分组同位素内标-超高效液相色谱-串联质谱混检快筛农产品中377种农药残留

Rapid detection of mixture of 377 pesticide residues in agricultural products by grouped isotope internal standard-ultra high performance liquid chromatography-tandem mass spectrometry

[目的]基于超高效液相色谱-串联质谱(UPLC-MS/MS),建立了分组同位素内标法定量农产品中377种农药的混样检测快速筛查方法。[方法]10个单样品组成1个混合样品,蔬菜食用菌和水果分别采用阴性叶芥菜和橙子作为标准曲线配标基质,分组同位素内标法定量。[结果]该方法混合样品的定量限为0.5~5μg/kg,方法的线性范围5~500μg/L,相关系数大于0.990。低质量分数0.5~5μg/kg的加标水平下回收率为73.9%~112.7%,变异系数为1.1%~22.3%;中质量分数10μg/kg的加标水平下回收率为70.7%~114.5%,变异系数为1.3%~17.6%;高质量分数50μg/kg的加标水平下回收率为86.4%~107.2%,变异系数为0.7%~11.0%,符合GB/T 27404—2008的要求。[结论]方法灵敏度高、准确性和稳定性好;实际检测中混检效率是常规方法的2.5~10倍,应用价值大,经济效益和社会效益显著。

[Aims] Based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),a rapid screening method through grouped isotope internal standard for the determination of 377 pesticides inagricultural products was established. [Methods] Ten samples composed a mixed sample. Negative leaf mustard andorange were used as the standard substrate for vegetables and fruits and the content of pesticide residues wasquantified with grouped isotope internal standard. [Results] The limit of quantitation of the method was 0.5-5 μg/kg,the linear range of the method was 5-500 μg/L, and the correlation coefficient was greater than 0.990. The recoverywas in the range of 73.9%-112.7% with the coefficient of variation of 1.1%-22.3% at the low spiked levels of0.5-5 μg/kg. The recovery was in the range of 70.7%-114.5% with the coefficient of variation of 1.3%-17.6% at themedium spiked levels of 10 μg /kg. The recovery was in the range of 86.4%-107.2% with the coefficient of variationof 0.7%-11.0% at the high spiked levels of 50 μg/kg, meeting the requirements of GB/T 27404-2008. [Conclusions]This method has high sensitivity, accuracy and stability. In practice, the detection efficiency is 2.5-10 times that of theconventional method, which has great application value, remarkable economic efficiency and social benefits.