CN106525997B - A method of organic acid and flavones ingredient in measurement serpentgrass - Google Patents
A method of organic acid and flavones ingredient in measurement serpentgrass Download PDFInfo
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- CN106525997B CN106525997B CN201610842261.7A CN201610842261A CN106525997B CN 106525997 B CN106525997 B CN 106525997B CN 201610842261 A CN201610842261 A CN 201610842261A CN 106525997 B CN106525997 B CN 106525997B
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- 235000012804 Polygonum viviparum Nutrition 0.000 title claims abstract description 41
- 241000118324 Bistorta vivipara Species 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000004615 ingredient Substances 0.000 title claims abstract description 30
- 229930003944 flavone Natural products 0.000 title claims abstract description 18
- 150000002213 flavones Chemical class 0.000 title claims abstract description 18
- 235000011949 flavones Nutrition 0.000 title claims abstract description 18
- 150000007524 organic acids Chemical class 0.000 title claims abstract description 17
- 238000005259 measurement Methods 0.000 title claims description 12
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000243 solution Substances 0.000 claims abstract description 64
- 239000013558 reference substance Substances 0.000 claims abstract description 50
- 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 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 35
- 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 35
- 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 35
- 235000001368 chlorogenic acid Nutrition 0.000 claims abstract description 35
- 229940074393 chlorogenic acid Drugs 0.000 claims abstract description 35
- 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 35
- 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 35
- 235000004515 gallic acid Nutrition 0.000 claims abstract description 35
- 229940074391 gallic acid Drugs 0.000 claims abstract description 35
- 239000012085 test solution Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 72
- 238000004458 analytical method Methods 0.000 claims description 12
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 10
- 238000004445 quantitative analysis Methods 0.000 claims description 9
- 239000000470 constituent Substances 0.000 claims description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 7
- 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 claims description 6
- LKZDFKLGDGSGEO-UJECXLDQSA-N kaempferol 3-O-beta-D-glucosyl-(1->2)-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O[C@H](CO)[C@@H](O)[C@@H]1O LKZDFKLGDGSGEO-UJECXLDQSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001819 mass spectrum Methods 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000011156 evaluation Methods 0.000 claims description 5
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000011088 calibration curve Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004949 mass spectrometry Methods 0.000 claims description 4
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims description 3
- PFTAWBLQPZVEMU-ZFWWWQNUSA-N (+)-epicatechin Natural products C1([C@@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-ZFWWWQNUSA-N 0.000 claims description 3
- PFTAWBLQPZVEMU-UKRRQHHQSA-N (-)-epicatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-UKRRQHHQSA-N 0.000 claims description 3
- LKZDFKLGDGSGEO-UHFFFAOYSA-N 2',8-Di-Me ether,7-O-beta-D-glucuronoside-2',5,7,8-Tetrahydroxyflavone Natural products OC1C(O)C(O)C(CO)OC1OC1C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)OC(CO)C(O)C1O LKZDFKLGDGSGEO-UHFFFAOYSA-N 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 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 claims description 3
- 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 claims description 3
- NRSUOHVIKLCXEE-UHFFFAOYSA-N Isorhamnetin 3-O-beta-D-glucopyranoside Natural products CCC1OC(OC2=C(Oc3cc(O)cc(O)c3C2=O)c4ccc(O)c(OC)c4)C(O)C(O)C1O NRSUOHVIKLCXEE-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- HIWPGCMGAMJNRG-ACCAVRKYSA-N Sophorose Natural products O([C@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HIWPGCMGAMJNRG-ACCAVRKYSA-N 0.000 claims description 3
- HIWPGCMGAMJNRG-UHFFFAOYSA-N beta-sophorose Natural products OC1C(O)C(CO)OC(O)C1OC1C(O)C(O)C(O)C(CO)O1 HIWPGCMGAMJNRG-UHFFFAOYSA-N 0.000 claims description 3
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000005487 catechin Nutrition 0.000 claims description 3
- 229950001002 cianidanol Drugs 0.000 claims description 3
- 238000001360 collision-induced dissociation Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 150000002116 epicatechin Chemical class 0.000 claims description 3
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 claims description 3
- 235000012734 epicatechin Nutrition 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 229930182470 glycoside Natural products 0.000 claims description 3
- 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 claims description 3
- CQLRUIIRRZYHHS-LFXZADKFSA-N isorhamnetin 3-O-beta-D-glucopyranoside Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=C1 CQLRUIIRRZYHHS-LFXZADKFSA-N 0.000 claims description 3
- 235000008777 kaempferol Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 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 claims description 3
