Royer A, Beguin S, Tabet JC, Hulot S, Reding MA, Communal PY
Groupement Interregional de Recherche sur les Produits Agropharmaceutiques, Angers Technopole, Beaucouze.
Anal Chem. 2000 Aug 15;72(16):3826-32. doi: 10.1021/ac000041d.
An analytical method for the determination of glyphosate and its principal metabolite, aminomethylphosphonic acid (AMPA), in water of different hardnesses (5, 20, and 30 degrees DH, french hardness) has been developed. Samples were fortified at different levels (0.05, 0.1, 1, and 5 microg/L) and were purified by column chromatography on ion-exchange resins. After derivatization with TFAA/HFB mixture, the derivatives were quantified by using capillary gas chromatography with an ion-trap tandem mass spectrometric detector. Analytical conditions for MS/MS detection were optimized, and the quantification was carried out on the sum of areas of the three most representative ions: m/z 283, 223, and 181 for AMPA and m/z 440, 321, and 261 for glyphosate. The limit of quantification was demonstrated to be at 0.05 microg/L for each compound. The mean recovery value and the relative standard deviation (n = 65) were 93 and 12% for AMPA and 95 and 13% for glyphosate.
已开发出一种用于测定不同硬度（5、20和30度DH，法国硬度）水中草甘膦及其主要代谢物氨甲基膦酸（AMPA）的分析方法。样品在不同水平（0.05、0.1、1和5微克/升）下进行加标，并通过离子交换树脂柱色谱法进行纯化。在用TFAA/HFB混合物衍生化后，使用带离子阱串联质谱检测器的毛细管气相色谱法对衍生物进行定量。优化了MS/MS检测的分析条件，并根据三种最具代表性离子的面积总和进行定量：AMPA的m/z 283、223和181，草甘膦的m/z 440、321和261。结果表明，每种化合物的定量限均为0.05微克/升。AMPA的平均回收率和相对标准偏差（n = 65）分别为93%和12%，草甘膦的平均回收率和相对标准偏差分别为95%和13%。
