HPLC-MS／MS联用技术测定人血浆中9-硝基喜树碱的含量

目的建立HPLC-MS—MS法测定人血浆中9-硝基喜树碱浓度。方法以喜树碱为内标，流动相为乙腈-2％甲酸水溶液（55：45，V／V），色谱柱为Agilent C18（3．5μm，2．1mm×150mm），电喷雾离子源（ESI），正离子多反应监测（MRM）方式进行检测。用于定量分析的离子对分别为[M＋H]^＋m／z 394．2→m/z 350．0（9-硝基喜树碱），[M＋H]^＋m／z 349.1→m/z 305．3（喜树碱）。结果9-硝基喜树碱线性范围1～300μg·L^-1内呈良好线性关系（r=0．9990），定量下限为1μg·L^-1。日内、日间精密度的RSD均〈15％，平均回收率为76.02％，RSD为5．7％。结论本方法专属性强，生物样品处理方便，灵敏度高，适用于9-硝基喜树碱临床药动学研究。

Determination of 9-Nitrocamptothecin in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry

Aim To establish an HPLC-MS-MS method for the determination of 9-Nitrocamptothecin in human plasma. Methods Camptothecin was used as the internal standard. 9-Nitrocamptothecin was separated on an Agilent Cls column （3.5 μm, 2.1 × 150mm）. The mobile phase consisted of acetonitrile-2% formic acid （55： 45, V/V）. Electrospray ionization（ESI） source was applied and operated in the positive multiple reaction monitoring（MRM） mode. The transi- tions of [ M ＋ H]^＋ m/z 394.2→m/z 350.0 and [ M ＋ H]^＋ m/z 349.1→m/z 305.3 were used to quantify 9-Nitrocamptothecin and the internal standard, respectively. Results The linear calibration curve was obtained over the concentration range of 1 -300μg·L^-1. The detection limit was 1μg·L^-1. The inter and intra-day precision （ RSD ） was less than 15%. The average recovery was 76.02%, RSD was 5.7%. Couclusion The method is proved to be specific, convenient, sensitive and suitable for the clinical pharmacokinetics of 9-Nitrocamptothecin.