Development and validation of rapid technique for trace level quantification of glyphosate and AMPA in water using LC-TQ MS

IF 8.2 1区环境科学与生态学 Q1 ENVIRONMENTAL SCIENCES

Science of the Total Environment Pub Date : 2025-04-20 DOI:10.1016/j.scitotenv.2025.179421

Subhajit Rakshit , Sumit Shekhar , Sudama Ram Sahu , Soumyajit Ghoshal , Neethu Narayanan , Neera Singh , Tirthankar Banerjee

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Abstract

Glyphosate, an age-old herbicide has now become an emerging concern to mankind because several case reports are there regarding the presence of this contaminant in different water resources along with its toxic metabolite, aminomethylphosphonic acid (AMPA). Furthermore, the International Agency for Research on Cancer (IARC) categorized glyphosate as “probably carcinogenic to humans” in 2015. In this scenario, a validated mass confirmatory method using the Agilent 6470 LC/TQ instrument has been developed to detect and quantify these contaminants at μg L⁻¹ levels in water. The proposed method includes the usage of only one mL of the water sample, a 30-min derivatization step with 9-FMOC-Cl [(9H-Fluoren-9-yl)methyl carbonochloridate], and clean up with dichloromethane (DCM). The developed method is time-saving and less laborious than the conventional methods for the analysis of the contaminants in water. The method validation parameters, like linearity, selectivity, accuracy, and intermediate precision, are satisfactory. Method LOQ (Limit of quantification) for glyphosate-FMOC and AMPA-FMOC was 0.05 μg L⁻¹ and 0.5 μg L⁻¹, respectively. The method can be used for routine monitoring of glyphosate and AMPA residues at very low level in different kinds of water like drinking water, packaged drinking water, irrigation water etc.

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LC-TQ质谱快速定量水中草甘膦和AMPA技术的建立与验证

草甘膦是一种古老的除草剂，现在已经成为人类关注的新问题，因为有几例报告表明，在不同的水资源中存在这种污染物及其有毒代谢物氨基甲基膦酸（AMPA）。此外，国际癌症研究机构（IARC）在2015年将草甘膦归类为“可能对人类致癌”。在这种情况下，使用Agilent 6470 LC/TQ仪器开发了一种经过验证的质量验证方法，用于检测和量化水中μg L−1水平的这些污染物。所提出的方法包括仅使用1 mL水样，用9-FMOC-Cl [（9h -芴-9-酰基）氯化甲酯进行30分钟衍生化步骤，并用二氯甲烷（DCM）进行清理。该方法比传统的水中污染物分析方法省时、省力。方法的线性度、选择性、准确度、中间精密度等验证参数均令人满意。方法草甘膦- fmoc和AMPA-FMOC的定量限分别为0.05 μg L−1和0.5 μg L−1。该方法可用于饮用水、包装饮用水、灌溉水等不同种类水中极低水平草甘膦和AMPA残留的常规监测。

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来源期刊

Science of the Total Environment 环境科学-环境科学

CiteScore

17.60

自引率

10.20%

发文量

8726

审稿时长

2.4 months

期刊介绍： The Science of the Total Environment is an international journal dedicated to scientific research on the environment and its interaction with humanity. It covers a wide range of disciplines and seeks to publish innovative, hypothesis-driven, and impactful research that explores the entire environment, including the atmosphere, lithosphere, hydrosphere, biosphere, and anthroposphere. The journal's updated Aims & Scope emphasizes the importance of interdisciplinary environmental research with broad impact. Priority is given to studies that advance fundamental understanding and explore the interconnectedness of multiple environmental spheres. Field studies are preferred, while laboratory experiments must demonstrate significant methodological advancements or mechanistic insights with direct relevance to the environment.