Department of Environment and Primary Industries, Farming Systems Research Division, TER 4 Ernest Jones Drive, Macleod 3085, Victoria, Australia; Centre for Aquatic Pollution Identification and Management (CAPIM), c/o School of Chemistry, The University of Melbourne, Parkville 3010, Victoria, Australia.
Department of Environment and Primary Industries, Farming Systems Research Division, TER 4 Ernest Jones Drive, Macleod 3085, Victoria, Australia; Centre for Aquatic Pollution Identification and Management (CAPIM), c/o School of Chemistry, The University of Melbourne, Parkville 3010, Victoria, Australia.
J Chromatogr A. 2014 Jan 17;1325:56-64. doi: 10.1016/j.chroma.2013.12.021. Epub 2013 Dec 16.
The method presented uses a mixed-mode anion exchange SPE and liquid chromatography tandem mass spectrometry to analyze 5 sulfonylurea, 8 phenoxy acid, 12 triazine and 6 other herbicides in environmental waters. The mixed-mode SPE cartridge is able to retain a wide range of herbicides with acidic-neutral-basic characteristics, particularly the highly polar and acidic compounds clopyralid, dicamba and picloram. The neutral and basic herbicides can be effectively eluted with methanol, after which the acidic herbicides can be eluted using acidified methanol. The method has achieved an LOD of 0.7-3ng/L for the sulfonylureas, 4-12ng/L for the phenoxy acids and 0.4-30ng/L for the triazine and additional herbicides, with recoveries in the range 76-107%, 73-126%, and 65-104%, respectively. The precision of the method, calculated as relative standard deviation (RSD), was below 10% for both sulfonylurea and phenoxy acid herbicides, and less than 20% for the remaining herbicides. The developed method was used to determine the concentration of target herbicides in a range of environmental waters, and many of the target herbicides were detected at ng/L level.
本方法采用混合模式阴离子交换固相萃取和液相色谱串联质谱法，分析环境水中的 5 种磺酰脲类、8 种苯氧羧酸类、12 种三嗪类和 6 种其他除草剂。混合模式固相萃取小柱能够保留具有酸性-中性-碱性特性的广泛范围的除草剂，特别是高度极性和酸性的化合物氯吡嘧磺隆、二甲四氯和草甘膦。中性和碱性除草剂可以用甲醇有效洗脱，然后用酸化甲醇洗脱酸性除草剂。该方法对磺酰脲类、苯氧羧酸类和三嗪及其他除草剂的检出限为 0.7-3ng/L、4-12ng/L 和 0.4-30ng/L，回收率分别为 76-107%、73-126%和 65-104%。该方法的精密度（以相对标准偏差表示），磺酰脲类和苯氧羧酸类除草剂均低于 10%，其余除草剂低于 20%。所建立的方法用于测定一系列环境水中目标除草剂的浓度，许多目标除草剂以 ng/L 水平检出。
