【摘要】 建立了QuEChERS-高效液相色谱-串联质谱法同时测定克氏原螯虾中31种杀虫剂残留，考察了不同提取液、净化剂对回收率的影响。样品采用纯乙腈提取，提取液经十八烷基键合硅胶（C18）、N-丙基乙二胺（PSA）和无水硫酸镁净化，氮吹至近干，流动相定容，以2 mmol/L甲酸铵溶液（含0.01%甲酸）-甲醇为流动相，采用Waters Acquity UPLC HSS T3色谱柱（2.1 mm×100 mm, 1.8μm）分离后，在多反应监测（MRM）模式下测定，空白基质配制标准曲线外标法定量。结果表明，31种杀虫剂在0.5～50.0μg/L内线性关系良好（r~2>0.99），检出限和定量限分别为0.1～0.3和0.4～1.0μg/kg，平均回收率为70.0%～92.4%，相对标准偏差为2.2%～9.9%。更多还原

【Abstract】 A Quechers-high performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of 31 pesticide residues in Procambarus clarkii, and the effects of different extracts and purifying agents on the recovery rate were investigated. The samples were extracted with pure acetonitrile, and the extract was purified by octadecyl bonded silica gel(C18), N-propyl ethylenediamine(PSA) and anhydrous magnesium sulfate, and diluted with mobile phase after concentration. The separation was performed on a Waters Acquity UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm) with 2 mmol/L ammonium formate solution(containing 0.01% formic acid)-methanol as the mobile phase. The detection was performed under multiple reaction monitoring(MRM) mode, and the blank matrix was prepared for standard curve external standard method.The linear relationship of 31 insecticides was good in the range of 0.5-50.0 μg/L(r~2>0.99). The limit of detection and limit of quantitation were 0.1-0.3 μg/kg and 0.4-1.0 μg/kg, respectively. The average recovery was 70.0%-92.4%, and the relative standard deviation was 2.2%-9.9%.更多还原