基于QuEChERS-GC-MS/MS法同时测定猕猴桃中15种有机磷农药残留

建立改良的QuEChERS方法结合气相色谱-三重四极杆串联质谱（GC-MS/MS）法同时检测猕猴桃中15种有机磷农药残留的分析方法。样品前处理采用改进的QuEChERS方法，乙腈-乙酸乙酯（1∶1，V/V）作为提取溶剂，经100 mg乙二胺-N-丙基硅烷（PSA）、200 mg十八烷基硅烷键合硅胶（C18）、40 mg石墨化碳黑（GCB）、300 mg无水硫酸镁固相分散净化，用GC-MS/MS法在多反应监测（MRM）模式下分析检测，内标法定量。结果表明，15种有机磷农药在质量浓度0.05～1.00 μg/mL范围内线性关系良好，相关系数R2均＞0.998，方法检出限为0.001 2～0.326 5 μg/kg，定量限为0.004～1.088 μg/kg；其平均加标回收率为76.95%～101.2%，精密度试验结果的相对标准偏差（RSD）（n=6）为0.21%～10.05%。该方法具有净化效果好、重复性强、灵敏度高等优势，适用于猕猴桃样品中多种农药残留的同时检测。

Simultaneous determination of 15 kinds of organophosphorus pesticides residues in kiwifruit based on QuEChERS-GC-MS/MS

A improved analysis method of QuEChERS combined with gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) was established for the simultaneous detection of 15 kinds of organophosphorus pesticides in kiwifruit (Actinidia chinensis). The sample was pretreated with improved QuEChERS method, using acetonitrile-ethyl acetate (1∶1, V/V) as the extraction solvent, and solid phase dispersion purified with ethylenediamine-N-propyl silane (PSA) 100 mg, Octaalkylsilane-bonded silica gel (C18) 200 mg, graphitized carbon black (GCB) 40 mg, anhydrous magnesium sulfate 300 mg, analyzed and detected by GC-MS/MS with multiple reaction monitoring (MRM) mode and quantified with internal standard method. The results showed that linear relationship of 15 organophosphorus pesticides was good within the mass concentration range of 0.05-1.00 μg/ml, the correlation coefficient R2 was all greater than 0.998, and the detection limit of the method was 0.001 2-0.326 5 μg/kg, the quantification limit was 0.004-1.088 μg/kg, the average spiked recovery rate was 76.95%-101.2%, and the relative standard deviation (RSD) of precision test (n=6) was 0.21%- 10.05%. The method had the advantages of good purification effect, strong reproducibility, and high sensitivity, which was suitable for simultaneous detection of multiple pesticide residues in kiwifruit samples.