液质联用法测定裸鼠血浆中吉西他滨浓度

目的:建立高效灵敏的液质联用法(LC-MS/MS)测定裸鼠血浆中吉西他滨浓度。方法:选用0.01%醋酸水和乙腈(80∶20)作为流动相;质谱检测选择正离子方式,多离子反应监测(MRM)扫描,用于吉西他滨和内标(头孢克洛)定量分析的离子反应对分别为m/z 264.1→m/z 112.0和m/z 368.1→m/z 174.1。结果:该方法线性范围为5～500 ng.mL-1,定量下限为5 ng.mL-1。日内日间精密度均<12.9%,准确度<3.4%。结论:本方法操作简便、快速,灵敏度高,能够满足裸鼠血浆中吉西他滨检测的要求。

Determination of Gemcitabine in Nude Mice by LC-MS/MS

OBJECTIVE: To determine the plasma concentration of gemcitabine in nude mice by establishing a rapid and sensitive liquid chromatography/tandem mass spectrometry(LC-MS/MS).METHODS: Water containing 0.01% acetic acid–acetonitrile(80∶20,v/v) was used as mobile phase.In mass-spectrometric detection,MSD Positive ion mode was applied with scanning performed using multiple reaction monitoring(MRM).The ionic reaction pair used for qualitative analysis were m/z 264.1→m/z 112.0 for gemcitabine and m/z 368.1→m/z 174.1 for internal standard.RESULTS: The linear range of gemcitabine was 5-500 ng·mL-1 with lower limit of quantification(LOQ) of 5 ng·mL-1,intra-day and inter-day precision of <12.9% and accuracy of<3.4%.CONCLUSION: The method was simple,rapid and sensitive,and it is up to the standard for the determination of plasma concentration of gemcitabine in nude mice.