Kudzin Zbigniew H, Gralak Dorota K, Drabowicz Józef, Luczak Jerzy
Department of Organic Chemistry, University of Lódź, Poland.
J Chromatogr A. 2002 Feb 15;947(1):129-41. doi: 10.1016/s0021-9673(01)01603-x.
A novel approach for the simultaneous analysis of glyphosate (PMG), and aminomethylphosphonic (AMPA, GlyP), N-methylaminomethylphosphonic (MAMPA. SarP) and methylphosphonic (MPA) acids is presented. This includes a preliminary 31P NMR analysis of mixtures of PMG, MPA, AMPA and MAMPA, their further derivatization to volatile phosphonates by means of the trifluoroacetic acid-trifluoroacetic anhydride-trimethyl orthoacetate reagent and subsequent MS [chemical ionization (CI) MS, GC-CI-MS, GC-electron impact ionization MS] and/or GC-flame ionization detection (FID) analysis of the products of derivatization. The detection limits of PMG, AMPA, MAMPA and MPA by means of GC-CI-MS and GC-FID were determined. The calibration graphs (GC-FID) for these derivatives were in the range 0.1 to 100 nmol linear and sufficiently reproducible for quantitative determinations. The applicability of the method was demonstrated during the analysis of water samples fortified with PMG, AMPA and MAMPA, characterized by recoveries of >95%.
提出了一种同时分析草甘膦（PMG）、氨甲基膦酸（AMPA，甘氨酸膦）、N-甲基氨甲基膦酸（MAMPA，草铵膦）和甲基膦酸（MPA）的新方法。这包括对PMG、MPA、AMPA和MAMPA混合物进行初步的³¹P NMR分析，通过三氟乙酸-三氟乙酸酐-原乙酸三甲酯试剂将它们进一步衍生为挥发性膦酸酯，随后对衍生化产物进行质谱分析[化学电离（CI）质谱、气相色谱-化学电离质谱、气相色谱-电子轰击电离质谱]和/或气相色谱-火焰离子化检测（FID）分析。测定了通过气相色谱-化学电离质谱和气相色谱-火焰离子化检测法对PMG、AMPA、MAMPA和MPA的检测限。这些衍生物的校准曲线（气相色谱-火焰离子化检测）在0.1至100 nmol范围内呈线性，且对于定量测定具有足够的重现性。在用PMG、AMPA和MAMPA强化的水样分析过程中证明了该方法的适用性，回收率>95%。
