首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Rapid determination of glyphosate, glufosinate, bialaphos, and their major metabolites in serum by liquid chromatography-tandem mass spectrometry using hydrophilic interaction chromatography
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Rapid determination of glyphosate, glufosinate, bialaphos, and their major metabolites in serum by liquid chromatography-tandem mass spectrometry using hydrophilic interaction chromatography

机译:液相色谱-串联质谱/亲水相互作用色谱法快速测定血清中的草甘膦,草铵膦,双丙氨磷及其主要代谢物

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摘要

We developed a simple and rapid method for the simultaneous determination of phosphorus-containing amino acid herbicides (glyphosate, glufosinate, bialaphos) and their major metabolites, aminomethylphosphonic acid (AMPA) and 3-methylphosphinicopropionic acid (MPPA), in human serum. Serum samples were filtrated through an ultrafiltration membrane to remove proteins. The filtrate was then washed with chloroform, and injected into a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. Chromatographic separation was achieved on a hydrophilic interaction chromatography (HILIC) column. Determination of the target herbicides and metabolites was successfully carried out without derivatization or solid phase extraction (SPE) cartridge clean-up. The recoveries of these compounds, added to human serum at 0.2. μg/mL, ranged from 94% to 108%, and the relative standard deviations (RSDs) were within 5.9%. The limits of detection (LODs) were 0.01. μg/mL for MPPA, 0.02. μg/mL for AMPA, 0.03. μg/mL for both glyphosate and glufosinate, and 0.07. μg/mL for bialaphos, respectively.
机译:我们开发了一种简单而快速的方法,可同时测定人血清中的含磷氨基酸除草剂(草甘膦,草铵膦,双丙氨磷)及其主要代谢产物氨基甲基膦酸(AMPA)和3-甲基膦酸丙酸(MPPA)。血清样品通过超滤膜过滤以去除蛋白质。然后将滤液用氯仿洗涤,并注入液相色谱-串联质谱(LC-MS / MS)系统中。在亲水相互作用色谱(HILIC)柱上进行色谱分离。无需衍生化或固相萃取(SPE)纯化柱即可成功完成目标除草剂和代谢物的测定。这些化合物的回收率以0.2加入人血清中。 μg/ mL,范围从94%到108%,相对标准偏差(RSD)在5.9%以内。检出限(LOD)为0.01。 MPPA的微克/毫升,0.02。 AMPA的微克/毫升,0.03。草甘膦和草铵膦的微克/毫升均为0.07。双丙氨磷的微克/毫升。

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