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目的建立高效液相色谱-串联质谱法(LC-MS/MS)测定人血浆中氯法拉滨浓度。方法采用API3000串联质谱仪及Shimadzu系列液相色谱仪进行检测。血浆样品经乙酸乙酯提取处理,以克拉屈滨为内标。色谱柱为ThermoC18柱(4.6mm×150mm,5μm),流动相为乙腈-水(250∶3,其中含4mmol的乙酸铵和0.3%的甲酸),流速为0.5mL.min-1。氯法拉滨和克拉屈滨的MRM扫描离子通道m/z分别为304.0→170.0,286.1→170.0。进样体积为20μL,每个样品的分析时间为5min。结果氯法拉滨和克拉屈滨保留时间分别为4.00,4.11min。氯法拉滨在10～2000ng·mL-1内线性关系良好(r=0.9995),日内、日间RSD均低于9.60%,准确度为101.10%～102.94%。结论本法样品预处理简便快速,检测准确、灵敏、专一,适用于氯法拉滨药动学的研究。
Objective To establish a method for the determination of clofarabine in human plasma by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods API3000 tandem mass spectrometer and Shimadzu series liquid chromatography were used for detection. Plasma samples were extracted with ethyl acetate and treated with cladribine as internal standard. The column was a Thermo C18 column (4.6 mm × 150 mm, 5 μm) with a mobile phase of acetonitrile-water (250: 3 containing 4 mmol of ammonium acetate and 0.3% of formic acid) at a flow rate of 0.5 mL · min -1. The MRM scanning ion channels of clofarabine and cladribine m / z were 304.0 → 170.0, 286.1 → 170.0, respectively. The injection volume was 20 μL and the analysis time for each sample was 5 min. Results The retention time of clofarabine and cladribine was 4.00,4.11min. Clofarabine showed a good linear relationship (r = 0.9995) within 10-2000 ng · mL-1. The intra-day and inter-day RSD were less than 9.60% and the accuracy was 101.10% -102.94%. Conclusion The sample pretreatment is simple, rapid, accurate, sensitive and specific. It is suitable for the study of clofarabine pharmacokinetics.