LC-MS/MS法测定肝脏中甲卡西酮和卡西酮

Determination of methcathinone and cathinone in liver by LC-MS/MS

为测定肝脏组织中甲卡西酮及其代谢物卡西酮,研究开发了液相色谱-串联质谱(LC-MS/MS)方法。肝脏组织剪碎、研磨成匀浆,添加含内标双苯戊二氨酯(SKF_(525A))的乙腈溶液,经涡旋、振荡、离心后,0.22μm微孔有机滤膜过滤,LC-MS/MS检测。采用ZORBAX SB-C_(18)色谱柱(50 mm×4.6 mm,1.8μm),柱温为23℃,乙腈和0.2%甲酸水溶液为流动相,流速为2.0 mL·min-1进行梯度洗脱。电喷雾离子源(ESI),正离子多反应监测模式(MRM)检测。结果表明该方法对甲卡西酮的检测在0.5~3000 ng·g^(-1)范围内呈现良好的线性关系,检出限为0.2 ng·g^(-1),定量限为0.5 ng·g^(-1);对卡西酮的检测在1.0~3000 ng·g^(-1)范围内呈现良好线性关系,检出限为0.5 ng·g^(-1),定量限为1.0 ng·g^(-1);甲卡西酮和卡西酮的回收率分别为91.51%~96.35%和90.55%~94.08%,精密度均小于15%。该方法操作简便、灵敏度较高,适用于肝脏组织中甲卡西酮及其代谢物卡西酮的浓度测定及代谢研究。

A liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was developed for the determination of methcathinone and its metabolite cathinone in liver.The liver tissue was ground into homogenate,and acetonitrile solution containing proadifen hydrochloride(SKF_(525A))was added.The sample was vortexed and centrifuged.The supernatant was separated and filtrated using 0.22μm Millipore filter before LC-MS/MS analysis.ZORBAX SB-C_(18)column(1.8μm,50 mm×4.6 mm)was used with column temperature of 23℃,mobile phase of acetonitrile and 0.2%formic acid in water,gradient elution,flow rate of 2.0 mL·min^(-1).Data was acquired using multiple reaction monitoring(MRM)mode with electrospray ion source(ESI).The calibration curves of methcathionone in liver tissue displayed good linear in the range of 0.5~3000 ng·g^(-1)with detection limit of 0.2 ng·g^(-1).The linear relationship of cathinone was in the range of 1.0~3000 ng·g^(-1)with detection limit of 0.5 ng·g^(-1).Their recoveries ranged from91.51%to 96.35%and 90.55%to 94.08%,respectively.The RSD was less than 15%.A simple and sensitive method was established to determine methcathinone and its metabolite cathinone in liver tissue.