同位素内标液质联用法测定动物源食品中的氯丙嗪残留量

摘要

Chlorpromazine residues in animal-based food were detected by liquid chromatography-tandem mass spectrometry and quantified by using an isotope-labeled internal standard. The samples were extracted by acetonitrile and water (80/20), purified by Waters Oasis PRiME HLB column, separated by Waters ACQUITY UPLC BEH C18 column.The acetonitrile and 0.1% formic acid aqueous solution were used as the mobile phase for gradient elution. The chlorpromazine was detected by using electrospray ionization (ESI+) in positive ion mode with multiple reaction monitoring (MRM), and its quantity was analyzed by using the matrix matched calibration method combined with the stable isotope-labeled internal standard. This combined method had a good linearity in the range of 0.1~20 g/L, and its correlation coefficient was r=0.998. The mean recoveries of spiked samples at three levels (low, moderate and high) ranged from 89.1% to 93.5% with relative standard deviations (RSD) of 2.5%~4.8%. The detection limit (S/N=3)was 0.1 g/kg,and the lower limit of quantitation(S/N=10)was 0.3 g/kg.%建立测定动物源食品中氯丙嗪(Chlorpromazine)残留量的液相色谱串联质谱同位素内标方法.样品用乙腈和水(80/20)超声波提取后,用Waters Oasis PRiME HLB小柱净化,Waters ACQUITY UPLC BEH C18色谱柱分?R离.以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,用电喷雾正离子(ESI+)多反应监测、基质校准同位素内标法进行定量分析.方法在0.1~20 μg/L范围内具有良好线性,相关系数r=0.998.样品在低、中、高3个浓度水平下的平均回收率为89.1%~93.5%,相对标准偏差(RSD)为2.5%~4.8%.检出限(S/N=3)为0.1 μg/kg,定量下限(S/N=10)为0.3 μg/kg.