Zhang Hao, Dou Jianrui, Miao Runfeng, Hu Jiacai, Huo Zongli, Zhang Feng, Ji Wenliang
Jiangsu Provincial Center for Disease Control and Prevention, Nanjing, China.
Yangzhou Center for Disease Control and Prevention, Yangzhou, China.
Anal Methods. 2023 Mar 30;15(13):1668-1673. doi: 10.1039/d3ay00039g.
An analytical method for the determination of glyphosate (GLY) and aminomethylphosphoric acid (AMPA) in biological fluid samples (serum and urine) from poisoning patients using liquid chromatography-tandem mass spectrometry (LC-MS/MS) is established. After the sample pretreatment, including protein precipitation and a modified liquid-liquid extraction method, the chromatographic separation was conducted on a trifunctional modified hydrophilic column. The mobile phases in the gradient program were 2.5% formic acid aqueous solution and acetonitrile. The multiple reaction monitoring (MRM) models and the isotope-labeled internal standards were used in the acquisition process. Good linearities and satisfying recovery rates were obtained in two sample matrices with good RSDs. The detection limits of GLY and AMPA were <2 μg L, which were close to those obtained in our previous research. The established method was applied to biological samples from five patients with glyphosate intoxication. The analysis of the trend for the concentration of GLY and AMPA in two biological samples was investigated, and the difference in the downward trend of AMPA in urine was found in patients with a relatively higher concentration of GLY in serum.
建立了一种使用液相色谱-串联质谱法（LC-MS/MS）测定中毒患者生物流体样本（血清和尿液）中草甘膦（GLY）和氨甲基磷酸（AMPA）的分析方法。经过包括蛋白质沉淀和改进的液-液萃取方法在内的样本预处理后，在三功能改性亲水柱上进行色谱分离。梯度程序中的流动相为2.5%甲酸水溶液和乙腈。在采集过程中使用多反应监测（MRM）模式和同位素标记内标。在两种样本基质中获得了良好的线性和令人满意的回收率，相对标准偏差良好。GLY和AMPA的检测限<2 μg/L，与我们之前研究中获得的检测限相近。所建立的方法应用于五例草甘膦中毒患者的生物样本。研究了两种生物样本中GLY和AMPA浓度的变化趋势分析，发现血清中GLY浓度相对较高的患者尿液中AMPA下降趋势存在差异。
