全血中杀鼠迷的高效液相色谱-电喷雾电离质谱联用法测定研究

Characterization of coumatetralyl in whole blood by liquid chromatography electrospray ionization mass spectrometry

目的:建立简便、准确、灵敏的测定全血中痕量杀鼠迷的高效液相色谱-电喷雾电离质谱检测方法。方法:全血样品经乙酸乙酯萃取,以甲醇+0.1%乙酸(50+50)为流动相,采用XDBC18柱(150mm×2.1mm×5μm)分离,通过电喷雾电离离子化技术及选择性离子检测(SIM)进行测定,定量分析离子为m/z:293[M+H]+。结果:线性范围为1.00～50.0μg/L,定量检测下限为0.50μg/L,方法回收率在90.8%～102.7%,RSD均小于10%。结论:该法操作简便、快速、灵敏、准确,适用于中毒病人的中毒诊断分析。

Objective:To establish a simple, accurate and sensitive method for characterization of coumatetralyl in whole blood by liquid chromatography-mass spectrometry with an electrospray ionization(ESI) interface.Methods:Samples were extracted by ethyl acetate and a satisfactory separation was achieved on Zorbax XDB C 18 column( 150 mm× 2.1 mm× 5 μm)by using the mobile phase consisting of CH 3OH(50%) and 0.1% HAC(50%).The ion mass spectral m/z:293\ + was slected to quantify by the selective ion monitoring(SIM) in a positive mode.Results:The linear range was 1.0～ 50.0 μg/L and the limit of quantification was found to be 0.50 μg/L for coumatetralyl.The extraction recoveries were between 90.8%~102.7%,the RSD was less than 10%.Conclusion:This method is found to be sensitive,fast,and accurate to characterize trace coumatetralyl in whole blood and can be used in the diagnosis of the clinic poisoning patients.