目的 :建立简单快速的LC-MS/MS检测大鼠血浆中紫杉醇浓度的方法。方法:血浆样本100μL加入终浓度为100ng/mL的多烯紫杉醇(内标),用混合溶剂乙酸乙酯-二氯甲烷-乙腈(4:1:1)萃取后用LC-MS/MS进行分析。采用多离子反应监测(MRM)扫描方式,在ESI源正离子加钠模式下,紫杉醇和内标物的离子对分别为m/z 876.29→308.1、m/z830.34→549.3。结果:样品分析时间仅需2min,方法线性范围在0.55-550ng/mL(r=0.997),最低检测限为0.55ng/mL。紫杉醇在三个质控浓度(1.1, 110, 550ng/mL)检测下的提取回收率分别为79.32%,77.54 %及78.64%。结论:LC-MS/MS检测方法灵敏度高、专属性强、简单快捷,采用加钠模式可增加紫杉醇检测的响应值,提高检测灵敏度,适用于检测血浆中微量紫杉醇的浓度。
OBJECTIVE To establish a simple and rapid LC-MS/MS method for the determination of paclitaxei in rat plas ma. METHODS He 100 bd. of sample plasma was extracted with mixed solvent (ethyl acetate:dichloromethane: acetonitrile = 4 : 1 :.1) after addition of 100 ng,mL^-1 doeetaxel(internal standard), and analyzed by LC-MS/MS system. Detection was per- formed with multiple reactions monitoring (MRM) using electrospray ionization (ES1) and adding Na ion mode. The precur- sor/product ion transitions of paclitaxel and docetaxel(internal standard)were monitored at m/z 876. 29→308. 1 and 830.34± 549. 3, respectively. RESULTS The analysis time was only 2 rain in positive mode; the calibration curve was linear in the con- centration range of 0. 55-550 ng·mL^-1. The lowest limit of quantification (LLOQ) reached 0. 55 ng·mL 1. The extraction recoveries were 79.320/00, 77. 54 % and 78. 64% for three QC concentration levels (1.1, 110, 550 ng·mL ^-1). CONCLU- SlONThe I.C-MS/MS method proved to be sensitive, specific, simple and rapid; using the adding sodium mode can increase pa- clitaxel detection response value, improve the detection sensitivity, suitable for detection of trace paclitaxel in plasma.