Bo Fang, Dou Ting, Wang Xingrui, Donkor Paul Owusu, Ouyang Huizi, Chang Yanxu, Tu Yaru, Gao Xiumei, He Jun
Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China.
The First Affiliated Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 May 15;990:80-3. doi: 10.1016/j.jchromb.2015.03.017. Epub 2015 Mar 30.
A method coupling high performance liquid chromatography with tandem mass spectrometry has been developed and validated for quantifying periplogenin in rat plasma using psoralen as an internal standard (IS). Plasma samples were pretreated using a simple liquid-liquid extraction with ethyl acetate and the chromatographic separation of periplogenin and psoralen was achieved on a Waters XBridge™ BEH C18 column with 0.1% formic acid and acetonitrile as mobile phase at a flow rate of 0.4mL/min. The detection was performed on a positive ion mode with electrospray ionization (ESI) source. The optimized ion transition pairs for quantitation were m/z 391.3→m/z 337.2 for periplogenin and m/z 187.0→m/z 131.0 for IS. The total run time was 9.0min. The calibration curve was linear over the range of 0.2-250ng/mL (r>0.99) with the lower limit of quantitation (LLOQ) at 0.2ng/mL. The intra- and inter-day precision were below 9.85% and the mean accuracy were from -10.03% to 10.26%. The average recoveries of periplogenin in plasma ranged from 85.1% to 95.6%. The proposed method was successfully applied in evaluating the pharmacokinetics of periplogenin after an oral dose of 30mg/kg Cortex Periplocae extract in rats.
已开发并验证了一种将高效液相色谱与串联质谱联用的方法，以补骨脂素作为内标（IS）定量大鼠血浆中的杠柳毒苷。血浆样品采用乙酸乙酯进行简单液液萃取预处理，杠柳毒苷和补骨脂素在 Waters XBridge™ BEH C18 柱上进行色谱分离，流动相为含 0.1%甲酸的乙腈，流速为 0.4mL/min。检测在电喷雾电离（ESI）源的正离子模式下进行。定量的优化离子跃迁对为杠柳毒苷的 m/z 391.3→m/z 337.2 和内标的 m/z 187.0→m/z 131.0。总运行时间为 9.0 分钟。校准曲线在 0.2 - 250ng/mL 范围内呈线性（r>0.99），定量下限（LLOQ）为 0.2ng/mL。日内和日间精密度均低于 9.85%，平均准确度在 -10.03%至 10.26%之间。杠柳毒苷在血浆中的平均回收率为 85.1%至 95.6%。所提出的方法成功应用于评估大鼠口服 30mg/kg 香加皮提取物后杠柳毒苷的药代动力学。
