.000 claims abstract description 36
- 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 claims abstract description 36
- 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 claims abstract description 36
- XLTFNNCXVBYBSX-UHFFFAOYSA-N wogonin Chemical compound COC1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=CC=C1 XLTFNNCXVBYBSX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000012937 correction Methods 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000013558 reference substance Substances 0.000 claims abstract description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 238000010828 elution Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000741 silica gel Substances 0.000 claims abstract description 4
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 15
- 239000000523 sample Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 239000012488 sample solution Substances 0.000 claims description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000012085 test solution Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012088 reference solution Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 6
- 238000004445 quantitative analysis Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 239000003814 drug Substances 0.000 description 11
- 238000000605 extraction Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 description 4
- 208000004880 Polyuria Diseases 0.000 description 4
- 230000035619 diuresis Effects 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 3
- 241001071795 Gentiana Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 3
- 235000001785 ferulic acid Nutrition 0.000 description 3
- 229940114124 ferulic acid Drugs 0.000 description 3
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 210000004185 liver Anatomy 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 3
- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical compound C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 description 2
- 241000282817 Bovidae Species 0.000 description 2
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 2
- 239000005770 Eugenol Substances 0.000 description 2
- 244000111489 Gardenia augusta Species 0.000 description 2
- IBFYXTRXDNAPMM-BVTMAQQCSA-N Geniposide Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1C(=CC2)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O IBFYXTRXDNAPMM-BVTMAQQCSA-N 0.000 description 2
- IBFYXTRXDNAPMM-FZEIBHLUSA-N Geniposide Natural products COC(=O)C1=CO[C@@H](O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O)[C@H]2[C@@H]1CC=C2CO IBFYXTRXDNAPMM-FZEIBHLUSA-N 0.000 description 2
- MPDGHEJMBKOTSU-UHFFFAOYSA-N Glycyrrhetinsaeure Natural products C12C(=O)C=C3C4CC(C)(C(O)=O)CCC4(C)CCC3(C)C1(C)CCC1C2(C)CCC(O)C1(C)C MPDGHEJMBKOTSU-UHFFFAOYSA-N 0.000 description 2
- 244000303040 Glycyrrhiza glabra Species 0.000 description 2
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 2
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 2
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- QMCLOHXDDPMAMI-UHFFFAOYSA-N alisol B Natural products CC(C)C(=O)C(O)CC(C)C1=C2CC(O)C3C4(C)CCC(=O)C(C)(C)C4CCC3(C)C2(C)CC1 QMCLOHXDDPMAMI-UHFFFAOYSA-N 0.000 description 2
- VGLLGNISLBPZNL-RBUKDIBWSA-N arborescoside Natural products O=C(OC)C=1[C@@H]2C([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)=C(CO)CC2 VGLLGNISLBPZNL-RBUKDIBWSA-N 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 229960003720 enoxolone Drugs 0.000 description 2
- 229960002217 eugenol Drugs 0.000 description 2
- 210000000232 gallbladder Anatomy 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013642 negative control Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940126680 traditional chinese medicines Drugs 0.000 description 2
- KDSWDGKIENPKLB-QJDQKFITSA-N verbascoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC(=O)CCC=2C=C(O)C(O)=CC=2)[C@@H](CO)O[C@@H](OCCC=2C=C(O)C(O)=CC=2)[C@@H]1O KDSWDGKIENPKLB-QJDQKFITSA-N 0.000 description 2
- QFRYQWYZSQDFOS-UHFFFAOYSA-N verbascoside Natural products CC1OC(COC2C(O)C(COC3OC(C(O)C(O)C3O)C(=O)O)OC(Oc4cc(O)cc5OC(=CC(=O)c45)c6ccc(O)c(O)c6)C2O)C(O)C(O)C1O QFRYQWYZSQDFOS-UHFFFAOYSA-N 0.000 description 2
- 241000722953 Akebia Species 0.000 description 1
- 240000008027 Akebia quinata Species 0.000 description 1
- 235000007756 Akebia quinata Nutrition 0.000 description 1
- 241000748223 Alisma Species 0.000 description 1
- 241001083548 Anemone Species 0.000 description 1
- 244000061520 Angelica archangelica Species 0.000 description 1
- 241000213006 Angelica dahurica Species 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 241000721047 Danaus plexippus Species 0.000 description 1
- 206010014020 Ear pain Diseases 0.000 description 1
- 235000018958 Gardenia augusta Nutrition 0.000 description 1
- 235000001287 Guettarda speciosa Nutrition 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 235000017443 Hedysarum boreale Nutrition 0.000 description 1
