Bressán I G, Llesuy S F, Rodriguez C, Ferloni A, Dawidowski A R, Figar S B, Giménez M I
Laboratory of Mass Spectrometry, Hospital Italiano de Buenos Aires, Buenos Aires, Argentina; Department of Chemistry, Instituto Universitario Escuela de Medicina del Hospital Italiano, Buenos Aires, Argentina.
Department of Chemistry, Instituto Universitario Escuela de Medicina del Hospital Italiano, Buenos Aires, Argentina.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 May 1;1171:122616. doi: 10.1016/j.jchromb.2021.122616. Epub 2021 Mar 5.
In 2015, glyphosate was classified as "Group 2A - probably carcinogenic to humans" by the International Agency for Research on Cancer (IARC). Therefore, public concerns about the environmental and health risks of this substance have rapidly increased. Considering its toxicokinetic characteristics, urinary levels of glyphosate could be a powerful tool for human biomonitoring. Nevertheless, the physicochemical properties of this molecule and the complexity of the matrix make this purpose particularly challenging. In order to solve this problem, the presented study describes a simple LC-MS/MS method for the quantification of glyphosate in human urine after pre-column derivatization with FMOC-Cl. Method development was focused on the optimization of the derivatization reaction in human urine, adjusting critical variables such as pH of borate buffer, FMOC-Cl concentration and derivatization time. Besides, chromatographic separation and spectrometric parameters were also established. The analytical method was fully validated according international guidelines for selectivity, carry over, linearity, accuracy, precision, lower limit of quantitation, matrix effect and stability under different conditions. All performance parameters were within the acceptance criteria. In addition, the method was successfully applied to 52 urine samples obtained from exposed subjects from northern Argentina, laying the foundation for future epidemiological studies.
2015年，国际癌症研究机构（IARC）将草甘膦归类为“2A组——可能对人类致癌”。因此，公众对该物质的环境和健康风险的担忧迅速增加。考虑到其毒代动力学特征，草甘膦的尿液水平可能是人体生物监测的有力工具。然而，该分子的物理化学性质和基质的复杂性使得这一目标极具挑战性。为了解决这个问题，本研究描述了一种简单的液相色谱-串联质谱法，用于在使用氯甲酸芴甲酯（FMOC-Cl）进行柱前衍生后定量测定人尿中的草甘膦。方法开发侧重于优化人尿中的衍生化反应，调整关键变量，如硼酸盐缓冲液的pH值、FMOC-Cl浓度和衍生化时间。此外，还确定了色谱分离和光谱参数。该分析方法根据国际指南对选择性、残留、线性、准确性、精密度、定量下限、基质效应和不同条件下的稳定性进行了全面验证。所有性能参数均在可接受标准范围内。此外，该方法成功应用于从阿根廷北部暴露人群中获得的52份尿液样本，为未来的流行病学研究奠定了基础。
