Martins-Júnior Helio A, Lebre Daniel T, Wang Alexandre Y, Pires Maria A F, Bustillos Oscar V
Instituto de Pesquisas Energéticas e Nucleares, Av. Prof. Lineu Prestes 2242, Cidade Universitária, São Paulo, Brazil.
Rapid Commun Mass Spectrom. 2009 Apr;23(7):1029-34. doi: 10.1002/rcm.3960.
A simple and specific method using reversed-phase liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was investigated, which allowed the determination of residues of glyphosate and its metabolite, aminomethylphosphonic acid (AMPA), in soybean samples. An aqueous extraction with liquid-liquid partition followed by protein precipitation was performed before the LC/MS/MS determination. The quantitation of glyphosate and AMPA was performed in positive and negative ESI mode, respectively, using the multiple reaction monitoring (MRM) mode with three transitions for each analyte to enhance the specificity of the method and avoid false positives. The methodology reported in this work is capable of detecting residues of glyphosate and AMPA in soybean samples with limits of quantification of 0.30 and 0.34 mg kg(-1), respectively. This alternative method has throughput advantages such as simpler sample preparation and faster chromatographic analysis.
研究了一种使用反相液相色谱与电喷雾电离串联质谱联用（LC/ESI-MS/MS）的简单且特异的方法，该方法可用于测定大豆样品中草甘膦及其代谢物氨甲基膦酸（AMPA）的残留量。在进行LC/MS/MS测定之前，先进行液液分配的水相萃取，然后进行蛋白质沉淀。草甘膦和AMPA的定量分别在正离子和负离子电喷雾电离模式下进行，采用多反应监测（MRM）模式，每种分析物有三个跃迁，以提高方法的特异性并避免假阳性。本研究报道的方法能够检测大豆样品中的草甘膦和AMPA残留量，定量限分别为0.30和0.34 mg kg⁻¹。这种替代方法具有样品制备更简单、色谱分析更快等通量优势。