- 235000007858 Hedysarum occidentale Nutrition 0.000 description 1
- 241000405414 Rehmannia Species 0.000 description 1
- 241000207929 Scutellaria Species 0.000 description 1
- 240000004534 Scutellaria baicalensis Species 0.000 description 1
- 235000017089 Scutellaria baicalensis Nutrition 0.000 description 1
- 208000009205 Tinnitus Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 208000007176 earache Diseases 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 description 1
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 235000011477 liquorice Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002547 new drug Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 231100000886 tinnitus Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Landscapes
- Physics & Mathematics (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)
- Spectroscopy & Molecular Physics (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a method for detecting the content of components in a deafness capsule based on a one-test-multiple evaluation method, which takes baicalin as an internal reference substance to perform one-test-multiple evaluation, establishes relative correction factors of the baicalin and chlorogenic acid, gentiopicrin, baicalein and wogonin, and calculates the content of the chlorogenic acid, the gentiopicrin, the baicalein and the wogonin in the deafness capsule through the relative correction factors. In the detection method, the detection wavelength of the high performance liquid chromatography is 270-290nm, the chromatographic column is a C18 silica gel chromatographic column, and the column temperature is 28-38 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.05 to 0.15 percent phosphoric acid water solution, gradient elution is adopted, and the flow rate is 0.5 to 2ml/min. The invention can well carry out quantitative analysis on the deafness capsule product through one test and multiple evaluations, and provides a basis for comprehensively evaluating the quality standard of the deafness capsule.
Description
Technical Field
The invention belongs to the technical field of medicine detection, and particularly relates to a method for detecting the content of components in a deafness capsule based on a one-test-multiple evaluation method.
Background
The deafness capsule is a Chinese patent medicine prepared by ten Chinese medicinal materials of scutellaria root, gentiana root, akebiaquinata stem, gardenia fruit, licorice root, rehmannia root, alisma tuber, chinese angelica root, irkutsk anemone rhizome and antelope horn according to a production process, is a traditional Chinese medicine preparation which is exclusively produced by Jing Zhong Shanguo medicine (Tangshan) Limited company, has the effects of clearing liver, purging fire, promoting diuresis and freeing orifices, can improve the hearing of patients and improve tinnitus symptoms, and is clinically used for treating earache, pus discharge, dizziness and headache caused by liver and gallbladder damp-heat. In the formula, gentian root, bitter in taste and cold in property, can clear excess fire of liver and gallbladder and promote diuresis and heat, is the monarch drug; scutellaria baicalensis and cape jasmine fruit for eliminating dampness and purging fire[7]The gentian is used as a minister to assist the efficacy of purging fire; the akebia stem is used for assisting in clearing heat and promoting diuresis, and the liquorice is used for regulating the effects of the medicines; the combination of the medicines can play a role in both upper and lower aspects, and has the functions of tonifying, eliminating evil, promoting diuresis, dredging orifices and the like in purgation.
The deafness capsule relates to 10 traditional Chinese medicines, has more complex components, the execution standard of the deafness capsule is loaded in the national food and drug administration (new drug transfer standard) WS3-992 (Z-259) -2007Z, only the baicalin is quantified, and the quantitative determination of a single component is difficult to be used as the evaluation standard of the overall quality of the deafness capsule. Based on the method, the research on the HPLC fingerprint of the deafness capsule and the quantitative analysis of various components in the deafness capsule by adopting a one-test-multiple-evaluation method have important practical significance, and the quality standard of the deafness capsule can be comprehensively controlled and evaluated.
Disclosure of Invention
The invention aims to provide a method for detecting the content of components in a deafness capsule based on a one-measurement-and-multiple-evaluation method, so as to solve the problem that the quantitative determination of a single component is difficult to serve as an evaluation standard of the overall quality of the deafness capsule only by quantifying baicalin in the prior art.