- 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 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- QJVXKWHHAMZTBY-GCPOEHJPSA-N syringin Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 QJVXKWHHAMZTBY-GCPOEHJPSA-N 0.000 claims description 3
- QJVXKWHHAMZTBY-KSXIZUIISA-N syringin Natural products COc1cc(C=CCO)cc(OC)c1O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O QJVXKWHHAMZTBY-KSXIZUIISA-N 0.000 claims description 3
- 238000002137 ultrasound extraction Methods 0.000 claims description 3
- CWVRJTMFETXNAD-BMNNCGMMSA-N (1s,3r,4s,5r)-3-[(e)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy-1,4,5-trihydroxycyclohexane-1-carboxylic 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-BMNNCGMMSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 claims description 2
- KRZBCHWVBQOTNZ-DLDRDHNVSA-N isochlorogenic acid Natural products O[C@@H]1[C@H](C[C@@](O)(C[C@H]1OC(=O)C=Cc2ccc(O)c(O)c2)C(=O)O)OC(=O)C=Cc3ccc(O)c(O)c3 KRZBCHWVBQOTNZ-DLDRDHNVSA-N 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 239000012453 solvate Substances 0.000 claims description 2
- 241001593750 Turcica Species 0.000 claims 1
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- 239000000463 material Substances 0.000 abstract description 9
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 abstract description 7
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- 230000008901 benefit Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000902 placebo Substances 0.000 description 4
- 229940068196 placebo Drugs 0.000 description 4
- 244000228295 Polygonum viviparum Species 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 235000005875 quercetin Nutrition 0.000 description 3
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 2
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
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- 230000001276 controlling effect Effects 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 229960001285 quercetin Drugs 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000219050 Polygonaceae Species 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 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 1
- 206010044565 Tremor 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
- 238000010521 absorption reaction Methods 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000001142 anti-diarrhea Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000002225 anti-radical effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- -1 coumarin, organic acid Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229930182486 flavonoid glycoside Natural products 0.000 description 1
- 150000007955 flavonoid glycosides Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004007 reversed phase HPLC Methods 0.000 description 1
- 239000002904 solvent Substances 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
- 239000000341 volatile oil Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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
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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of methods for measuring organic acid and flavones ingredient in serpentgrass simultaneously, comprising the following steps: (1) preparation of test solution；(2) LC-MS/MS is detected；(3) qualitative analysis of ingredient.Reference substance solution is prepared on the basis of serpentgrass ingredient qualitative analysis, the content of its Content of Chlorogenic Acid and gallic acid can also be measured.The present invention is for the first time measured 10 kinds of substances in two active component of organic acid in serpentgrass and flavones simultaneously, perfect serpentgrass quality of medicinal material control method.Using LC-MS/MS analyzing detecting method combination multi-wavelength changeover program, have the advantages that easy, stable, quick, efficient, high sensitivity, reproducible, interference is small, the detection of 10 kinds of substances can be completed in 1 hour, obtaining one can be simultaneously comprising the chromatogram of multiple wavelength informations.
Description
Invention field
The technical field that the invention belongs to be detected using modern analysis detection means to the quality of Tibetan medicine material, more specifically
Say be using multi-wavelength switching measurement serpentgrass in organic acid and flavones ingredient method.
Background technique
Serpentgrass is the dry rhizome of polygonaceae plant serpentgrass (Polygonum Viviparum L), in " Jingzhubencao "
Record, right cloth (serpentgrass) is sweet in flavor, puckery, sour, have antidiarrheal, town intestines tremble with fear pain the effect of.It can be used for controlling wind-heat, except epidemic disease heat, can adjust
With and occlusion disorder, control ageing diseases, rheumatism can also bring down a fever, menstruation regulating, convergence, hemostasis etc.." Chinese Tibetan medicine " is recorded, serpentgrass master
Containing ingredients such as anthraquinone, tannin, polysaccharide, flavonoid glycoside, coumarin, organic acid, fatty acid, existing research also shows to contain in serpentgrass
The Multiple components such as volatile oil, tannin, flavones, polysaccharide, wherein the organic acids ingredient such as gallic acid and chlorogenic acid has anti-oxidant
The effects of, flavones ingredient has stronger anti-radical action and oxidation resistance.
