LC-MS/MS法测定全血中西罗莫司的药物浓度

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

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。

Objective To establish a LC - MS/MS method for determination of sirolimus in human whole blood. Methods The samples of whole blood were deproteinated by ZeSO4 - aeetonitrile mixed liquid and separated by a Zobox XDB - CN column with a mobile plase of water - aeetonitrile 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. Results The linear range of siroli- mus 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%. Conclusion The method is sensitive, accurate and simple for monitoring of whole blood concentration of sirolimus.