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采用QuEChERS萃取法结合超高效液相色谱/四极杆飞行时间质谱法测定小麦粉中的农药残留。

Determining pesticide residues in wheat flour by ultrahigh-performance liquid chromatography/quadrupole time-of-flight mass spectrometry with QuEChERS extraction.

作者信息

Song Nho-Eul, Kim Dan-Bi, Lim Tae-Gyu, Lee Yun-Yeol, Yoo Miyoung, Nam Tae Gyu

机构信息

Food Analysis Center, Korea Food Research Institute , Wanju , Republic of Korea.

Research Group of Traditional Food, Korea Food Research Institute , Wanju , Republic of Korea.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2019 Sep;36(9):1337-1347. doi: 10.1080/19440049.2019.1628356. Epub 2019 Jun 28.

Abstract

Pesticides are used to increase crop yields and preserve quality by protecting crops against pests; however, their overuse can adversely affect human health and the environment. Herein, we report the development of a multi-pesticide screening method using optimized QuEChERS coupled with liquid chromatography/quadrupole time-of-flight (QTOF) mass spectrometry for the analysis of 13 pesticides in wheat flour. Mass accuracies with errors of less than 2.4 ppm were obtained for all analysed pesticides, and the method provided satisfactory recovery and linearity. Repeatabilities of 0.3-12.7% and reproducibilities of 2.5-15.2% were observed in full-scan TOF mode. The performance of the developed full-scan TOF method was compared to that obtained in high-resolution multiple reaction monitoring (MRM-HR) mode. The limits of quantification for the full-scan TOF and MRM-HR modes ranged from 2 to 10, and 3 to 9 μg kg, respectively. The two quantification methods exhibited high sensitivities (limit of detections: 1-3 μg kg in full-scan TOF, and 1-3 μg kg for MRM-HR mode). No pesticide residues were detected when the developed method was applied to 22 real wheat flour samples.

摘要

农药用于通过保护作物免受害虫侵害来提高作物产量和保持品质;然而,过度使用农药会对人类健康和环境产生不利影响。在此,我们报告了一种多农药筛选方法的开发,该方法使用优化的QuEChERS结合液相色谱/四极杆飞行时间(QTOF)质谱法来分析小麦粉中的13种农药。所有分析农药的质量准确度误差均小于2.4 ppm,该方法具有令人满意的回收率和线性度。在全扫描TOF模式下,重复性为0.3 - 12.7%,重现性为2.5 - 15.2%。将所开发的全扫描TOF方法的性能与高分辨率多反应监测(MRM - HR)模式下获得的性能进行了比较。全扫描TOF和MRM - HR模式的定量限分别为2至10 μg/kg和3至9 μg/kg。这两种定量方法均表现出高灵敏度(检测限:全扫描TOF模式下为1至3 μg/kg,MRM - HR模式下为1至3 μg/kg)。当将所开发的方法应用于22个实际小麦粉样品时,未检测到农药残留。

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