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Effect of organic matter content in the trace analysis of triazines in various types of soils with GC-NPD

机译:有机物含量对GC-NPD分析不同土壤中三嗪类微量元素的影响

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Recent work demonstrated that the combination of microwave assisted solvent extraction (MASE) and capillary gas chromatography with selective nitrogen detection (GC-NPD) is a viable approach for the efficient determination of triazine herbicides in soils. However, for soils with a high organic matter content or the injection of more concentrated extracts to obtain lower LOD's the performance of gas chromatographic analysis of uncleaned extracts is hampered. This results in both a decrease of the chromatographic response of analytes and a decrease in the life time of the column due to co-extracted matrix substances. The effect of various types of soils on the chromatographic analysis of triazine herbicides was studied. It appeared that for the investigated samples with an organic matter content below 5 % processing of uncleaned extracts is possible. Samples with a higher organic matter content required a cleanup step. A rapid procedure on 100 mg silica cartridges has been developed using solvents compatible with the MASE extracts and the instrumental analysis. Beside the testing with different standard soils, about 120 samples of an ongoing monitoring program involving three different types of soil (organic matter content: 3-37 %) were analysed. The selected compounds atrazine, desethylatrazine, desisopropyl-atrazine and simazine could be assayed in the various soil types to a level of at least 2 mu g kg(-1). For soil samples with a high organic matter content (> 5 %), the rapid cleanup procedure allowed the trace analysis of the triazines and considerably increased the life time of the capillary column. Recoveries at levels from 2 to 50 mu g kg(-1) ranged from 70 to 100 % with RSDs ranging from 5.1 to 9.5 %. Confirmation of positive samples was carried out by gas chromatography mass spectrometry. [References: 10]
机译:最近的工作表明,微波辅助溶剂萃取(MASE)和毛细管气相色谱与选择性氮检测(GC-NPD)相结合是有效测定土壤中三嗪类除草剂的可行方法。但是,对于有机物含量较高的土壤或注入更高浓度的提取物以获得较低的检测限,未清洗提取物的气相色谱分析性能会受到阻碍。由于共萃取的基质物质,这会导致分析物色谱响应的降低和色谱柱寿命的降低。研究了各种土壤对三嗪类除草剂色谱分析的影响。对于有机物含量低于5%的被调查样品,似乎可以对未清洗的提取物进行处理。有机物含量较高的样品需要净化步骤。使用与MASE提取物和仪器分析兼容的溶剂,开发了一种在100 mg硅胶柱上的快速程序。除了使用不同的标准土壤进行测试外,还对涉及三种不同类型土壤(有机物含量:3-37%)的正在进行的监测程序的约120个样品进行了分析。所选化合物阿特拉津,去乙基阿特拉津,去异丙基阿特拉津和西玛津可以在各种土壤类型中测定,含量至少为2μg kg(-1)。对于有机物含量较高(> 5%)的土壤样品,快速净化程序可对三嗪进行痕量分析,并显着增加了毛细管柱的使用寿命。回收率为2至50μg kg(-1),范围为70至100%,RSD为5.1至9.5%。阳性样品的确认通过气相色谱质谱法进行。 [参考:10]

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