摘要
建立高效液相色谱-串联质谱法测定大鼠血浆中淫羊藿素(ICT)。血浆样品经乙腈沉淀蛋白后,以乙腈-水-乙酸(72:28:1.5,v/v/v)为流动相,通过Dikma C18柱分离,采用电喷雾离子化四极杆串联质谱,以多反应监测(MRM)方式进行检测。用于定量分析的二级碎片离子分别为m/z387→m/z313(ICT)和m/z331→m/z315(麦黄酮,内标)。ICT血浆浓度测定方法的线性范围为2.5～1000ng·mL-1,定量限为2.5ng·mL-1。日内、日间精密度(RSD)均小于9.63%,准确度(RE)在±7.42%之内。本方法专属性强,灵敏度高,血浆用量少,适用于临床前药代动力学研究。
The paper is to report the development of a high-performance liquid chromatographic/tandem mass spectrometry（HPLC-MS/MS） method for the determination of icaritin（ICT） in rat plasma.After precipitated with acetonitrile from the plasma,ICT was isolated chromatographically on a Dikma C18 column.The mobile phase consisted of acetonitrile-water-acetic acid（72：28：1.5,v/v/v）.Electrospray ionization（ESI） source was applied and operated in the positive ion mode.Multiple reaction monitoring（MRM） mode with the transitions of m/z 387 → m/z 313 and m/z 331 → m/z 315 were used to quantify ICT and the internal standard,respectively.The linear calibration curve was obtained in the concentration range of 2.5-1 000 ng·mL^-1.The lower limit of quantification was 2.5 ng·mL-1.The inter-and intra-day precision（RSD） were less than 9.63%,and the accuracy（relative error） was within ±7.42%.The method was proved to be suitable for the pharmacokinetics of ICT,which offers advantages of high sensitivity and selectivity.
出处
《药学学报》
CAS
CSCD
北大核心
2009年第10期1140-1144,共5页
Acta Pharmaceutica Sinica
