LC-MS/MS determination and pharmacokinetic study of four lignan components in rat plasma after oral administration of Acanthopanax sessiliflorus extract

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• 作者：Yang Song ; Ying Deng ; Danxue Huang ; Jing Wen ; Zhigang Liu ; Famei Li ; ^{lifamei@syphu.edu.cn}
• 关键词：UPLC&ndash ; MS/MS ; ultra-performance liquid chromatography&ndash ; tandem mass spectrometry
• 刊名：Journal of Ethnopharmacology
• 出版年：2012
• 期刊代码：26_03788741
• 类别：pha
• 出版时间：14 June, 2012
• 卷：141
• 期：3
• 页码：957-963
• 文件大小：607 K

摘要

Ethnopharmacological relevance

Acanthopanax sessiliflorus (Rupr. et Maxim.) Seem. is a shrub mainly present in China, Japan and Korea, the root bark of which is considered as one of the sources of Wujiapi and widely used for its various pharmacological effects.

Aim of the study

A selective and sensitive UPLC-MS/MS method was developed and validated for the determination and pharmacokinetic study of asarinin, sesamin, helioxanthin and savinin in rat plasma.

Materials and methods

Sample preparation involved a liquid-liquid extraction of the analytes with methyl tert-butyl ether (MTBE). LC separation was achieved on a UPLC C₁₈ column at 30 掳C with a mobile phase consisting of methanol-2 mM ammonium acetate (68:32, v/v). The detection was accomplished by multiple-reaction monitoring (MRM) scanning with electrospray ionization (ESI) source operating in the positive ionization mode. The optimized mass transition ion-pairs (m/z) monitored for asarinin, sesamin, helioxanthin, savinin and IS were 372.2/233.0, 372.2/233.0, 349.1/319.0, 352.9/334.9 and 180.0/109.7, respectively.

Results

The current LC-MS/MS assay was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery and stability and was suitable for pharmacokinetic studies of the four lignans after oral administration of Acanthopanax sessiliflorus extract. The time to reach the maximum plasma concentration (T_max) was 2.50 卤 0.15 h for asarinin, 1.94 卤 0.28 for sesamin, 2.22 卤 0.48 h for helioxanthin and 2.83 卤 0.29 h for savinin. The elimination half-time (t_1/2) of asarinin, sesamin, helioxanthin and savinin was 6.08 卤 1.10, 11.69 卤 0.50, 7.16 卤 0.52 and 6.26 卤 0.57 h, respectively.

Conclusion

This paper described a simple, sensitive and validated UPLC-MS/MS method for simultaneous determination of four lignans in rat plasma after oral administration of Acanthopanax sessiliflorus extract, and investigated on their pharmacokinetic studies as well.