Simultaneous determination of the herbicides glyphosate, glufosinate and bialaphos and their metabolites by capillary gas chromatography-ion-trap mass spectrometry
Simultaneous determination of the herbicides glyphosate, glufosinate and bialaphos and their metabolites by capillary gas chromatography-ion-trap mass spectrometry
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毛细管气相色谱-离子阱质谱法同时测定除草剂草甘膦、草铵膦和双丙氨膦及其代谢物
DOI：
10.1016/0021-9673(93)83209-b
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发表时间：
1993
影响因子：
4.1
通讯作者：
N. Tsunoda
中科院分区：
文献类型：
--
作者：
N. Tsunoda
开发了一种灵敏的气相色谱（GC）-离子阱质谱（IT-MS）方法，可同时测定除草剂草甘膦、草铵膦和双丙氨膦及其主要代谢物。使用试剂 N-甲基-N-(叔丁基二甲基甲硅烷基)三氟乙酰胺在二甲基甲酰胺中于 80°C 进行单步衍生化 30 分钟，在活性氢处引入叔丁基二甲基甲硅烷基，并且每种化合物仅产生一个峰。三种除草剂的衍生物、它们的代谢物和 19 种氨基酸在 DB-1 熔融石英毛细管柱上同时进行色谱分析并在单次运行中得到很好的分离。每个叔丁基二甲基甲硅烷基化衍生物都会产生易于解释的质谱，主要由独特的 M - 15、M - 57、M - 85 和 M - 159 碎片离子主导。通过 GC-IT-MS 估计，草甘膦和草铵膦及其代谢物的检测限为 10-20 ng，双丙氨膦的检测限为 500 ng。另一方面，使用火焰离子化检测的GC分析，可检测到约100ng水平的草甘膦和草铵膦及其代谢物，但无法检测到5000ng水平的双丙氨膦。
A sensitive gas chromatographic (GC)—ion-trap mass spectrometric (IT-MS) method has been developed to determine simultaneously the herbicides glyphosate, glufosinate and bialaphos and their major metabolises. A single-step derivatization is achieved at 80°C for 30 min with the reagent N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide in dimethylformamide, which introduces thetert.-butyldimethylsilyl group at active hydrogens and gives only a single peak for each compound. The derivatives of three herbicides, their metabolises and nineteen amino acids were simultaneously chromatographed and well separated in a single run on a DB-1 fused-silica capillary column. Eachtert.-butyldimethylsilylated derivative produces an easily interpretable mass spectrum dominated by unique M - 15, M - 57, M - 85 and M - 159 fragment ions. The limits of detection were estimated to be 10–20 ng for glyphosate and glufosinate and their metabolises, and 500 ng for bialaphos, by GC-IT-MS. On the other hand, using GC analysis with flame ionization detection, glyphosate and glufosinate and their metabolises were detectable at levels of approximately 100 ng, but bialaphos could not be detected at a level of 5000 ng.