The technical scheme adopted by the invention for realizing the purpose is as follows: a method for detecting the content of components in a deafness capsule based on a one-test-multiple evaluation method is characterized in that baicalin is used as an internal reference to perform one-test-multiple evaluation, relative correction factors of baicalin, chlorogenic acid, gentiopicrin, baicalein and wogonin are established, and the content of the chlorogenic acid, the gentiopicrin, the baicalein and the wogonin in the deafness capsule is calculated through the relative correction factors, and specifically comprises the following steps:
a. collecting the content of the deafness capsule, grinding, extracting with 60-80% ethanol water solution, and filtering to obtain test solution;
b. dissolving chlorogenic acid, gentiopicrin, baicalin, baicalein, and wogonin reference substances in methanol to obtain mixed reference substance solution;
c. detecting the mixed reference substance solution by using a high performance liquid chromatograph, wherein the detection wavelength is 270-290nm, the chromatographic column is a C18 silica gel chromatographic column, and the column temperature is 28-38 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.05-0.15% phosphoric acid water solution, gradient elution is adopted, the flow rate is 0.5-2ml/min, and the gradient elution procedure is as follows: 0-10min, 95% -92% B;10 to 15min,92 to 85% by weight of B; 15-35min, 85 percent B; 35-65min, 85% -70% B; 65-85min, 70% -50% B; 85-95min, 50-30 percent of B;
d. taking baicalin as an internal reference, and respectively calculating relative correction factors of chlorogenic acid, gentiopicrin, baicalein and wogonin according to a formula of fAC = fA/fC = (CA multiplied by AC)/(CC multiplied by AA); wherein, AC is the peak area of an internal reference substance C, CC is the concentration of the internal reference substance C, AA is the peak area of a component A to be detected, and CA is the concentration of the component A to be detected;
e. detecting the sample solution with high performance liquid chromatograph, determining baicalin content in the deafness capsule, with the same chromatographic conditions as in step c, and calculating to obtain chlorogenic acid, gentiopicrin, baicalein, and wogonin content in the deafness capsule according to relative correction factors of baicalin and chlorogenic acid, gentiopicrin, baicalein, and wogonin.
In the step a, the preparation of the test solution is as follows: weighing the content of the deafness capsule, grinding, placing into a conical flask with a plug, adding 75% ethanol water solution, weighing, refluxing for 25-35min, cooling, supplementing 75% ethanol water solution, shaking, and filtering with microporous membrane; wherein, the ratio of the content of the deafness capsule to the added 75% ethanol water solution is 2 g: 20-30mL.
In the step b, the concentrations of chlorogenic acid, gentiopicrin, baicalin, baicalein and wogonin are respectively 0.02-0.03mg/mL, 0.08-0.09mg/mL, 0.3-0.4mg/mL, 0.05-0.07mg/mL and 0.02-0.03mg/mL.
In step C, the detection wavelength is 280nm, the chromatographic column is a Wondasil C18-WR chromatographic column, the mobile phase B is 0.1% phosphoric acid aqueous solution, the column temperature is 35 ℃, and the sample injection amount is 10 mu L.
In the step d, the relative correction factors of the baicalin, the chlorogenic acid, the gentiopicrin, the baicalein and the wogonin are 0.6243, 0.2444, 1.8218 and 1.9965 respectively.
The prescription of the deafness capsule (180 ten thousand capsules) is as follows:
pulverizing radix Angelicae sinensis and cornu Saigae Tataricae into fine powder respectively; extracting the rest eight materials such as radix Gentianae with ethanol under reflux for 2 hr for the first time and 1.5 hr for the second time, mixing the ethanol extractive solutions, filtering, recovering ethanol from the filtrate under reduced pressure, and concentrating to obtain soft extract; decocting the dregs in water twice, the first time lasts for 1.5 hours, the second time lasts for 1 hour, the decoction is combined and filtered, the filtrate is decompressed and concentrated into clear paste with the relative density of 1.30-1.35 (50 ℃), the clear paste is combined with the thick paste, the mixture is stirred evenly and dried in vacuum, the mixture is crushed into fine powder, the fine powder of angelica and antelope horn is added, the mixture is mixed evenly, a proper amount of corn starch and 2 percent of superfine silica gel powder are added, the mixture is mixed evenly and filled into capsules, and the Chinese medicine preparation is obtained.
