液质联用法测定南美白对虾中84种农药残留

Determination of 84 Pesticide Residues in Penaeus vannamei by Ultra High Performance Liquid Chromatography Tandem Mass Spectrum

建立固相萃取-超高效液相色谱串联质谱法快速测定南美白对虾样品中多农药残留的分析方法。南美白对虾样品匀浆后使用80%乙腈对农药残留进行提取,加入氯化钠使乙腈与水相分层,使用固相萃取柱对提取液进行净化,氮气吹扫浓缩后复溶,并利用超高效液相色谱串联质谱进行分析。质谱仪在正离子扫描模式下进行多反应监测(MRM)检测,通过保留时间和离子碎片丰度比进行定性分析,外标法定量分析。结果表明, 65种农药回收率在80%~120%范围内,所监测的84种农药定量限在1~10μg/kg范围内, 5, 10和50μg/kg这3个添加水平上方法回收率为51.9%~132.2%,精密度(n=6)为0.13%~11.04%。经实际样品检测,市售南美白对虾中有西草净检出。该方法快速、准确、稳健,能够很好地对南美白对虾中的农药残留进行测定分析。

A solid-phase extraction-ultra high performance liquid chromatography tandem mass spectrometry method was established for the rapid determination of multiple pesticide residues in Penaeus vannamei.A total of 80% acetonitrile was used to extract the pesticide residues.Sodium chloride was added to salt out to separate the acetonitrile from the water phase,and the extract was purified with a solid phase extraction column.The samples were analyzed with UHPLC-MS/MS after concentrating and reconstituting.The mass spectrometer performs multiple reaction monitoring(MRM) detection in positive scanning mode,qualitative analysis by retention time and ion fragment abundance ratio,and quantitative analysis by an external standard method.The results showed that the quantification limits of the 84 pesticides monitored was 1-10 μg/kg,and the recovery rate of 65 pesticides out of 84 was in the range of 80% to 120%.The method total recovery rate was 51.9%-132.2% at the three addition levels of 5,10 and 50 μg/kg,and the precision was 0.13%-11.04%.Simetryne was detected in the commercially available Penaeus vannamei using the method described above.This method which was fast,accurate and robust,was suitable for the determination and analysis of pesticide residues in Penaeus vannamei.