液相色谱-串联质谱法测定人全血中阿莫地喹的浓度

LC- MS/MS methods for determination of amodiaquine in human whole blood

目的建立液相色谱-串联质谱(LC-MS/MS)法测定人全血中阿莫地喹的浓度。方法以稳定同位素化合物氘10-阿莫地喹为内标,全血经直接沉淀后稀释进样分析。以CAPCELL PAK C18 MGIII(100 mm×2.0 mm,5μm)为分析柱,0.2%甲酸的水溶液-0.2%甲酸的乙腈溶液为流动相,梯度洗脱。电喷雾离子源,正离子MRM扫描分析,阿莫地喹和内标离子对分别为m/z 358.2→285.2和m/z 368.2→285.2。结果阿莫地喹在1～100μg.L-1范围内线性关系良好,定量下限为1μg.L-1。批内、批间精密度RSD均小于6%,平均提取回收率在80.9%～87.7%范围内。结论本方法灵敏度高、专一性好、操作简单,可用于人全血中阿莫地喹的检测。

AIM To develop a LC-MS/MS method for determination of amodiaquine in human whole blood. METHODS After addition of [2H10] -amodiaquine （internal standard, IS）, the analyte was achieved by protein precipitation. The analytes were separated using a CAPCELL PAK C18 MGM （100 mm X 2.0 mm, 5 μm） . The mobile phase consisted of 0.2% formic acid water solution-0.2% formic acid acetonitrile solution. The protonated ion of the analytes was detected in positive ionization by Multiple Reaction Monitoring （MRM） mode. The mass transition pairs of m/z 358.2--285.2 for amodiaquine and m/z 368.2-285.2 for IS. RESULTS The linear calibration curve of amodiaquine was obtained in the concentration range of 1 - 100 μg. L-1. The lower limit of quantitation was 1 μg.L-1. The inter-and intra-run precision （RSD） were less than 6%. The averagerecovery was range of 80.9% to 87.7%. CONCLUSION The established LC-MS/MS method is shown to be sensitive, accurate, simple and suitable for the determination of amodiaquine in human whole blood.