Serpentgrass is recorded in " Drug Standard of Ministry of Public Health of the Peoples Republic of China Tibetan medicine (first) ", wherein only to medicinal material
Carrying out microscopical characters does not have assay index, is unfavorable for effectively controlling the quality of serpentgrass.Have at present and continues the reports such as gorgeous
The reports such as " content that RP-HPLC method measures Vitexin, quercitin and Quercetin in Tibetan medicine serpentgrass simultaneously " and Li Juan
" HPLC method measures the content of gallic acid in serpentgrass, chlorogenic acid and quercetin component simultaneously " in serpentgrass organic acid and
Flavones ingredient carries out quantitative study, is all only capable of being measured 3 kinds of substances, cannot reflect the quality of medicinal material, Wu Fashi comprehensively
The comprehensive and overall evaluation now is carried out to serpentgrass medicinal material.
Summary of the invention
Present invention aims at disadvantages described above and deficiency is directed to, a kind of LC-MS/MS of different periods multi-wavelength switching is established
The method that graphical spectrum technology detects a variety of organic acids and flavones ingredient in serpentgrass simultaneously.
The present invention is achieved by the following technical solutions:
On the one hand, the present invention provides a kind of method of organic acid and flavones ingredient in measurement serpentgrass, feature exists
In this method comprises the following steps:
1) serpentgrass powder the preparation of test solution: is prepared into test solution using methanol solution extraction；
2) high performance liquid chromatography-mass spectrometry analysis condition:
High-efficient liquid phase chromatogram condition: Agilent ZORBAX SB-Aq chromatographic column, having a size of 150mm × 4.6mm × 5 μ
M, mobile phase A are 0.1% aqueous formic acid, and Mobile phase B is acetonitrile, gradient elution, flow velocity 0.8mLmin-1, DAD detector
Detection wavelength: 272nm, 325nm, 360nm switch, 30 DEG C of column temperature in different periods；10 μ L of sample volume；
Eluent gradient elution program are as follows:
Different periods wavelength changeover program are as follows:
Mass Spectrometry Conditions: level four bars mass spectrum, ion source: electric spray ion source ESI；Scanning mode: positive ion mode；Ion is swept
Retouch range: 100-1000m/z；Collision induced dissociation voltage Fragmentor:70V；Atomizing pressure: 50psi；Dry temperature degree:
350℃；Dry gas stream speed: 12L/min；Capillary voltage: 3000V；
3) constituent analysis: NIST standard mass spectrum picture library is retrieved by chem workstation, in combination with related mass spectrogram document
Parsing, qualitative analysis confirm organic acid and flavones ingredient in serpentgrass.
In some embodiments, the preparation step of test solution includes: the accurate serpentgrass powder for weighing No. 3 sieves
1.0g is placed in stuffed conical flask, and precision measures methanol solution 30mL, weighed weight, and ultrasonic extraction supplies less loss with methanol
Weight shakes up, filtering, then through 0.22 μm of membrane filtration.
In some embodiments, the constituent analysis further includes quantitative analysis, is carried out as follows:
(a) preparation of reference substance solution: the reference substance for needing to quantitative determine ingredient is taken to add methanol solvate that reference substance is made molten
Liquid；
(b) Specification Curve of Increasing: taking reference substance solution to dilute multiple concentration, to compare quality as abscissa, peak area
For ordinate, draws standard curve and carry out recurrence calculating, obtain regression equation, related coefficient and the range of linearity；
(c) sample size measure: using different periods multi-wavelength measurement after HPLC spectrum data, by calibration curve method with
Need to measure the content of ingredient in calculated by peak area sample.
