液相色谱-质谱联用和气相色谱-质谱联用检测蜂蜜中农药的方法优化
Optimization of Method for Pesticide Detection in Honey by Using Liquid and Gas Chromatography Coupled with Mass Spectrometric Detection.
作者信息
Almeida Mariana O, Oloris Silvia Catarina S, Faria Vanessa Heloisa F, Ribeiro Márcia Cassimira M, Cantini Daniel M, Soto-Blanco Benito
机构信息
Instituto Otávio Magalhães, Fundação Ezequiel Dias (Funed), Rua Conde Pereira Carneiro 80, Belo Horizonte 30510-010, MG, Brazil.
Departamento de Clínica e Cirurgia Veterinárias, Escola de Veterinária, Universidade Federal de Minas Gerais (UFMG), Avenida Antônio Carlos 6627, Belo Horizonte 30123-970, MG, Brazil.
出版信息
Foods. 2020 Sep 26;9(10):1368. doi: 10.3390/foods9101368.
Abstract
This study aimed to optimize and validate a multi-residue method for identifying and quantifying pesticides in honey by using both gas and liquid chromatographic separation followed by mass spectrometric detection. The proposed method was validated to detect 168 compounds, 127 of them by LC-MS/MS (liquid chromatography tandem mass spectrometric detection) and 41 by GC-MS/MS (gas chromatography tandem mass spectrometric detection). The limit of detection (LOD) and limit of quantification (LOQ) values for the analytes determined by LC-MS/MS were 0.0001-0.0004 mg/kg and 0.0002-0.0008 mg/kg, respectively. For GC-MS/MS analyses, the LOD and LOQ values were 0.001-0.004 mg/kg and 0.002-0.008 mg/kg. In total, 33 samples of commercial honey produced by apiaries in six Brazilian states were analyzed with the validated method. Residual amounts of 15 analytes were detected in 31 samples (93.9%). The method described in the present study was able to detect an extensive and broad range of pesticides with very high sensitivity.
摘要
本研究旨在优化并验证一种多残留方法，该方法通过气相色谱和液相色谱分离，随后进行质谱检测，来鉴定和定量蜂蜜中的农药。所提出的方法经验证可检测168种化合物，其中127种通过液相色谱-串联质谱检测（LC-MS/MS），41种通过气相色谱-串联质谱检测（GC-MS/MS）。通过LC-MS/MS测定的分析物的检测限（LOD）和定量限（LOQ）值分别为0.0001 - 0.0004 mg/kg和0.0002 - 0.0008 mg/kg。对于GC-MS/MS分析，LOD和LOQ值分别为0.001 - 0.004 mg/kg和0.002 - 0.008 mg/kg。总共使用经过验证的方法分析了巴西六个州养蜂场生产的33个商业蜂蜜样品。在31个样品（93.9%）中检测到15种分析物的残留量。本研究中描述的方法能够以非常高的灵敏度检测广泛的农药。
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