The traditional Chinese medicine compound preparation related by the invention has more traditional Chinese medicines, the active ingredients are relatively complex, and the quality of the traditional Chinese medicine preparation is difficult to accurately grade only by measuring the content of one active ingredient. The invention can well carry out qualitative and quantitative analysis on the quality of the deafness capsule product by constructing the HPLC fingerprint of the deafness capsule and combining a one-test-multiple-evaluation method, thereby providing a basis for comprehensively evaluating the quality standard of the deafness capsule.
Drawings
FIG. 1 is an HPLC chromatogram of a control and a test. Wherein, 3 chlorogenic acid, 4 gentiopicrin, 5 baicalin, 11 baicalein and 12 wogonin.
FIG. 2 HPLC profile of each negative control. Wherein, 3 chlorogenic acid, 4 gentiopicrin, 5 baicalin, 11 baicalein and 12 wogonin.
Detailed Description
The invention is further illustrated by the following examples, which are given by way of illustration only and are not intended to limit the scope of the invention in any way. In the examples of the present invention, LC-20AT HPLC (Shimadzu corporation, japan); KQ-300DE type numerical control ultrasonic cleaner (ultrasonic instruments, inc. of Kunshan city); a Wondasil C18-WR chromatography column (4.6 mm. Times.250mm, 5 μm); DK-98-II electric constant temperature water bath (Tester instruments, tianjin Co., ltd.); an electronic analytical balance of the ME204E102 type (MettlerToledo, switzerland);
chlorogenic acid (lot No. AF9082001 with a content mass fraction of 98.83%), baicalein (lot No. AF0022325 with a content mass fraction of 98.86%), ferulic acid (lot No. AF20062351 with a content mass fraction of 99.65%), gentiopicroside (lot No. AF9061002 with a content mass fraction of 99.75%), baicalin (lot No. AF20022601 with a content mass fraction of 98.33%), and wogonin (lot No. AF0022331 with a content mass fraction of 98.91%) were purchased from Chengyo Biotech Limited. Batches of deaf capsules 10 (lot numbers 190202, 190802, 20030, 201001, 200901, 190502, 200903, 200302, 200902, 201002) were all from Jing Zhong Shang Yao (Tangshan) Inc.; acetonitrile and phosphoric acid are chromatographically pure, methanol and ethanol are analytically pure, and ultrapure water is adopted for testing.
Example 1
1. Preparation of test solution
Grinding the content of the deafness capsule, precisely weighing 2g, placing in a conical flask with a plug, precisely adding 25mL of 75% ethanol, weighing, refluxing for 30min, cooling, supplementing 75% ethanol, shaking up, collecting the subsequent filtrate, and filtering with 0.45 μm microporous membrane.
2. Preparation of stock solutions of Mixed controls
Precisely weighing appropriate amount of chlorogenic acid, gentiopicrin, baicalin, baicalein, and wogonin, adding methanol to obtain mixed reference stock solutions containing chlorogenic acid, gentiopicrin, baicalin, baicalein, and wogonin at concentrations of 0.0212mg/mL, 0.0827mg/mL, 0.3797mg/mL, 0.0592mg/mL, and 0.0236mg/mL, respectively, filtering, and collecting secondary filtrate.
3. Negative sample solution preparation
Preparing negative samples of radix Scutellariae (containing baicalin, baicalein and wogonin), fructus Gardeniae, radix Angelicae sinensis, rhizoma Acori Graminei (containing chlorogenic acid) and radix Gentianae (containing gentiopicrin) according to the proportion and production process of the formula, taking the contents, grinding, taking 2g, precisely weighing, placing in a conical bottle with a plug, precisely adding 25mL of 75% ethanol, weighing, refluxing for 30min, cooling, supplementing with 75% ethanol, shaking up, taking the subsequent filtrate, and filtering with a 0.45 μm microporous membrane to obtain the product.