In some embodiments, the constituent analysis is to carry out quantitative analysis survey to gallic acid in sample and chlorogenic acid
It is fixed, it carries out as follows:
(a) preparation of reference substance solution:
Mixing reference substance: take gallic acid and chlorogenic acid reference substance add methanol solution be made gallic acid, chlorogenic acid it is mixed
Close reference substance solution；
Gallic acid reference substance solution: gallic acid is taken to add methanol solution that gallic acid reference substance solution is made；
Chlorogenic acid reference substance solution: chlorogenic acid is taken to add methanol solution that chlorogenic acid reference substance solution is made；
(b) Specification Curve of Increasing: taking mixed reference substance solution to dilute, with gallic acid and chlorogenic acid signal-to-noise ratio greater than 10
Dilution is quantitative limit solution.It is accurate respectively to draw 10 μ L of quantitative limit solution, 3 μ L of mixed reference substance solution, 5 μ L, 10 μ L, 15 μ
L, 20 μ L injecting chromatograph, to compare quality as abscissa, peak area is ordinate, draws standard curve and carries out recurrence meter
It calculates, obtains regression equation, related coefficient and the range of linearity；
(c) sample size measure: using different periods multi-wavelength measurement after HPLC spectrum data, by calibration curve method with
The content of gallic acid and chlorogenic acid ingredient in calculated by peak area sample.
In some embodiments, the constituent analysis further include to carrying out efficiency evaluation after quantitative analysis, including
System suitability, specificity, quantitative limit and linear, repeatability, stability and sample recovery rate.
In some embodiments, the methanol solution is 50% methanol aqueous solution.
In some embodiments, the ultrasonic extraction temperature in the preparation of the step 1) test solution is 55 DEG C, ultrasound
Time is 15min.
In some embodiments, the organic acid and flavones ingredient include gallic acid, isochlorogenic acid, epicatechin
Dimer, epicatechin/catechin, Syringin, chlorogenic acid, isoquercitrin, Kaempferol -3-O- sophoroside, Kaempferol -3-O-
Sophorose glycoside isomers, Isorhamnetin -3-O- glucoside.
Multi-wavelength of the present invention, which switches while measuring the method for organic acid and flavones ingredient in serpentgrass, to be had
Have the active effect that
1. the present invention for the first time surveys 10 kinds of substances in two active component of organic acid in serpentgrass and flavones simultaneously
It is fixed, perfect serpentgrass quality of medicinal material control method.
2. of the invention use LC-MS/MS analyzing detecting method to have easy, stable, quick, efficient, high sensitivity, repetition
Property good, the small advantage of interference, the detection of 10 kinds of substances can be completed in 1 hour, and separating degree is good.Establishing reference substance mark
On the basis of directrix curve, additionally it is possible to quantitative analysis detection is carried out to it, to obtain information content extremely abundant.
3. the present invention obtains an energy under the premise of guaranteeing data information loss reduction by multi-wavelength changeover program
Chromatogram that is enough while including multiple wavelength informations.
4. middle test sample of the invention is Extraction solvent with 50% methanol, solid-liquid ratio 1:30 is mentioned using 55 DEG C of ultrasound 15min
Filtering can be detected directly after taking, and sample pre-treatments step is simple, and extraction efficiency is also higher, is not necessarily to column purification, and liquid phase color
It is few to compose interference impurity in separation process.
5. the present invention use be added using acetonitrile-water as mobile phase 0.1% first acid for adjusting pH so that the peak shape at each peak compared with
Good, disengaging time is moderate and separating degree is good, has also reached the ionising effect of each ingredient of increase.
Detailed description of the invention
Fig. 1 different periods multi-wavelength switches the HPLC map of serpentgrass ingredient, and 1-10 is respectively gallic acid, different green original
Acid, epicatechin dimer, epicatechin/catechin, Syringin, chlorogenic acid, isoquercitrin, Kaempferol -3-O- sophoroside,
Kaempferol -3-O- sophorose glycoside isomers, Isorhamnetin -3-O- glucoside.
The HPLC chromatogram of Fig. 2 gallic acid and chlorogenic acid mixed reference substance solution.
The comparison of Fig. 3 gallic acid and chlorogenic acid reference substance solution, test solution and placebo solution HPLC map
Figure.
The standard curve of Fig. 4 gallic acid reference substance solution.
