QuEChERS-HPLC-MS/MS法在咖啡因中毒案例中的应用研究

Application of QuEChERS-HPLC-MS/MS method in the case of caffeine poisoning

目的:通过对1例服用咖啡因中毒死亡的典型案例,利用QuEChERS前处理结合液相色谱-串联质谱法建立一种快速、准确测定咖啡因中毒者血液和尿液中的咖啡因浓度的方法。方法:使用标准加入法,以己可碱为内标将其添加在血液和尿液中,经DisQuE萃取管用乙腈提取,Captiva ND Lipids净化管净化,浓缩后经液相色谱分离,经三重串联四极杆质谱法测定。结果:对案例血液和尿液中加入浓度为10~1000μg/mL范围的咖啡因时线性关系大于0.999,呈良好的线性关系。血液中基质效应为46.9%,提取回收率为87.3%;尿液中基质效应为48.2%,提取回收率为65.1%。两者精密度均小于15%。结论:本方法具有快速、简便的优点,适用于咖啡因中毒者的血液和尿液中咖啡因浓度快速测定。

For quantification of target compounds in this study,standard addition method was employed,pentifylline(internal standard:IS)and common chemicals were added to blood and urine.QuEChRES dispersive extraction method was employed for extraction of target compounds from samples,the extraction solution was purified by Captiva ND Lipid cartridge.When caffeine was in the range of 10-1,000μg/mL,the linear correlation coefficient was greater than 0.999 and the linearity was good.The matrix effect in whole blood sample was 46.9%and the extraction recovery was 87.3%;the matrix effect in urine was 48.2%and the extraction recovery was 65.1%.The precision of the whole blood and urine samples were less than 15%.This method is rapid,simple,and suitable for determination of caffeine concentration in human whole blood and urine samples.