Thompson D G, Cowell J E, Daniels R J, Staznik B, MacDonald L M
Canadian Forestry Service, Forest Pest Management Institute, Marie, Ontario.
J Assoc Off Anal Chem. 1989 Mar-Apr;72(2):355-60.
A liquid chromatographic method for determining glyphosate (GLYPH) and its major metabolite aminomethylphosphonic acid (AMPA) in various environmental substrates is described. Ion-exchange column chromatography is coupled with post-column ninhydrin derivatization and absorbance detection at 570 nm. Use of a valve-switching technique allowed quantitation of both analytes in a single chromatographic run and eliminated slow-eluting, coextracted interferences. The method was successfully used to quantitate GLYPH and AMPA in organic and mineral soils, stream sediments, and foliage of 2 hardwood brush species. Mean recovery efficiencies for GLYPH as determined from fortified blank field samples were as follows: bottom sediment 84%, suspended sediment 66%, organic soils 79%, mineral soils 73%, alder leaf litter 81%, salmonberry leaf litter 84%, and artificial deposit collectors 87%. Precision for GLYPH determination was good with less than 14% coefficient of variation on mean recovery for all substrates. Limits of detection were lowest for sediments (0.01 microgram/g dry mass) and highest for foliage substrates (0.10 microgram/g dry mass). Using this system, 6 samples/person/day were routinely analyzed.
描述了一种用于测定各种环境基质中草甘膦(GLYPH)及其主要代谢物氨甲基膦酸(AMPA)的液相色谱方法。离子交换柱色谱与柱后茚三酮衍生化和570nm处的吸光度检测相结合。使用阀切换技术可在一次色谱运行中对两种分析物进行定量,并消除了洗脱缓慢、共萃取的干扰物。该方法成功用于定量有机和矿质土壤、河流沉积物以及两种硬木灌木叶片中的草甘膦和氨甲基膦酸。从强化空白田间样品中测定的草甘膦平均回收效率如下:底部沉积物84%,悬浮沉积物66%,有机土壤79%,矿质土壤73%,桤木叶凋落物81%,美洲茶藨子叶凋落物84%,人工沉积物收集器87%。草甘膦测定的精密度良好,所有基质的平均回收率变异系数小于14%。沉积物的检测限最低(0.01微克/克干质量),叶片基质的检测限最高(0.10微克/克干质量)。使用该系统,每人每天常规分析6个样品。