The standard curve of Fig. 5 chlorogenic acid reference substance solution.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
1. reagent, medicinal material, standard items and instrument
1.1 reagents and medicinal material
1.2 standard items
1.3 instrument
2. the preparation of test solution
Precision weighed the serpentgrass powder 1.0g of No. 3 sieves, was placed in stuffed conical flask, and precision measures 30mL50% first
Alcohol, weighed weight are placed in ultrasound 15min in 55 DEG C of Ultrasound Instruments, let cool, and weighed weight is supplied the weight of less loss with methanol, shaken
It is even, filtering, then filtered through 0.22 μm of filter membrane, take subsequent filtrate to get.
The liquid chromatogram and Mass Spectrometry Conditions of 3.LC-MS/MS
The liquid phase chromatogram condition of 3.1 LC-MS/MS
Agilent ZORBAX SB-Aq chromatographic column (150mm × 4.6mm, 5 μm), 0.1% aqueous formic acid of mobile phase
(A)-acetonitrile (B) carries out gradient elution, flow velocity: 0.8mLmin by table 1-1, Detection wavelength: 272nm, 325nm, 360nm be not
Changeover program with the period is carried out by table 2.DAD detector carries out multi-wavelength switching in different periods；30 DEG C of column temperature；Sample volume 10
μL；
1 eluent gradient of table elutes table
The Mass Spectrometry Conditions of 3.2 LC-MS/MS
Testing conditions: level four bars mass spectrum, ion source: electric spray ion source ESI；Scanning mode: positive ion mode；Ion is swept
Retouch range: 100-1000m/z；Collision induced dissociation voltage Fragmentor:70V；Atomizing pressure: 50psi；Dry temperature degree:
350℃；Dry gas stream speed: 12L/min；Capillary voltage: 3000V；
2 different periods multi-wavelength detection table of table
4. the Components identification that multi-wavelength switches the HPLC map of serpentgrass
Experimental result is shown in Fig. 1, and qualitative analysis retrieves NIST standard mass spectrum picture library by chem workstation, in combination with related
The parsing of mass spectrogram document confirms that organic acid and flavones ingredient are as shown in table 3 in serpentgrass:
Components identification result in 3 serpentgrass of table
The quantitative analysis of embodiment 2 gallic acid and chlorogenic acid
On the basis of embodiment 1, can also quantitative analysis be carried out to gallic acid and chlorogenic acid.
1. the preparation of reference substance solution:
Mixing reference substance: taking gallic acid and chlorogenic acid reference substance appropriate, accurately weighed, and 50% methanol solution is added to be made often
1mL 0.086mg containing gallic acid, chlorogenic acid 0.173mg mixed reference substance solution to get；
Gallic acid reference substance solution: taking gallic acid appropriate, accurately weighed, adds 50% methanol solution that every 1mL is made and contains
The reference substance solution of gallic acid 0.0216mg；
Chlorogenic acid reference substance solution: going chlorogenic acid appropriate, accurately weighed, adds 50% methanol solution that every 1mL is made containing green original
The reference substance solution of sour 0.945mg.
2. assay
Serpentgrass quality of medicinal material control method of the present invention, by the serpentgrass sample of 4 parts of separate sources respectively according to
" preparations of 2. test solutions " method progress sample preparation in embodiment 1, sequentially determining calculating gallic acid and chlorogenic acid
Content (n=3).The result is shown in tables 4；
4 four batches of serpentgrass sample size measurement results of table, mg/g, n=3, x ± s
3. the efficiency evaluation of content assaying method
Content assaying method of the present invention carries out efficiency evaluation, including system suitability, specificity, quantifies
Limit and linear, repeatability, stability and sample recovery rate.
The experiment of 3.1 system suitabilities
Precision absorption mixed reference substance solution is appropriate, and by aforementioned chromatographic condition, 6 needle of continuous sample introduction measures peak area, calculates
The peak area RSD of gallic acid is 0.22% (n=6), and the peak area RSD of chlorogenic acid is 0.67% (n=6).2 kinds of ingredient separation
Degree is all larger than 1.5, and tailing factor is greater than 5000, illustrates that system suitability is good in 0.8-1.2, theoretical cam curve.
