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采用凝胶渗透净化(GPC)结合 GC-MS/MS 和 LC-MS/MS 分析测定脂肪基质中的农药:低压和高压 GPC 柱的比较。

Determination of pesticides in fatty matrices using gel permeation clean-up followed by GC-MS/MS and LC-MS/MS analysis: A comparison of low- and high-pressure gel permeation columns.

机构信息

Research Institute for Chromatography, President Kennedypark 26, B-8500 Kortrijk, Belgium.

Research Institute for Chromatography, President Kennedypark 26, B-8500 Kortrijk, Belgium.

出版信息

Talanta. 2017 Apr 1;165:201-210. doi: 10.1016/j.talanta.2016.12.032. Epub 2016 Dec 18.

Abstract

Two low-pressure columns (Bio-Beads SX-3) and three high-pressure GPC columns were compared for clean-up of a wide range of pesticides in fatty matrices of vegetable or animal origin. The GPC fractions were analyzed by GC-MS/MS and LC-MS/MS without additional clean-up. The performance of the GPC clean-up on the five column types was compared in terms of solvent consumption, lipid removal, pesticide recovery and repeatability. It was found that for fatty matrices, mainly consisting of high molecular weight triglycerides i.e. most vegetable oils and animal fats, good fractionation is obtained for the majority of the pesticides. On the other hand, for fats and oils containing relatively high amounts of low molecular weight triglycerides, i.e. butter fat and palm kernel oil, none of the columns provided sufficient clean-up and cause interferences and system contamination, especially in the case of GC-MS/MS analysis. For the latter case, best results in terms of lipid removal and pesticide recovery were obtained on a set (2×300mmlength) of narrow bore (7.5mm ID) columns packed with 5µm PL Gel material. Column loadability is, however, much lower on that set of columns compared the other evaluated GPC columns, impairing overall method sensitivity.

摘要

两种低压柱(Bio-Beads SX-3)和三种高压 GPC 柱被比较用于清洁各种来源的蔬菜或动物脂肪基质中的农药。GPC 馏分通过 GC-MS/MS 和 LC-MS/MS 进行分析,无需额外的净化。在溶剂消耗、脂质去除、农药回收率和重复性方面,比较了五种柱类型的 GPC 净化性能。结果表明,对于主要由高分子量三酸甘油酯(即大多数植物油和动物脂肪)组成的脂肪基质,大多数农药的分离效果良好。另一方面,对于含有相对大量低分子量三酸甘油酯的脂肪和油,即黄油脂肪和棕榈仁油,没有一种柱能够提供足够的净化效果,会导致干扰和系统污染,尤其是在 GC-MS/MS 分析的情况下。对于后一种情况,在一组(2×300mm 长度)填充有 5µm PL Gel 材料的窄口径(7.5mm ID)柱上,在脂质去除和农药回收率方面获得了最佳结果。然而,与其他评估的 GPC 柱相比,该组柱的柱载量要低得多,从而降低了整体方法的灵敏度。

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