QuEChERS-GC-MS/MS法测定淡水鱼中6种拟除虫菊酯的残留量

Residue analysis of 6 pyrethroids in freshwater fish by QuEChERS-gas chromatography-tandem mass spectrometry

建立了气相色谱-串联质谱法(GC-MS/MS)结合QuEChERS前处理技术检测淡水鱼(鲤鱼、鲟鱼、鲢鱼)中6种拟除虫菊酯(氯氰菊酯、溴氰菊酯、氰戊菊酯、氯氟氰菊酯、甲氰菊酯、联苯菊酯)的残留量。样品经乙腈提取,N-丙基乙二胺(PSA)和十八烷基键合硅胶(C18)粉末分散固相萃取(SPE)净化浓缩后,采用GC-MS/MS选择反应监测(SRM)模式测定,内标法定量。结果表明,6种拟除虫菊酯在3~300μg/L的质量浓度范围内,各农药峰面积与进样质量浓度间线性关系良好,决定系数>0.9995,检出限(LOD)低于0.9μg/kg,定量限(LOQ)低于3μg/kg,在添加水平分别为3μg/kg、30μg/kg及300μg/kg时,6种拟除虫菊酯的平均回收率在83%~102%之间,相对标准偏差(RSDs)在0.9%~4.9%之间。该方法简便、快速,灵敏度高,能够满足市场上淡水鱼中6种拟除虫菊酯的检测。

The residues of six pyrethroids(cypermethrin,deltamethrin,cyvalerate,cyhalothrin,fenprothrin and biphenthrin)in freshwater fish(carp,sturgeon and silver carp)were determined by GC-MS/MS combined with QuEChERS pretreatment technique.The samples were extracted by acetonitrile,purified and concentrated by dispersed solid phase extraction(SPE)with N-propyl ethylenediamine(PSA)and octadecyl bonded silica gel(C18)powder,determined by GC-MS/MS selective reaction monitoring(SRM)mode,and quantified by internal standard method.The results showed that there was a good linear relationship between the peak area and the concentration of the six pyrethroids in the concentration range of 3-300μg/L,the determination coefficient was higher than 0.9995,the limit of detection(LOD)was lower than 0.9μg/kg,and the limit of quantification(LOQ)was lower than 3μg/kg.The average recoveries of the six pyrethroids ranged from 83%-102%with RSDs of 0.9%-4.9%at 3μg/kg,30μg/kg and 300μg/kg,respectively.The method was simple,rapid and sensitive,and could be used for the determination of 6 pyrethroids in freshwater fish.