The experiment of 3.2 specificities
Precision draws reference substance solution, test solution, placebo solution (50% methanol) in right amount, by aforementioned chromatostrip
Part, 1 needle of sample introduction, records chromatogram and reference substance solution, the test solution and placebo solution of reference substance solution respectively
The stacking chart of three, sees Fig. 2 and Fig. 3.The results show that in reference substance in gallic acid and chlorogenic acid and test sample each peak reservation
Time consistency, and placebo solution does not interfere with.
3.3 quantitative limits and linear
Mixed reference substance solution is taken to dilute, it is molten as quantitative limit greater than 10 dilution using gallic acid and chlorogenic acid signal-to-noise ratio
Liquid.It is accurate respectively to draw 10 μ L of quantitative limit solution, 3 μ L of mixed reference substance solution, 5 μ L, 10 μ L, 15 μ L, 20 μ L injecting chromatographs,
With compare quality (μ g) be abscissa, peak area (105) it is ordinate, standard curve is made, sees Fig. 4 and Fig. 5 respectively.It obtains
Regression equation, related coefficient and the range of linearity, are shown in Table 5.
5 linear equation of table
3.4 stability
Take serpentgrass to be prepared into test solution by preceding method, respectively at 0,4,8,12, inject HPLC instrument, record for 24 hours
The peak area of two kinds of ingredients simultaneously calculates RSD, and respectively less than 2.0%, the results showed that sample is stablized interior for 24 hours.
3.5 repeated
Precision weighs 6 parts of same batch sample, prepares test solution by preceding method, measures peak area, calculates 2 kinds of ingredients
Content, RSD is respectively less than 2.0%, and illustration method is reproducible.
The test of 3.6 sample recovery rates
The serpentgrass 0.25g of known content is taken, it is 0.02161mgmL that precision, which draws concentration,-1Gallic acid reference substance is molten
Liquid 1mL, concentration 0.9454mgmL-1Chlorogenic acid reference substance 1mL be added in 6 parts of samples, by preceding method carry out sample
Preparation, measurement analysis, calculates average recovery rate, the results are shown in Table 6.
6 sample recovery rate test result (n=6) of table
Finally it should be noted that: the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, it should be understood by those ordinary skilled in the art that: still
It can modify to a specific embodiment of the invention or some technical features can be equivalently replaced；Without departing from this hair
The spirit of bright technical solution should all cover within the scope of the technical scheme claimed by the invention.
Claims (6)
1. a kind of method of organic acid and flavones ingredient in measurement serpentgrass, which is characterized in that this method comprises the following steps:
1) serpentgrass powder the preparation of test solution: is prepared into test solution using methanol solution extraction；The methanol
Solution is 50% methanol aqueous solution；
2) high performance liquid chromatography-mass spectrometry analysis condition:
High-efficient liquid phase chromatogram condition: Agilent ZORBAX SB-Aq chromatographic column, having a size of 150mm × 4.6mm × 5 μm, stream
Dynamic phase A is 0.1% aqueous formic acid, and Mobile phase B is acetonitrile, gradient elution, flow velocity 0.8mLmin-1, the detection of DAD detector
Wavelength: 272nm, 325nm, 360nm switch, 30 DEG C of column temperature in different periods；10 μ L of sample volume；
Eluent gradient elution program are as follows:
Different periods wavelength changeover program are as follows:
Mass Spectrometry Conditions: level four bars mass spectrum, ion source: electric spray ion source ESI；Scanning mode: positive ion mode；Ion scan model
It encloses: 100-1000m/z；Collision induced dissociation voltage: 70V；Atomizing pressure: 50psi；Dry temperature degree: 350 DEG C；Dry gas stream
Speed: 12L/min；Capillary voltage: 3000V；
3) constituent analysis: retrieving NIST standard mass spectrum picture library by chem workstation, parse in combination with related mass spectrogram document,
Qualitative analysis confirms organic acid and flavones ingredient in serpentgrass；The organic acid and flavones ingredient include galla turcica
Acid, isochlorogenic acid, epicatechin dimer, epicatechin/catechin, Syringin, chlorogenic acid, isoquercitrin, Kaempferol -3-
O- sophoroside, Kaempferol -3-O- sophorose glycoside isomers, Isorhamnetin -3-O- glucoside.
