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首页> 外文期刊>Analytical and bioanalytical chemistry >Optimization of extraction procedure and chromatographic separation of glyphosate, glufosinate and aminomethylphosphonic acid in soil
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Optimization of extraction procedure and chromatographic separation of glyphosate, glufosinate and aminomethylphosphonic acid in soil

机译:土壤中草甘膦,草铵膦和氨基甲基膦酸的提取工艺优化及色谱分离

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摘要

Analysing herbicides in soil is a complex issue that needs validation and optimization of existing methods. An extraction and analysis method was developed to assess concentrations of glyphosate, glufosinate and aminomethylphophonic acid (AMPA) in field soil samples. After testing extractions by accelerated solvent extraction and ultrasonic extraction, agitation was selected with the best recoveries. Water was preferred as solvent extraction because it resulted in a cleaner chromatogram with fewer impurities than was the case with alkaline solvents. Analysis was performed by FMOC pre-column derivatization followed by high-performance liquid chromatography (HPLC) on a 300 mm C18 column which permitted enhanced separation and sensitivity than a 250 mm C18 column and increased resistance than the NH2 column for soil samples. This extraction and analysis method allowing a minimum of steps before the injection in the HPLC with fluorescence detection is efficient and sensitive for a clay-loamy soil with detection limits of 103 μg kg-1 for glyphosate, 15 μg kg-1 for glufosinate and 16 μg kg-1 for AMPA in soil samples.
机译:分析土壤中的除草剂是一个复杂的问题,需要对现有方法进行验证和优化。开发了一种提取和分析方法,以评估田间土壤样品中草甘膦,草铵膦和氨基甲基膦酸(AMPA)的浓度。在通过加速溶剂萃取和超声萃取对萃取进行测试之后,选择了具有最佳回收率的搅拌。优选水作为溶剂萃取,因为与碱性溶剂相比,其色谱图更干净,杂质更少。通过FMOC柱前衍生化,然后在300 mm C18色谱柱上进行高效液相色谱(HPLC)进行分析,与250 mm C18色谱柱相比,该色谱柱的分离度和灵敏度更高,与土壤样品相比,与NH2色谱柱相比,其耐受性更高。这种萃取和分析方法可在HPLC进样前进行最少的步骤,并具有荧光检测功能,对粘土-壤土质高效且灵敏,草甘膦的检出限为103μgkg-1,草铵膦的检出限为15μgkg-1,16土壤样品中AMPA的微克kg-1。

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