QuEChERS-GC-MS/MS法测定淡水鱼中6种拟除虫菊酯的残留量

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3～300 μg/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＞0.999 5，检出限（LOD）低于0.9 μg/kg，定量限（LOQ）低于3 μg/kg，在添加水平分别为3 μg/kg、30 μg/kg及300 μg/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。

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

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 3-300 μg/L, the determination coefficient was higher than 0.999 5, the limit of detection (LOD) was lower than 0.9 μg/kg, and the limit of quantification (LOQ) was lower than 3 μg/kg. The average recoveries of the six pyrethroids ranged from 83%-102% with RSDs of 0.9%-4.9% at 3 μg/kg, 30 μg/kg and 300 μg/kg, respectively. The method was simple, rapid and sensitive, and could be used for the determination of 6 pyrethroids in freshwater fish.