Simultaneous determination of glyphosate, glufosinate and their metabolites in soybeans using solid-phase analytical derivatization and LC-MS/MS determination

IF 6.5 1区农林科学 Q1 CHEMISTRY, APPLIED Food Chemistry: X Pub Date : 2024-09-02 DOI:10.1016/j.fochx.2024.101806

Ryoichi Sasano , Junpei Sekizawa , Isao Saito , Mikihisa Harano , Kyoka Katsumoto , Rie Ito , Yusuke Iwasaki , Takaaki Taguchi , Tomoaki Tsutsumi , Hiroshi Akiyama

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Abstract

Glyphosate and glufosinate are the most widely used herbicides worldwide. We developed a simple and rapid analytical method for detecting glyphosate, glufosinate, and their metabolites (N-acetyl glyphosate: Gly-A, N-acetyl glufosinate: Glu-A, and 3-(hydroxymethylphosphinyl)propanoic acid: MPPA) in soybeans. The method involved extraction with water, trapping in a mini-column containing polymer-based resin with strong anion exchange groups, dehydration with acetonitrile, and solid-phase analytical derivatization at ambient temperature for 1 min using N-(tert-butyldimethylsilyl)-N-methyl trifluoroacetamide (MTBSTFA), followed by Liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination. This method offers a straightforward and rapid analysis, using on-solid phase dehydration and rapid derivatization at an ambient temperature with MTBSTFA, yielding reliable results for glyphosate, glufosinate, and their metabolites. The method was applied to both domestic and imported soybean samples. Glyphosate, glufosinate, and Glu-A were detected in imported feed soybeans and processed soybean meal for feed use, reflecting the current conditions of GM soybean cultivation.

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利用固相分析衍生化和 LC-MS/MS 测定法同时测定大豆中的草甘膦、草胺膦及其代谢物

草甘膦和草铵膦是全球使用最广泛的除草剂。我们开发了一种简单快速的分析方法，用于检测草甘膦、草铵膦及其代谢物（N-乙酰草甘膦：Gly-A；N-乙酰草铵膦：Gly-A；N-乙酰草胺膦：Gly-A）：Gly-A、N-乙酰草铵膦：Glu-A）和 3-（羟甲基膦酰基）丙酸（MPPA）：MPPA）。该方法包括用水提取，在含有强阴离子交换基团聚合物树脂的微型柱中截留，用乙腈脱水，在环境温度下用 N-（叔丁基二甲基硅基）-N-甲基三氟乙酰胺（MTBSTFA）固相分析衍生 1 分钟，然后进行液相色谱-串联质谱（LC-MS/MS）测定。该方法采用固相脱水和 MTBSTFA 在常温下快速衍生的方法，可直接快速地分析草甘膦、草胺膦及其代谢物，结果可靠。该方法适用于国产和进口大豆样品。在进口饲料用大豆和加工后的饲料用豆粕中检测到了草甘膦、草胺膦和 Glu-A，反映了转基因大豆种植的现状。

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来源期刊

Food Chemistry: X CHEMISTRY, APPLIED-

CiteScore

4.90

自引率

6.60%

发文量

315

审稿时长

55 days

期刊介绍： Food Chemistry: X, one of three Open Access companion journals to Food Chemistry, follows the same aims, scope, and peer-review process. It focuses on papers advancing food and biochemistry or analytical methods, prioritizing research novelty. Manuscript evaluation considers novelty, scientific rigor, field advancement, and reader interest. Excluded are studies on food molecular sciences or disease cure/prevention. Topics include food component chemistry, bioactives, processing effects, additives, contaminants, and analytical methods. The journal welcome Analytical Papers addressing food microbiology, sensory aspects, and more, emphasizing new methods with robust validation and applicability to diverse foods or regions.