Abstract：
Residues of various highly polar pesticides and their metabolites are commonly found in numerous food products. Some of these compounds, such as glyphosate, are not only used in large amounts in agriculture, but are also controversially discussed in public. Here, we present a method, employing ion chromatography (IC) coupled to tandem mass spectrometry (IC-MS/MS), for the analyses of glyphosate, aminomethyl phosphonic acid (AMPA), N-acetyl-glyphosate (NAGly), fosetyl, and 10 further highly polar pesticides and metabolites in various plant and animal matrices following a minimal sample preparation by means of the QuPPe method. Thorough investigations showed that an AS19 column enabled the analysis of all 14 compounds within 30 min. The best sensitivity could be obtained with the make-up solvent acetonitrile being admixed to the mobile phase at a 1:2 flow rate ratio. Matrix effects were thoroughly studied in terms of ion suppression and retention time shifts. Conductivity detection was used to monitor elution profiles of matrix co-extractives in comparison with matrix effect profiles obtained by continuous post-column infusion of a mix with 13 highly polar pesticides and metabolites. These tests indicated that a fivefold dilution of QuPPe extracts was suitable for the routine analysis of samples for MRL-conformity, as it considerably reduced matrix effects maintaining sufficient sensitivity and high recovery rates in eight different commodities. The suitability of the final method for its application in routine analysis was verified by the analysis of >130 samples containing incurred residues where the results were compared with two existing LC-MS/MS methods.
摘要：
各种高极性农药的残留物及其代谢物通常存在于许多食品中。其中一些化合物，比如草甘膦，不仅在农业中大量使用，但在公开场合也有争议。这里,我们提出了一种方法，采用离子色谱（IC）耦合串联质谱（IC-MS/MS），对于草甘膦的分析，氨甲基膦酸(AMPA),N-乙酰草甘膦(NAGly),Fosetyl,以及在通过QuPPe方法进行最少的样品制备之后,在各种植物和动物基质中的进一步的高极性农药和代谢物。彻底的研究表明，AS19柱可以在30分钟内分析所有14种化合物。通过将补充溶剂乙腈以1：2的流速比与流动相混合，可以获得最佳的灵敏度。在离子抑制和保留时间偏移方面对基体效应进行了彻底研究。与通过连续柱后输注13种高极性农药和代谢物的混合物获得的基体效应曲线相比，电导率检测用于监测基质共提取物的洗脱曲线。这些测试表明，QuPPe提取物的五倍稀释适用于样品的MRL符合性的常规分析，因为它大大减少了基质效应，在八种不同的商品中保持足够的灵敏度和高回收率。最终方法在常规分析中的应用的适用性通过分析>130个含有招致的残留物的样品来验证,其中结果与两种现有的LC-MS/MS方法进行比较。