4. Chromatographic conditions
A chromatographic column: wondasil C18-WR column (4.6 mm. Times.250mm, 5 μm), column temperature: 35 ℃; mobile phase acetonitrile (A) -0.1% aqueous phosphoric acid (B), gradient elution (0-10min, 95-92% B, 10-15min, 92-85% B, 15-35min, 85-65min, 85-70% B, 85-95min, 70-50% B, 85-95min, 50-30% B; the volume flow is 1.0mL/min; the detection wavelength is 280nm; the amount of the sample was 10. Mu.L.
5. Precision test
Sampling 10 μ L of the mixed reference stock solution, repeating sampling 6 times, and calculating RSD of the peak areas of chlorogenic acid, gentiopicrin, baicalin, baicalein and wogonin to be 0.23%, 0.16%, 0.27%, 0.11% and 0.10%, respectively, which indicates that the precision of the instrument is good.
6. Stability test
Sampling deaf capsule sample solution (batch number 190202) at 0, 4, 8, 12, 16 and 24h respectively according to the chromatographic conditions, calculating peak areas RSD of chlorogenic acid, gentiopicrin, baicalin, baicalein and wogonin to be 1.58%, 1.71%, 1.38%, 1.68% and 0.13%, respectively, and indicating that the sample solution is stable within 24 h.
7. Repeatability test
Taking 6 parts of deafness capsules (batch number 190802), preparing a test solution according to the method in step 1, injecting samples under the chromatographic conditions, and calculating the peak areas RSD of chlorogenic acid, gentiopicroside, baicalin, baicalein and wogonin to be 1.80%, 1.32%, 0.26%, 0.12% and 0.32% respectively, which shows that the method has good repeatability.
8. System adaptability survey
The mixed reference substance, test substance and negative sample solution are injected under the chromatographic conditions, and the results are shown in FIG. 1 and FIG. 2. The peak separation degree of each component chromatogram meets the requirement, the number of theoretical plates is more than 5000, and the negative control has no interference at retention time corresponding to chlorogenic acid, gentiopicroside, baicalin, baicalein and wogonin.
Example 2
Investigation of linear relationships
Precisely sucking 1, 3, 5, 7 and 9 μ L of mixed reference stock solution, respectively, performing sample injection measurement according to the above chromatographic conditions, recording chromatogram, and performing regression treatment with the peak area of each chromatogram as ordinate (Y) and the sample injection amount as abscissa (X), wherein the regression equation and linear range result are shown in Table 5.
Table 5: regression equation and linear relation of each component
Example 3
Sample application recovery test
Taking 0.04g of deaf capsules with determined content (batch number 190802), weighing 6 parts in total, precisely placing the deaf capsules into a 50mL conical flask with a plug, precisely adding 0.0106mg/mL of chlorogenic acid, 0.0414mg/mL of gentiopicroside, 0.1899mg/mL of baicalin, 0.0296mg/mL of baicalein and 0.0118mg/mL of wogonin into 0.5mL of mixed reference stock solution respectively, preparing a sample solution according to the method in example 1, injecting a sample under the chromatographic condition of example 1, recording a chromatogram, and calculating the sample adding recovery rates of the chlorogenic acid, the gentiopicroside, the baicalin, the baicalein and the wogonin, wherein the results are shown in Table 6.
Table 6: result of sample recovery rate of 5 components of deafness capsule
Example 4
Relative correction factor calculation
Precisely sucking 2, 6, 10, 14 and 18 μ L of the mixed control solution, injecting sample under the chromatographic condition of example 1, measuring, taking baicalin as an internal reference, and calculating relative correction factors of chlorogenic acid, gentiopicroside, baicalein and wogonin according to the formula fAC = fA/fC = (CA × AC)/(CC × AA), respectively. Wherein, AC is the peak area of the internal reference substance C, CC is the concentration of the internal reference substance C, AA is the peak area of the component A to be detected, and CA is the concentration of the component A to be detected, and the result is shown in Table 7.
Table 7: relative correction factor of 5 ingredients in deafness capsule
Example 5
Comparing the results of one-test-multiple evaluation with the results of external standard method
10 batches of deafness capsules were taken, a sample solution was prepared according to the method of example 1, samples were injected under the above chromatographic conditions, and the contents of gentiopicrin, chlorogenic acid, baicalein and wogonin were calculated by external standard method and one-test-multiple evaluation method, respectively, and the results are shown in table 8.
