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目的:建立高效液相色谱-串联质谱法测定大鼠血浆中依立替康及其代谢物SN-38的浓度。方法:血浆中加入内标后经固相萃取后进行分析。采用Symmetry C18色谱柱(150 mm×2.1 mm,5μm),流动相为pH=3.0的5 mmol.L-1甲酸铵缓冲液(A)-含0.1%甲酸的甲醇(B),梯度洗脱,梯度流速恒定为0.25 mL.min-1,柱温为30℃,整个分析时间为10min。采用ESI正离子多反应监测模式进行检测。结果:依立替康及其代谢物SN-38线性范围分别为1～2000 ng.mL-1和0.5～100 ng.mL-1;血浆中依立替康及SN-38的LLOQ分别为1 ng.mL-1和0.5 ng.mL-1;提取回收率均在88%以上;方法回收率在90%～110%之间;批内、批间RSD均小于9%。结论:本方法灵敏度高,操作简便,可应用于大鼠血浆中依立替康及其代谢物SN-38浓度的测定。
OBJECTIVE: To establish a method for the determination of irinotecan and its metabolite SN-38 in rat plasma by high performance liquid chromatography-tandem mass spectrometry. Methods: Plasma samples were analyzed by solid-phase extraction after adding internal standard. The column was eluted with a Symmetry C18 column (150 mm × 2.1 mm, 5 μm) with 5 mmol·L -1 ammonium formate buffer (A) and 0.1% formic acid in methanol (B) with a mobile phase of pH 3.0. The gradient flow rate was constant at 0.25 mL.min-1, the column temperature was 30 ° C, and the entire analysis time was 10 min. ESI positive ion multiple reaction monitoring mode was used for detection. RESULTS: The linear range of irinotecan and its metabolite SN-38 was 1 ~ 2000 ng.mL-1 and 0.5 ~ 100 ng.mL-1 respectively. The LLOQs of irinotecan and SN-38 in plasma were 1 ng. mL-1 and 0.5 ng.mL-1 respectively. The recoveries of the two methods were over 88%. The recoveries were between 90% and 110%. The intra-assay and inter-assay RSD were less than 9%. Conclusion: The method is sensitive and easy to operate and can be applied to the determination of irinotecan and its metabolite SN-38 in rat plasma.