Abstract

High-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (HPLC/QTOF–MS) is reported for quantitative determination of pesticide residues in apples. After a simple, rapid extraction, 300 mg MgSO₄, 50 mg primary secondary amine (PSA), and 250 mg octadecyl (C₁₈) were used for sample clean-up to ensure efficient recovery. The pesticides were quantified by HPLC/QTOF–MS using high-resolution multiple reaction monitoring (HR-MRM). Matrix-matched external standard calibration was used for quantitative analysis. The developed method was validated by spiking blank samples with the analytes and provided satisfactory accuracy verified by recoveries from 78.9% to 109.4% and good precision (relative standard deviation ≤12.4%). The limits of quantification for all analytes were between 0.85 and 3.0 µg/kg. The method was successfully applied to the analysis of forty batches of real samples, demonstrating its effectiveness for routine application.

摘要

据报道，高效液相色谱/四极杆飞行时间质谱 (HPLC/QTOF-MS) 可用于苹果中农药残留的定量测定。经过简单、快速的萃取后，加入 300 mg MgSO ₄、50 mg 伯仲胺 (PSA) 和 250 mg 十八烷基 (C ₁₈) 用于样品净化以确保有效回收。使用高分辨率多反应监测 (HR-MRM) 通过 HPLC/QTOF-MS 对农药进行定量。使用基质匹配的外标校准进行定量分析。所开发的方法通过在空白样品中加入分析物进行了验证，并通过从 78.9% 到 109.4% 的回收率和良好的精密度（相对标准偏差 ≤12.4%）提供了令人满意的准确度。所有分析物的定量限在 0.85 和 3.0 µg/kg 之间。该方法成功应用于四十批真实样品的分析，证明了其在常规应用中的有效性。