Table 8: comparison of external standard method and one-test-multiple evaluation method for determining content of 5 components in deafness capsule
The results of the content determination in table 8 show that the external standard method is substantially consistent with the results of the content determination by the one-test-multiple-evaluation method, which indicates that the one-test-multiple-evaluation method established in the test can be used for determining the content of 5 chemical components including chlorogenic acid, gentiopicroside, baicalin, baicalein and wogonin in the deafness capsules and effectively controlling the quality of the capsules.
Example 6
The influence of different types of chromatographic columns of Thermo Acclaim 120, agilent Eclipse Plus C18 and Wondasil C18-WR 3 (the specification is 4.6mm multiplied by 250mm and 5 mu m), and Waters e2695, agilent 1260 and Shimadzu LC-20A3 on the relative correction factors of each component are examined, and the results are shown in Table 9, and no obvious influence is found (RSD is less than 5%).
Table 9: effect of different instruments, chromatography columns on relative correction factors
Example 7
Index component and internal standard selection
According to the main components and pharmacological action of 10 medicinal materials of the deafness capsule, baicalin, gentiopicrin, 23-acetyl alisol B, geniposide, ferulic acid, baicalein, eugenol, ligustilide, glycyrrhetinic acid, chlorogenic acid, wogonin and verbascoside are investigated in the experiment. Wherein the contents of verbascoside, geniposide, eugenol and ligustilide are too low, and 23-acetyl alisol B, ferulic acid and glycyrrhetinic acid are not easy to extract and analyze, so chlorogenic acid, gentiopicroside, baicalin, baicalein and wogonin are selected as index components. In addition, the baicalin in the test solution has the largest peak area, good peak shape and moderate retention time, so the baicalin is selected as the internal standard.
Example 8 extraction method and chromatographic Condition optimization
The test was conducted according to the method of preparing the test solution of example 1, except that the solvents were extracted with 25%, 50%, 75%, 100% methanol and 25%, 50%, 75%, 100% ethanol, respectively, and as a result, it was found that there was no significant difference in the extraction rates of methanol in different proportions, and that they were all smaller than the extraction contents of ethanol in different proportions, the extraction amount of ethanol in 75% was the highest, and the contents of each component extracted were about twice as much as that of methanol, so that 75% ethanol was selected as the extraction solvent in the most preferable example.
Experiments are carried out according to the preparation method of the test solution in the embodiment 1, except that reflux extraction and ultrasonic extraction are respectively adopted for extraction, and as a result, the reflux extraction content is found to be high, so that the reflux extraction is adopted in the optimal embodiment.
The experiment was carried out under the chromatographic conditions of example 1, except that the detection was carried out at detection wavelengths of 254nm, 280nm and 327nm, respectively, and it was found from the obtained chromatogram that gentiopicroside, baicalin, baicalein and wogonin have the maximum absorption at the detection wavelength of 280nm, chlorogenic acid has the maximum absorption at the detection wavelength of 327, and gentiopicroside has no absorption, and therefore 280nm was selected as the detection wavelength in the most preferred embodiment.
Claims (5)
1. A method for detecting the content of components in a deafness capsule based on a one-test-multiple evaluation method is characterized in that baicalin is used as an internal reference substance to perform one-test-multiple evaluation, relative correction factors of the baicalin, chlorogenic acid, gentiopicrin, baicalein and wogonin are established, and the content of the chlorogenic acid, the gentiopicrin, the baicalein and the wogonin in the deafness capsule is calculated through the relative correction factors, and specifically comprises the following steps:
a. collecting the content of the deafness capsule, grinding, extracting with 60-80% ethanol water solution, and filtering to obtain test solution;
b. dissolving chlorogenic acid, gentiopicrin, baicalin, baicalein, and wogonin reference substances in methanol to obtain mixed reference substance solution;
c. detecting the mixed reference solution by using a high performance liquid chromatograph, wherein the detection wavelength is 270-290nm, the chromatographic column is a C18 silica gel chromatographic column, and the column temperature is 28-38 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.05 to 0.15 percent phosphoric acid water solution, gradient elution is adopted, the flow rate is 0.5 to 2ml/min, and the gradient elution procedure is as follows: 0-10min, 95-92 percent of B;10 to 15min,92 to 85% by weight of B; 15-35min, 85% by weight of B; 35-65min, 85% -70% B; 65-85min, 70% -50% B; 85-95min, 50-30 percent of C;
d. taking baicalin as an internal reference, and respectively calculating relative correction factors of chlorogenic acid, gentiopicrin, baicalein and wogonin according to a formula of fAC = fA/fC = (CA multiplied by AC)/(CC multiplied by AA); wherein, AC is the peak area of an internal reference substance C, CC is the concentration of the internal reference substance C, AA is the peak area of a component A to be detected, and CA is the concentration of the component A to be detected;
e. detecting the sample solution with high performance liquid chromatograph, determining baicalin content in the deafness capsule, with the same chromatographic conditions as in step c, and calculating to obtain chlorogenic acid, gentiopicrin, baicalein, and wogonin content in the deafness capsule according to relative correction factors of baicalin and chlorogenic acid, gentiopicrin, baicalein, and wogonin.
