Liu Man, Liu Huiping, Lu Xiumei, Li Chao, Xiong Zhili, Li Famei
Department of Analytical Chemistry, Shenyang Pharmaceutical University, Shenyang 110016, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Dec 1;860(1):113-20. doi: 10.1016/j.jchromb.2007.10.019. Epub 2007 Oct 22.
A sensitive, specific and accurate LC-MS/MS method was developed for simultaneous determination of icariin, icariside II and osthole in rat plasma. With carbamazepine as the internal standard, plasma samples were prepared by protein precipitation with acetonitrile. Analysis was carried out on an ACQUITY UPLC BEH C(18) column with a linear gradient and 0.1% aqueous acetic acid and acetonitrile were used as mobile phase. Detection was performed by means of electrospray ionization mass spectrometry in positive ion mode with multiple reaction monitoring. Linear calibration curves of icariin, icariside II and osthole were obtained over the concentration ranges of 2.00-200, 2.00-200 and 2.00-500 ng/ml, respectively. The intra- and inter-day precisions were within 8.0% and 14%, and the accuracy was from -6.0% to 9.0%. The method was successfully applied to pharmacokinetic studies of icariin, icariside II and osthole in rats after oral administration of Gushudan extract.
建立了一种灵敏、特异且准确的液相色谱-串联质谱法，用于同时测定大鼠血浆中淫羊藿苷、淫羊藿次苷II和蛇床子素。以卡马西平为内标，血浆样品采用乙腈蛋白沉淀法制备。在ACQUITY UPLC BEH C(18)柱上进行分析，采用线性梯度，以0.1%的乙酸水溶液和乙腈为流动相。通过电喷雾电离质谱在正离子模式下进行多反应监测检测。淫羊藿苷、淫羊藿次苷II和蛇床子素的线性校准曲线分别在2.00 - 200、2.00 - 200和2.00 - 500 ng/ml的浓度范围内获得。日内和日间精密度均在8.0%以内，准确度在-6.0%至9.0%之间。该方法成功应用于大鼠口服骨疏丹提取物后淫羊藿苷、淫羊藿次苷II和蛇床子素的药代动力学研究。
