中文摘要：本文在9种不同色谱条件下应用LC-MS(/MS)技术检测24种极性农药，并对检测效果进行评估。结果发现：在1.8μm粒度UHPLC HILIC色谱柱条件下应用LC-MS(/MS)技术检测效果最好，可以检测出其中22种极性农药，而另外两种极性农药（草甘膦和氨甲基膦酸）只有在离子型混合模式色谱柱条件下应用LC-MS(/MS)技术进行检测。实证结果表明，UHPLC HILIC色谱柱适用于HILIC-ESI-MS/MS法测定柑橘类多种农药残留，且在大多数样本中可以检测到微克/千克水平以下的残留。
外文摘要：The aim of the study was to evaluate the performance of different chromatographic approaches for the liquid chromatography/mass spectrometry (LC-MS(/MS)) determination of 24 highly polar pesticides. The studied compounds, which are in most cases unsuitable for conventional LC-MS(/MS) multiresidue methods were tested with nine different chromatographic conditions, including two different hydrophilic interaction liquid chromatography (HILIC) columns, two zwitterionic-type mixed-mode columns, three normal-phase columns operated in HILIC-mode (bare silica and two silica-based chemically bonded columns (cyano and amino)), and two standard reversed-phase C-18 columns. Different sets of chromatographic parameters in positive (for 17 analytes) and negative ionization modes (for nine analytes) were examined. In order to compare the different approaches, a semi-quantitative classification was proposed, calculated as the percentage of an empirical performance value, which consisted of three main features: (i) capacity factor (k) to characterize analyte separation from the void, (ii) relative response factor, and (iii) peak shape based on analytes' peak width. While no single method was able to provide appropriate detection of all the 24 studied species in a single run, the best suited approach for the compounds ionized in positive mode was based on a UHPLC HILIC column with 1.8 mu m particle size, providing appropriate results for 22 out of the 24 species tested. In contrast, the detection of glyphosate and aminomethylphosphonic acid could only be achieved with a zwitterionic-type mixed-mode column, which proved to be suitable only for the pesticides detected in negative ion mode. Finally, the selected approach (UHPLC HILIC) was found to be useful for the determination of multiple pesticides in oranges using HILIC-ESI-MS/MS, with limits of quantitation in the low microgram per kilogram in most cases.
外文关键词：Polar pesticides；HILIC；Mixedmode；LC-MS；Pesticide testing；Food
作者：Andrea Vass；José Robles-Molina；Patricia Pérez-Ortega
期刊名称：ANALYTICAL AND BIOANALYTICAL CHEMISTRY
期刊影响因子：3.125
出版年份：2016
出版刊次：4
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