2. measuring method according to claim 1, which is characterized in that the preparation step of test solution includes: accurate title
The serpentgrass powder 1.0g for taking No. 3 sieves, is placed in stuffed conical flask, and precision measures methanol solution 30mL, weighed weight, ultrasound
It extracts, the weight of less loss is supplied with methanol, is shaken up, filter, then through 0.22 μm of membrane filtration.
3. measuring method according to claim 1, which is characterized in that the constituent analysis further includes quantitative analysis, by such as
Lower step carries out:
(a) preparation of reference substance solution: the reference substance for needing to quantitative determine ingredient is taken to add methanol solvate that reference substance solution is made；
(b) Specification Curve of Increasing: reference substance solution is taken to dilute multiple concentration, to compare quality as abscissa, peak area is vertical
Coordinate draws standard curve and carries out recurrence calculating, obtains regression equation, related coefficient and the range of linearity；
(c) sample size measures: using the HPLC spectrum data after the measurement of different periods multi-wavelength, by calibration curve method with peak face
Product calculates the content for needing to measure ingredient in sample.
4. measuring method according to claim 3, which is characterized in that the constituent analysis be to gallic acid in sample and
Chlorogenic acid carries out quantitative analysis measurement, carries out as follows:
(a) preparation of reference substance solution:
Mix reference substance: the mixing pair for taking gallic acid and chlorogenic acid reference substance to add methanol solution that gallic acid, chlorogenic acid is made
According to product solution；
Gallic acid reference substance solution: gallic acid is taken to add methanol solution that gallic acid reference substance solution is made；
Chlorogenic acid reference substance solution: chlorogenic acid is taken to add methanol solution that chlorogenic acid reference substance solution is made；
(b) Specification Curve of Increasing: taking mixed reference substance solution to dilute, and 10 dilution is greater than with gallic acid and chlorogenic acid signal-to-noise ratio
Liquid is quantitative limit solution, accurate respectively to draw 10 μ L of quantitative limit solution, 3 μ L of mixed reference substance solution, 5 μ L, 10 μ L, 15 μ L, 20 μ
L injecting chromatograph, to compare quality as abscissa, peak area is ordinate, draws standard curve and carries out recurrence calculating, obtains
Regression equation, related coefficient and the range of linearity out；
(c) sample size measures: using the HPLC spectrum data after the measurement of different periods multi-wavelength, by calibration curve method with peak face
Product calculates the content of gallic acid and chlorogenic acid ingredient in sample.
5. measuring method according to claim 3, which is characterized in that the constituent analysis further includes laggard to quantitative analysis
Row efficiency evaluation is recycled including system suitability, specificity, quantitative limit and linear, repeatability, stability and sample-adding
Rate.
6. measuring method according to claim 1-5, which is characterized in that the system of the step 1) test solution
Ultrasonic extraction temperature in standby is 55 DEG C, ultrasonic time 15min.
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| CN109270177A (en) * | 2018-08-27 | 2019-01-25 | 贵州医科大学 | The multicomponent content assaying method of one seedling medicine largespike woodnettle root |
| CN110082455B (en) * | 2019-05-24 | 2022-10-04 | 山东省食品药品检验研究院 | Method for identifying bistort rhizome, polygonum bulborum and polygonum palustre |
| CN110514775B (en) * | 2019-09-02 | 2022-03-08 | 中国林业科学研究院林产化学工业研究所 | High performance liquid chromatography analysis method of tannic acid |
| CN110579558B (en) * | 2019-10-09 | 2022-04-05 | 浙江寿仙谷医药股份有限公司 | Detection system and detection method for component content of saffron |
| CN111150739B (en) * | 2019-10-10 | 2023-04-07 | 东莞市东阳光冬虫夏草研发有限公司 | Application of polygonin and method for extracting polygonin from polygonum bulbiferum |
| CN110967432B (en) * | 2019-12-25 | 2021-03-30 | 江南大学 | Method for measuring content of organic acid in root exudates |
| CN111189951A (en) * | 2020-03-17 | 2020-05-22 | 东莞市东阳光冬虫夏草研发有限公司 | Method for rapidly determining chlorogenic acid isomer in polygonum bulbiferum and application |
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