LC-MS/MS法测定全血中西罗莫司的药物浓度

目的建立测定人全血中西罗莫司(免疫抑制剂)浓度的LC-MS/MS的方法。方法全血样品经硫酸锌乙腈混合液沉淀后,用Zobox XDB-CN色谱柱,0.1 mmol.L-1乙酸水-0.1 mmol.L-1乙酸乙腈(60∶40)为流动相,流速0.45 mL.min-1,通过电喷雾离子化电离源,经多反应监测模式检测。结果全血中西罗莫司的线性范围为1.12～33.47μg.L-1,日内、日间RSD均小于10%,提取回收率为81.4%～92.4%。结论本法灵敏、准确、快速,可用于人全血中西罗莫司浓度监测和药代动力学研究。

LC-MS/MS determination of sirolimus in human whole blood

Objective To establish a LC-MS/MS method for determination of sirolimus in human whole blood.MethodsThe samples of whole blood were deproteinated by ZeSO4-acetonitrile mixed liquid and separated by a Zobox XDB-CN column with a mobile plase of water-acetonitrile solution(containing 0.1 mmol·L-1 acetic acid,60∶40) at the flow rate of 0.45 mL·min-1.Detection was performed on a tandem mass spectrometry with electrospray ionization source in positive ion mode.Multiple reactions monitoring mode was used to quantify sirolimus and internal standard respectively.ResultsThe linear range of sirolimus was 1.12-33.47 μg·L-1.The intra-day and inter-day RSD were both less than 10%.The extraction recoveries were 81.4%-92.4%.ConclusionThe method is sensitive,accurate and simple for monitoring of whole blood concentration of sirolimus.