QuEChERS-HPLC-MS/MS法检测谷物运动营养粉中40种农药残留

Determination of 40 pesticide residues in cereal sports nutrition powder by QuEChERS-HPLC-MS/MS

建立了高效液相色谱-串联质谱法结合改良的QuEChERS技术对谷物运动营养粉中40种农药残留的分析方法。样品前处理采用改良的QuEChERS方法,用乙腈-丙酮(2∶1,v/v)作为样品农药残留提取溶剂,经乙二胺-N-丙基硅烷(PSA,80 mg)、十八烷基硅烷键合硅胶(C_(18),160 mg)、石墨化碳黑(GCB,60 mg)、无水硫酸镁(300 mg)固相分散净化,浓缩定容后用HPLC-MS/MS在多反应监测模式下分析检测,外标法定量。所测农药在配制工作曲线液内线性关系良好,相关系数均大于0.995,检出限为0.0019~0.0745μg/kg,分别向样品中添加40种农药标准品浓度为25、75和150μg/kg的3个水平,其加标平均回收率为76.78%~109.78%,相对标准偏差为0.25%~11.12%(n=6)。结果表明该方法操作便捷、快速高效、重复性强、灵敏度高等优势,适用于谷物运动营养粉中40种农药同时检测。

A HPLC-MS/MS combined with the improved QuEChERS method was established to simultaneously detect the multi-residues of 40 pesticides in grain-derived foods.The modified QuEChERS method was used in samples pretreatment,using acetonitrile-acetone(2∶1,v/v)as the extraction solvent of pesticide residues in the sample,the pesticide residues were purified by solid-phase dispersion of 80 mg of ethylenediamine-N-propylsilane(primary secondary amine,PSA),160 mg octadecyl silane-bonded silica gel(C_(18)),60 mg graphitized carbon black(GCB),and 300 mg anhydrous magnesium sulfate,concentrated to constant volume,analyzed and detected by HPLC-MS/MS in multiple reaction monitoring mode(multiple reaction monitoring,MRM),and quantified by external standard method.The tested pesticides had good linear relationship in the preparation working curve solution.the correlation coefficient(r2)was greater than 0.995,the detection limit was 0.0019~0.0645μg/kg,40 kinds of pesticide standards were added to the samples with a concentration of 25μg/kg,75μg/kg and 150μg/kg respectively,and the average recovery rates of spiking were 76.78%~109.78%,and the relative standard deviations(RSDs)were 0.25%~11.12%(n=6).The results showed that the method had the advantages of convenient operation,fast and efficient,strong repeatability and high sensitivity,and was suitable for the simultaneous detection of 40 pesticides in cereal sports nutrition powder.