全自动QuEChERS样品制备系统结合高效液相色谱-串联质谱法检测植物源性食品中34种农药残留

Determination of 34 pesticide residues in plant-derived foods by automated QuEChERS sample preparation system combined with high performance liquid chromatography-tandem mass spectrometry

建立了全自动QuEChERS样品制备系统结合高效液相色谱-串联质谱(HPLC-MS/MS)同时检测植物源性食品中34种农药残留的分析方法。方法利用全自动QuEChERS样品制备系统涡旋振动和离心功能,将手动QuEChERS方法中样品提取和分散固相萃取相结合;优化了操作参数及前处理步骤,在多反应监测(MRM)模式下检测,基质匹配外标法定量。从方法学验证角度对全自动QuEChERS法与手动QuEChERS法进行了比较。结果表明:该方法中大多数农药在一定范围内呈现良好的线性关系,相关系数( R 2)均大于0.99,检出限为0.76~3.60 μ g/kg ,定量限为2.28~10.80 μ g/kg ,加标回收率为53.0%~125.2%,相对标准偏差(RSD)<15.9%( n =5)。该方法与手动QuEChERS法的方法验证比对结果显示差异不明显,用于植物源性食品中多农药残留检测可有效降低劳动强度和出错概率。

An analytical method for the determination of 34 pesticide residues in plant-derived foods was established using an automated QuEChERS sample preparation system combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample extraction and dispersive solid-phase extraction in the manual QuEChERS method were combined using the vortex vibration and centrifugation functions of the automated QuEChERS sample preparation system. The operating parameters and pretreatment steps were optimized, and the analytes were detected in the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by the matrix-matched external standard method. The automated and the manual QuEChERS methods were compared from the methodological verification standpoint. The calibration curves showed good linearity in a certain range, and the correlation coefficients ( R 2) were greater than 0.99. The limits of detection and limits of quantification were 0.76-3.60 μ g/kg and 2.28-10.80 μ g/kg , respectively. Moreover, the recoveries ranged from 53.0% to 125.2%, and the relative standard deviations (RSDs) were less than 1.59%( n =5). The results obtained by the manual QuEChERS method were not significantly different from those obtained by the automated QuEChERS method. This method can effectively reduce the labor intensity and probability of error in the determination of pesticide residues.