2. The detection method according to claim 1, wherein in the step a, the sample solution is prepared by: weighing the content of the deafness capsule, grinding, placing into a conical flask with a plug, adding 75% ethanol water solution, weighing, refluxing for 25-35min, cooling, supplementing 75% ethanol water solution, shaking, and filtering with microporous membrane; wherein, the ratio of the content of the deafness capsule to the added 75% ethanol water solution is 2 g: 20-30mL.
3. The detection method according to claim 1, wherein in step b, the concentrations of chlorogenic acid, gentiopicroside, baicalin, baicalein, and wogonin are 0.02-0.03mg/mL, 0.08-0.09mg/mL, 0.3-0.4mg/mL, 0.05-0.07mg/mL, and 0.02-0.03mg/mL, respectively.
4. The detection method according to claim 1, wherein in the step C, the detection wavelength is 280nm, the chromatographic column is a Wondasil C18-WR chromatographic column, the mobile phase B is a 0.1% phosphoric acid aqueous solution, the column temperature is 35 ℃, and the sample amount is 10 μ L.
5. The method of claim 1, wherein in step d, the relative correction factors of baicalin to chlorogenic acid, gentiopicrin, baicalein, and wogonin are 0.6243, 0.2444, 1.8218, and 1.9965, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110474978.1A CN115266955A (en) | 2021-04-29 | 2021-04-29 | Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110474978.1A CN115266955A (en) | 2021-04-29 | 2021-04-29 | Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115266955A true CN115266955A (en) | 2022-11-01 |
Family
ID=83746075
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110474978.1A Pending CN115266955A (en) | 2021-04-29 | 2021-04-29 | Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115266955A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116626199A (en) * | 2023-06-01 | 2023-08-22 | 山东宏济堂制药集团股份有限公司 | Method for measuring content of 10 components in Angong bezoar pills |
| CN116818940A (en) * | 2023-06-21 | 2023-09-29 | 河北省中医药科学院 | Method for detecting component content in turbidity-resolving, toxin-resolving and liver-soothing prescription based on one-measurement-multiple-evaluation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017148418A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining component contents of chinese medicine composition |
| CN110907550A (en) * | 2019-11-28 | 2020-03-24 | 健民药业集团股份有限公司 | Method for simultaneously detecting contents of six components in infant lung-ventilating and cough-relieving granules |
| CN111812247A (en) * | 2020-07-23 | 2020-10-23 | 安徽中医药大学第一附属医院(安徽省中医院) | Quality evaluation method of five-flavor capsule for warming, dredging and removing arthralgia |
-
2021
- 2021-04-29 CN CN202110474978.1A patent/CN115266955A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017148418A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining component contents of chinese medicine composition |
| CN110907550A (en) * | 2019-11-28 | 2020-03-24 | 健民药业集团股份有限公司 | Method for simultaneously detecting contents of six components in infant lung-ventilating and cough-relieving granules |
| CN111812247A (en) * | 2020-07-23 | 2020-10-23 | 安徽中医药大学第一附属医院(安徽省中医院) | Quality evaluation method of five-flavor capsule for warming, dredging and removing arthralgia |
Non-Patent Citations (5)
| Title |
|---|
| 代春红 等: "一测多评法同时测定牛黄清感胶囊中5个指标性成分的研究", 《中国药师》, vol. 21, no. 11, pages 2041 - 2044 * |
| 张宏梅;昌盛;崔佰吉;李星梅;冯宪敏;: "HPLC法同时测定茵胆平肝胶囊中6种成分的含量", 中国药房, no. 09 * |
| 王维宁;周清;李虹;王中彦;: "HPLC法同时测定耳聋胶囊中龙胆苦苷和黄芩苷的含量", 中国药事, no. 07 * |
| 郭俊国;毕宏生;宋继科;郭大东;: "龙胆泻肝配方颗粒HPLC-DAD指纹图谱的建立及主要成分含量测定", 时珍国医国药, no. 05 * |
