数字农科院2.0

Direct determination of glyphosate and its major metabolite, aminomethylphosphonic acid, In fruits and vegetables by mixed-mode hydrophilic interaction/weak anion-exchange liquid chromatography coupled with electrospray tandem mass spectrometry

文献类型： 外文期刊

作者： Chen, Ming-Xue;Cao, Zhao-Yun;Jiang, Yan;Zhu, Zhi-Wei

作者机构：

关键词： AMPA;Direct determination;ESI-MS/MS;Glyphosate;Mixed-mode HILIC/WAX

期刊名称： JOURNAL OF CHROMATOGRAPHY A

ISSN：

年卷期：

页码：

收录情况： SCI

摘要： A novel method was developed for the direct, sensitive, and rapid determination of glyphosate and its major metabolite, aminomethylphosphonic acid (AMPA), in fruit and vegetable samples by mixed-mode hydrophilic interaction/weak anion-exchange liquid chromatography (HILIC/WAX) coupled with electrospray tandem mass spectrometry (ESI-MS/MS). Homogenized samples were extracted with water, without derivatization or further clean-up, and the extracts were injected directly onto the Asahipak NH2P-50 4E column (250mm×4.6mm i.d., 5μm). The best results were obtained when the column was operated under mixed-mode HILIC/WAX elution conditions. An initial 10-min washing step with acetonitrile/water (10:90, v/v) in HILIC mode was used to remove potentially interfering compounds, and then the analytes were eluted in WAX mode with acetonitrile and water containing 0.1molL~(-1) ammonium hydroxide under gradient elution for the ESI analysis in negative ion mode. Limits of quantification of glyphosate and AMPA were 5μgkg~(-1) and 50μgkg~(-1), respectively, with limits of detection as low as 1.2μgkg~(-1) for glyphosate and 15μgkg~(-1) for AMPA. The linearity was satisfactory, with correlation coefficients (r)>0.9966. Recovery studies were carried out on spiked matrices (6 vegetables, 3 fruits) with glyphosate at four concentrations and AMPA at three concentrations. The mean recoveries for glyphosate and AMPA were 75.3-110% and 76.1-110%, respectively, with relative standard deviations in the range of 1.1-13.8%. The intra-day precision (n=7) for glyphosate and AMPA in vegetable and fruit samples spiked at an intermediate level between 5.9% and 7.5%, and the inter-day precision over 11 days (n=11) was between 7.0% and 13%.

分类号： O65

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