化学
色谱法
电喷雾电离
选择性反应监测
甲酸
蛋白质沉淀
高效液相色谱法
串联质谱法
质谱法
液相色谱-质谱法
作者
Shuanghu Wang,Haiya Wu,Peiwu Geng,Yuan-Yao Lin,Zezheng Liu,Lijing Zhang,Jianshe Ma,Yunfang Zhou,Xianqin Wang,Congcong Wen
摘要
Abstract Dendrobine, considered as the major active alkaloid compound, has been used for the quality control and discrimination of Dendrobium which is documented in the Chinese Pharmacopoeia . In this work, a sensitive and simple ultra‐performance liquid chromatography tandem mass spectrometry (UPLC‐MS/MS) method for determination of dendrobine in rat plasma is developed. After addition of caulophyline as an internal standard (IS), protein precipitation by acetonitrile–methanol (9:1, v/v) was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C 18 (2.1 ×100 mm, 1.7 µm) column with acetonitrile and 0.1% formic acid as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reaction monitoring mode was used for quantification using target fragment ions m / z 264.2 → 70.0 for dendrobine and m / z 205.1 → 58.0 for IS. Calibration plots were linear throughout the range 2–1000 ng/mL for dendrobine in rat plasma. The RSDs of intra‐day and inter‐day precision were both <13%. The accuracy of the method was between 95.4 and 103.9%. The method was successfully applied to pharmacokinetic study of dendrobine after intravenous administration. Copyright © 2015 John Wiley & Sons, Ltd.
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