| 黄宝明;陈汀波;鲍涵;林雪颖;张军;赖小平;: "高效液相色谱法测定清感利咽颗粒中绿原酸、龙胆苦苷、葛根素的含量", 环球中医药, no. 04 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116626199A (en) * | 2023-06-01 | 2023-08-22 | 山东宏济堂制药集团股份有限公司 | Method for measuring content of 10 components in Angong bezoar pills |
| CN116818940A (en) * | 2023-06-21 | 2023-09-29 | 河北省中医药科学院 | Method for detecting component content in turbidity-resolving, toxin-resolving and liver-soothing prescription based on one-measurement-multiple-evaluation method |
| CN116818940B (en) * | 2023-06-21 | 2024-05-24 | 河北省中医药科学院 | Method for detecting component content in turbidity-resolving, toxin-resolving and liver-soothing prescription based on one-measurement-multiple-evaluation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105842373B (en) | A method of establishing the finger-print of the pharmaceutical preparation of honeysuckle | |
| CN110412155B (en) | Detection method of HPLC (high performance liquid chromatography) characteristic spectrum of Erdi decoction | |
| CN115266955A (en) | Method for detecting content of ingredients in deafness capsule based on one-test-multiple evaluation method | |
| CN101028388B (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN106290599A (en) | A kind of content assaying method of Chinese medicine composition | |
| CN111624295B (en) | Quality detection method of 'Jihui Tongbiang' capsule | |
| CN104614450A (en) | Fingerprint detection method of Xiaokeqing preparation | |
| CN108020613B (en) | Method for measuring content of menthol in traditional Chinese medicine composition | |
| CN112684036A (en) | Fingerprint spectrum determination method of kidney-tonifying capsules containing leeches and application of fingerprint spectrum determination method | |
| CN101816753B (en) | Method for detecting quality of compound preparation for treating cold | |
| CN109239250B (en) | Method for measuring fingerprint of brain-benefiting heart tablet and standard fingerprint thereof | |
| CN102590423B (en) | Fingerprint spectrum determination method of ligusticum wallichii tea-blending granular preparation | |
| CN114942291A (en) | Method for detecting quality of 'Zhenyang Yangyin' granule | |
| CN110794049B (en) | Detection method of cold granules | |
| CN108614066A (en) | A kind of Traditional Chinese medicine composition detection method for treating coronary heart disease | |
| CN113252826A (en) | HPLC fingerprint detection method of hypnotic brain-nourishing oral liquid | |
| CN103575823A (en) | Detection method of 8 chemical components in Tangminling preparation | |
| CN113484429A (en) | Method for establishing reference of peach pit qi-bearing soup substance | |
| CN113759011A (en) | Method for establishing characteristic spectrum of starwort root and preparation thereof | |
| CN101574477A (en) | Method for controlling quality of menstruation regulation and macula removal tablet | |
| CN111679012B (en) | Preparation method of salvia miltiorrhiza extract and composition thereof | |
| CN114894922B (en) | Detection and quality control method of gynostemma pentaphylla water extract | |
| CN113884585B (en) | Fingerprint of zhengxin Jiangzhi tablet and its application in quality control | |
| CN115308331B (en) | Method for measuring content of 5 ingredients in oldenlandia standard decoction freeze-dried powder or formula granules by adopting one-measurement-multiple-evaluation method | |
| CN115372516B (en) | Method for measuring content of nucleoside components in houttuynia cordata, radix scutellariae and blue mixture intermediate |
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 |