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从不同基质中提取草甘膦和氨甲基膦酸的新标准化程序:用于高效液相色谱 - 紫外检测的试剂盒

New Standardized Procedure to Extract Glyphosate and Aminomethylphosphonic Acid from Different Matrices: A Kit for HPLC-UV Detection.

作者信息

Chiara Francesco, Allegra Sarah, Arrigo Elisa, Di Grazia Daniela, Shelton Agar Francesco Maximillian Anthony, Abalai Raluca Elena, Gilardi Sara, De Francia Silvia, Mancardi Daniele

机构信息

Department of Physics, University of Trento, Via Sommarive 14, 38123 Povo, Turin, Italy.

Department of Clinical and Biological Sciences, University of Torino, San Luigi Gonzaga Hospital Regione Gonzole 10, 10043 Orbassano, Turin, Italy.

出版信息

J Xenobiot. 2025 Feb 2;15(1):23. doi: 10.3390/jox15010023.

Abstract

BACKGROUND

Glyphosate has been extensively used as herbicide since the early 1970s. The daily exposure limit is set at 0.3 mg/kg bw/d in Europe and 1.75 mg/kg bw/d in the USA. Among its derivatives, aminomethylphosphonic acid is the most stable and abundant. Understanding their biological effects then requires reliable methods for quantification in biological samples.

METHODS

We developed and validated a fast, low-cost, and reliable chromatographic method for determining glyphosate and aminomethylphosphonic acid concentrations. The validation included following parameters: specificity, selectivity, matrix effect, accuracy, precision, calibration performance, limit of quantification, recovery, and stability. Sample extraction employed an anion exchange resin with elution using hydrochloric acid 50.0 mmol/L. For HPLC analysis, analytes were derivatized, separated on a C18 column with a mobile phase of phosphate buffer (0.20 mol/L, pH 3.0) and acetonitrile (85:15), and detected at 240 nm.

RESULTS

The method demonstrated high reliability and reproducibility across various matrices. Its performance met all validation criteria, confirming its suitability for quantifying glyphosate and aminomethylphosphonic acid in different biological and experimental setups.

CONCLUSIONS

This method can offer a practical resource for applications in experimental research, medical diagnostics, quality control, and food safety.

摘要

背景

自20世纪70年代初以来,草甘膦作为除草剂被广泛使用。欧洲设定的每日暴露限值为0.3毫克/千克体重/天,美国为1.75毫克/千克体重/天。在其衍生物中,氨甲基膦酸是最稳定且含量最高的。因此,了解它们的生物学效应需要可靠的生物样品定量方法。

方法

我们开发并验证了一种快速、低成本且可靠的色谱方法,用于测定草甘膦和氨甲基膦酸的浓度。验证包括以下参数:特异性、选择性、基质效应、准确度、精密度、校准性能、定量限、回收率和稳定性。样品提取采用阴离子交换树脂,用50.0毫摩尔/升盐酸洗脱。对于高效液相色谱分析,分析物进行衍生化处理,在C18柱上用磷酸盐缓冲液(0.20摩尔/升,pH 3.0)和乙腈(85:15)的流动相进行分离,并在240纳米处检测。

结果

该方法在各种基质中都表现出高可靠性和可重复性。其性能符合所有验证标准,证实了其适用于在不同生物和实验设置中对草甘膦和氨甲基膦酸进行定量。

结论

该方法可为实验研究、医学诊断、质量控制和食品安全等应用提供实用资源。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/c28a/11856786/50a7bc549a53/jox-15-00023-g001.jpg

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