Central Institute of the Bundeswehr Medical Service Koblenz, Laboratory Department of Food and Environmental Chemistry, Koblenz, Germany.
J Sep Sci. 2010 Apr;33(8):1139-46. doi: 10.1002/jssc.200900556.
For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission.
为了测定饮用水中的草甘膦、氨甲基膦酸和草铵膦,使用阴离子交换或 SPE 对不同的富集和净化程序进行了考察。在许多情况下,在富集和净化过程中,例如碱性土金属离子(尤其是钙)的相互作用会导致分析物的损失。因此,本研究开发了一种使用阳离子交换树脂测定这些膦酸类除草剂的新型净化和富集程序。总的来说,本研究中开发的阳离子交换树脂净化程序避免了上述相互作用,适用于富钙饮用水样品。用 9-芴甲基氯甲酸酯衍生化后,用 LC 荧光检测,草甘膦、氨甲基膦酸和草铵膦的 LOD 分别为 12、14 和 12ng/L,从实际饮用水样品中的平均回收率分别为 98+/-9%、100+/-16%和 101+/-11%。低的 LOD 和高的精密度允许根据欧洲委员会的指南分析这些膦酸类除草剂。