A sensitive,fast and comprehensive method for the quality assessment of Semen Ziziphi Spinosae(SZS)standard decoction with characterization of its chemical components was developed and validated.UPLC-Q/TOF-MS/MS syste...A sensitive,fast and comprehensive method for the quality assessment of Semen Ziziphi Spinosae(SZS)standard decoction with characterization of its chemical components was developed and validated.UPLC-Q/TOF-MS/MS system was used to identify thirty-six chemical components of SZS standard decoction which included nucleosides,phenolic acids,alkaloids,and flavonoids.Furthermore,a UPLC-PDA method was validated to simultaneously determine adenosine,protocatechuic acid,magnoflorine,catechin,protocatechin,vicenin II,spinosin,kaempferol-3-rutinoside,and 6'''-feruloylspinosin which represent four species of characteristic compounds.The qualitative method had been validated according to Chinese Pharmacopoeia(2015 edition)in terms of lineary,repeatability,recovery and stability for all analytes,with the results showing good precision,accuracy and stability.In conclusion,the method using UPLC combined with MS and PDA provided a novel way for the standardization and identification of SZS standard decoction,and also offered a basis for qualitative analysis and quality assessment of the preparations for SZS standard decoction.展开更多
A sensitive and reliable ultra fast liquid chromatography tandem mass spectrometry(UFLC-MS/MS)method has been developed and validated for simultaneous quantitation of alisol A and alisol B 23-acetate from Alisma orien...A sensitive and reliable ultra fast liquid chromatography tandem mass spectrometry(UFLC-MS/MS)method has been developed and validated for simultaneous quantitation of alisol A and alisol B 23-acetate from Alisma orientale(Sam.)Juz.in rat plasma using diazepam as an internal standard(IS).The plasma samples were extracted by liquideliquid extraction with methyl tert-butyl ether and separated on a Venusil MP C18 column(100 mm×2.1 mm,3.0 mm)(Venusil,China)using gradient elution with the mobile phase consisting of methanol and 0.1%acetic acid in water at a flow rate of 0.4 ml/min.The two analytes were monitored with positive electrospray ionization by multiple reaction monitoring mode(MRM).The lower limit of quantitation was 5.00 ng/ml for alisol A and 5.00 ng/ml for alisol B 23-acetate.The calibration curves were linear in the range of 5.00 e2500 ng/ml for alisol A and 5e2500 ng/ml for alisol B 23-acetate.The mean extraction recoveries were above 63.8%for alisol A and 68.0%for alisol B 23-acetate from biological matrixes.Both intra-day and inter-day precision and accuracy of analytes were well within acceptance criteria(15%).The validated method was successfully applied to the pharmacokinetic study of alisol A and alisol B 23-acetate in rat plasma after oral administration of alcohol extract of Alismatis Rhizoma.展开更多
基金financially supported by the National Key Scientific Project for China New Drug Discovery and Twelfth Five-Year Plan-preclinical study on Suanzaoren granules(No.2014ZX09304306)the Key Technologies of Common Quality Evaluation of New Drugs(Grant no.2015010201)
文摘A sensitive,fast and comprehensive method for the quality assessment of Semen Ziziphi Spinosae(SZS)standard decoction with characterization of its chemical components was developed and validated.UPLC-Q/TOF-MS/MS system was used to identify thirty-six chemical components of SZS standard decoction which included nucleosides,phenolic acids,alkaloids,and flavonoids.Furthermore,a UPLC-PDA method was validated to simultaneously determine adenosine,protocatechuic acid,magnoflorine,catechin,protocatechin,vicenin II,spinosin,kaempferol-3-rutinoside,and 6'''-feruloylspinosin which represent four species of characteristic compounds.The qualitative method had been validated according to Chinese Pharmacopoeia(2015 edition)in terms of lineary,repeatability,recovery and stability for all analytes,with the results showing good precision,accuracy and stability.In conclusion,the method using UPLC combined with MS and PDA provided a novel way for the standardization and identification of SZS standard decoction,and also offered a basis for qualitative analysis and quality assessment of the preparations for SZS standard decoction.
基金This study was financially supported by Liaoning Innovative Research Team in University(LNIRT,Grant No.LT2013022).
文摘A sensitive and reliable ultra fast liquid chromatography tandem mass spectrometry(UFLC-MS/MS)method has been developed and validated for simultaneous quantitation of alisol A and alisol B 23-acetate from Alisma orientale(Sam.)Juz.in rat plasma using diazepam as an internal standard(IS).The plasma samples were extracted by liquideliquid extraction with methyl tert-butyl ether and separated on a Venusil MP C18 column(100 mm×2.1 mm,3.0 mm)(Venusil,China)using gradient elution with the mobile phase consisting of methanol and 0.1%acetic acid in water at a flow rate of 0.4 ml/min.The two analytes were monitored with positive electrospray ionization by multiple reaction monitoring mode(MRM).The lower limit of quantitation was 5.00 ng/ml for alisol A and 5.00 ng/ml for alisol B 23-acetate.The calibration curves were linear in the range of 5.00 e2500 ng/ml for alisol A and 5e2500 ng/ml for alisol B 23-acetate.The mean extraction recoveries were above 63.8%for alisol A and 68.0%for alisol B 23-acetate from biological matrixes.Both intra-day and inter-day precision and accuracy of analytes were well within acceptance criteria(15%).The validated method was successfully applied to the pharmacokinetic study of alisol A and alisol B 23-acetate in rat plasma after oral administration of alcohol extract of Alismatis Rhizoma.