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自动QuEChERS样品制备系统结合高效液相色谱-串联质谱法测定植物性食品中的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].

作者信息

Chen Ting, Xu Yanli, Zhang Wen, Yan Jun, Peng Tao

机构信息

Lanzhou Institutes for Food and Drug Control, Lanzhou 730050, China.

出版信息

Se Pu. 2019 Sep 8;37(9):1019-1025. doi: 10.3724/SP.J.1123.2019.02010.

Abstract

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 () were greater than 0.99. The limits of detection and limits of quantification were 0.76-3.60 μg/kg and 2.28-10.80 μg/kg, respectively. Moreover, the recoveries ranged from 53.0% to 125.2%, and the relative standard deviations (RSDs) were less than 1.59% (=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.

摘要

建立了一种使用自动QuEChERS样品制备系统结合高效液相色谱 - 串联质谱法(HPLC - MS/MS)测定植物源性食品中34种农药残留的分析方法。利用自动QuEChERS样品制备系统的涡旋振动和离心功能,将手动QuEChERS方法中的样品提取和分散固相萃取相结合。对操作参数和预处理步骤进行了优化,并在多反应监测(MRM)模式下检测分析物。采用基质匹配外标法进行定量分析。从方法学验证的角度对自动和手动QuEChERS方法进行了比较。校准曲线在一定范围内呈现良好的线性,相关系数()大于0.99。检测限和定量限分别为0.76 - 3.60μg/kg和2.28 - 10.80μg/kg。此外,回收率在53.0%至125.2%之间,相对标准偏差(RSD)小于1.59%(=5)。手动QuEChERS方法获得的结果与自动QuEChERS方法获得的结果无显著差异。该方法可有效降低农药残留测定中的劳动强度和误差概率。

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