Grupo de Análisis de Compuestos Traza, Departamento de Química Orgánica, Facultad de Química, Universidad de la República, General Flores 2124, 11700, Montevideo, Uruguay.
Graduate Program in Chemistry, Facultad de Química, Universidad de la República, Montevideo, Uruguay.
Anal Methods. 2024 Oct 31;16(42):7255-7263. doi: 10.1039/d4ay00516c.
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 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.
串联质谱仪的仪器开发促进了痕量分析有机化合物的实际趋势，发展了允许在单个分析样品中分析最多种来源污染物的方法。多类方法与世界卫生组织的“One Health”倡议保持一致，同时实现了绿色化学的理念。然而，在这个基质中，关于广泛的多类污染物分析方法的报道很少。在这项工作中，根据 DG-SANTE/11813/2021 指南，开发并验证了一种同时测定牛脂中 62 种化合物的方法。液氮研磨的脂肪用甲苯和乙腈提取。然后在低温浴中进行净化，再进行分散固相萃取。使用液相色谱法对 44 种化合物和气相色谱法对 18 种化合物进行残留测定，均采用 MRM 模式串联质谱法。该方法首先针对两种外寄生虫杀虫剂进行了开发和验证，然后扩展了分析范围，以分析 13 种兽药和 49 种农药。回收率在 60-134%之间，50%的方法范围内观察到高基质效应。大多数化合物的定量限为 10μgkg，符合国际要求。该方法应用于监测 49 个商业样品以评估其性能。80%的样品含有乙硫磷，10%的样品含有氟虫脲，均在 MRL 范围内，这突出表明需要适当的停药时间。
