Optimization and validation of a multi-residue LC-MS/MS method for pesticides in spinach and cabbage by using Thermo Scientific Vanquish UHPLC and TSQ Quantis mass spectrometer. Sample preparation was performed using QuEChERS method that provided high recoveries for an extensive scope of pesticides in several simple steps. Data acquisition and processing were carried out using Thermo Scientific TraceFinder software. The optimized method was validated as per the SANTE guideline and applied to real samples demonstrating that the workflow is fit for purpose.
Multi-residue instrumental method that can be applied for high-throughput quantitation of pesticide residues in garlic and cumin at or below the current legislative requirements. The Thermo Scientific Orbitrap Exploris 120 mass spectrometer was operated in two different workflows: using full-scan Data-Independent Acquisition for quantitation and confirmation and using Thermo Scientific AcquireX intelligent data acquisition background exclusion workflow for full spectrum filtering, retrospective analysis, and multi-parameter-based compound identification.
Reduce post-column dispersion with small ID capillaries for fast gradient UHPLC-MS methods using sub-2 μm particle next-generation columns
本文探索了利用双三元液相色谱结合 AXP 辅助泵，实现氨基甲酸酯柱后两级衍生并荧光检测的可行性。结果表明，该方法完全可以满足 NY/T 761-2008 方法的灵敏度要求。本方法所分析的化合物中，杀线威并未包含在 NY/T 761-2008 方法中，但在色谱图中，杀线威和涕灭威砜出峰时间相近，如果二者在色谱柱上分离度差，势必会对实际样品检测有影响，因此对于色谱柱的选择非常重要；本方法中，杀线威和涕灭威砜的分离度为 1.62，可达到完全基线分离，因此该条件下 Acclaim C18, 5μm 4.6×250mm 色谱柱完全可以用于氨基甲酸酯的分析，此外选用Acclaim PAII, 5μm 4.6×250 mm 色谱柱，同样可以达到很好的分析效果。 该柱后衍生系统为实验室自己搭建，在双三元的基础上，只需额外配置一台 AXP 泵和常规柱温箱即可实现氨基甲酸酯的检测，与 Pickering 等柱后衍生仪相比，成本 大大降低，且完全满足 NY/T 761-2008 的灵敏度要求。如果用户需要更高灵敏度的分析，如环境方向，建议配置Pickering 等柱后衍生仪
We present a multi-residue instrumental method that can be applied for high-throughput screening and semi-quantitation of pesticide residues in food matrices at or below the current legislative requirements. A high-resolution, accurate-mass mass spectrometer operated in Full Scan – Variable Data-Independent Analysis (FS-vDIA)* mode provided an option for full spectrum filtering, retrospective analysis, and multi-parameter-based compound identification. The method was validated for 328 target pesticides, with an option for the future extension to a larger number. (*vDIA not available in US.)
