开发一种新颖实用的方法,用于同时分析牛脂肪中的多类污染物

IF 2.7 3区 化学 Q2 CHEMISTRY, ANALYTICAL
Rodrigo Souza, Natalia Gérez García, Natalia Besil, Maria Veronica Cesio, Horacio Heinzen, Maria Lucia Pareja
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引用次数: 0

摘要

串联质谱仪的仪器发展促进了有机化合物痕量分析的实际趋势,即开发可在单一分析样本中分析来源最多样化的污染物的方法。多类别方法符合 "谁的健康谁负责 "倡议,同时也实现了绿色化学的概念。然而,目前还很少有关于在这种基质中分析污染物的大范围多类别方法的报道。本研究根据 DG-SANTE/11813/2021 指南,开发并验证了同时测定牛脂肪中 62 种化合物的方法。液氮研磨脂肪用甲苯和乙腈提取。然后在低温槽中进行净化,接着进行分散固相萃取。使用液相色谱法测定 44 种化合物的残留量,使用气相色谱法测定 18 种化合物的残留量,两种方法均与 MRM 模式下的串联质谱联用。该方法首先针对两种体外寄生虫药物进行了开发和验证,随后又扩展到 13 种兽药和 49 种农药的分析。该方法的回收率在 60-134% 之间,50% 的分析范围存在基质效应。大多数化合物的定量限为 10 µg kg-1,符合国际要求。为评估该方法的性能,对 49 份商业样品进行了监测。80%的样品中含有乙硫磷,10%的样品中含有氟脲,两者均在最高残留限量范围内,这突出表明了适当停药时间的必要性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Development of a novel and useful methodology for the simultaneous analysis of multiclass contaminants in bovine fat
The instrumental development of tandem mass spectrometers fosters the actual trend in the trace analysis of organic compounds to the development of methods that allow the analysis of contaminants of the most diverse origin in a single analytical sample. The multiclass methods are aligned with the Who´s One Health initiative while accomplishing the concepts of green chemistry. However, there are few reports of wide scope multiclass methods for the analysis of contaminants in this matrix. In this work, a method for the simultaneous determination of 62 compounds in bovine fat, was developed and validated following DG-SANTE/11813/2021 guidance. Liquid nitrogen milled fat was extracted with toluene and acetonitrile. Then a clean-up in a cryogenic bath, followed by dispersive solid phase extraction was performed. Residue determination was done using liquid chromatography for 44 compounds and gas chromatography for 18 compounds, both coupled to tandem mass spectrometry in MRM mode. The method was first developed and validated for two ectoparasiticides, then the scope was expanded for the analysis of 13 veterinary drugs and 49 pesticides. Recovery percentages were in the range of 60-134%, high matrix effect was observed in 50% of the scope of the method. Most compounds presented limits of quantification of 10 µg kg-1 in compliance with international requirements. The method was applied to monitor 49 commercial samples to evaluate its performance. Eighty percent of samples contained ethion and 10% had fluazuron, both within MRLs, highlighting the need for proper withdrawal times.
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来源期刊
Analytical Methods
Analytical Methods CHEMISTRY, ANALYTICAL-FOOD SCIENCE & TECHNOLOGY
CiteScore
5.10
自引率
3.20%
发文量
569
审稿时长
1.8 months
期刊介绍: Early applied demonstrations of new analytical methods with clear societal impact
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