Department of Chrono-Environment, University of Franche-Comté, UMR UFC/CNRS 6249 usc INRA, Place Leclerc, 25030 Besançon Cedex, France.
Anal Bioanal Chem. 2011 Feb;399(4):1725-32. doi: 10.1007/s00216-010-4468-z. Epub 2010 Dec 12.
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 C(18) column which permitted enhanced separation and sensitivity than a 250 mm C(18) column and increased resistance than the NH(2) 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.
分析土壤中的除草剂是一个复杂的问题，需要对现有的方法进行验证和优化。本研究开发了一种提取和分析方法，用于评估田间土壤样品中草甘膦、草铵膦和氨甲基膦酸（AMPA）的浓度。在对加速溶剂提取和超声波提取进行了测试后，选择了具有最佳回收率的搅拌提取方法。由于水作为溶剂提取时产生的色谱图更干净，杂质更少，因此优于碱性溶剂。分析采用 FMOC 柱前衍生化，然后在 300mm C（18）柱上进行高效液相色谱（HPLC）分析，与 250mm C（18）柱相比，该方法具有更好的分离度和灵敏度，并且对土壤样品的耐受力也强于 NH（2）柱。该提取和分析方法在 HPLC 荧光检测前的步骤最少，对于粘壤土，该方法具有较高的效率和灵敏度，其检测限分别为草甘膦 103μgkg（-1）、草铵膦 15μgkg（-1）和 AMPA 16μgkg（-1）。
