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液相色谱-四极杆-飞行时间质谱法对谷物和豆类中农药残留的定量及确证分析

Quantitative and Confirmatory Analysis of Pesticide Residues in Cereal Grains and Legumes by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry.

作者信息

Saito-Shida Shizuka, Nemoto Satoru, Akiyama Hiroshi

机构信息

Division of Foods, National Institute of Health Sciences, Tonomachi 3-25-26, Kawasaki-ku, Kawasaki, Kanagawa 210-9501, Japan.

出版信息

Foods. 2021 Jan 3;10(1):78. doi: 10.3390/foods10010078.

Abstract

For controlling pesticide residues in food and ensuring food safety, multiresidue methods that can monitor a wide range of pesticides in various types of foods are required for regulatory monitoring. In this study, to demonstrate the applicability of liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for quantitative and confirmatory analysis of pesticide residues in cereal grains and legumes, the LC-QTOF-MS method using full-scan acquisition was validated for 151 pesticides in brown rice, soybeans, and peanuts at a spiked level of 0.01 mg/kg. With the exception of 5 out of 151 target pesticides, sufficiently high signal intensities were obtained at 0.005 μg/mL (corresponding to 0.01 mg/kg). Trueness was in the range 70-95%, with intra- and inter-day precisions below 16% and 24%, respectively, with the exception of 7 pesticides in brown rice, 10 pesticides in soybeans, and 9 pesticides in peanuts. No interfering peaks were observed near the retention times of the target pesticides. Furthermore, information on accurate fragment-ion masses obtained by a data-independent acquisition enabled unambiguous confirmation. The results suggest that the LC-QTOF-MS method is suitable for pesticide residues' analysis of cereal grains and legumes, and can be utilized for regulatory routine analysis.

摘要

为控制食品中的农药残留并确保食品安全,监管监测需要能够监测各类食品中多种农药的多残留方法。在本研究中,为证明液相色谱-四极杆飞行时间质谱(LC-QTOF-MS)用于谷物和豆类中农药残留定量和确证分析的适用性,对采用全扫描采集的LC-QTOF-MS方法在糙米、大豆和花生中添加水平为0.01 mg/kg的151种农药进行了验证。除151种目标农药中的5种外,在0.005 μg/mL(相当于0.01 mg/kg)时获得了足够高的信号强度。除糙米中的7种农药、大豆中的10种农药和花生中的9种农药外,准确度在70-95%范围内,日内和日间精密度分别低于16%和24%。在目标农药的保留时间附近未观察到干扰峰。此外,通过数据非依赖采集获得的准确碎片离子质量信息能够实现明确确证。结果表明,LC-QTOF-MS方法适用于谷物和豆类中农药残留的分析,可用于监管常规分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/dc90/7823789/dbfa594cbde1/foods-10-00078-g001.jpg

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