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
A rapid, simple and practical high-performance liquid chromatography method coupled with diode array detector（HPLC–DAD） was developed to evaluate the quality of Alisma orientale（Sam.） Juz.through a simultaneous d...A rapid, simple and practical high-performance liquid chromatography method coupled with diode array detector（HPLC–DAD） was developed to evaluate the quality of Alisma orientale（Sam.） Juz.through a simultaneous determination of four major active triterpenes using a single standard to determine the multi-components（SSDMCs）. Alisol B 23-acetate was selected as the reference compound for calculating the relative response factors. All calibration curves showed good linearity（R240.9998） within test ranges. RSDs for intra- and inter-day of four analytes were less than 3.6% and 2.3%; the overall recovery was 92.1–110.2%（SSDMC）. The proposed method was successfully applied to quantify the four components in 20 samples from different localities in China. Moreover, significant variations were demonstrated in the content of these compounds. In addition, hierarchical clustering analysis（HCA） and principal components analysis（PCA） were performed to differentiate and classify the samples based on the contents of Alisol C 23-acetate, Alisol A, Alisol A 24-acetate and Alisol B 23-acetate. This simple,rapid, low-cost and reliable HPLC–DAD method using SSDMC is suitable for routine quantitative analysis and quality control of A. orientale（Sam.） Juz.展开更多
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.
基金financially supported by Liaoning Innovative Research Team in University (LNIRT, Grant no.LT2013022)
文摘A rapid, simple and practical high-performance liquid chromatography method coupled with diode array detector（HPLC–DAD） was developed to evaluate the quality of Alisma orientale（Sam.） Juz.through a simultaneous determination of four major active triterpenes using a single standard to determine the multi-components（SSDMCs）. Alisol B 23-acetate was selected as the reference compound for calculating the relative response factors. All calibration curves showed good linearity（R240.9998） within test ranges. RSDs for intra- and inter-day of four analytes were less than 3.6% and 2.3%; the overall recovery was 92.1–110.2%（SSDMC）. The proposed method was successfully applied to quantify the four components in 20 samples from different localities in China. Moreover, significant variations were demonstrated in the content of these compounds. In addition, hierarchical clustering analysis（HCA） and principal components analysis（PCA） were performed to differentiate and classify the samples based on the contents of Alisol C 23-acetate, Alisol A, Alisol A 24-acetate and Alisol B 23-acetate. This simple,rapid, low-cost and reliable HPLC–DAD method using SSDMC is suitable for routine quantitative analysis and quality control of A. orientale（Sam.） Juz.
