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Quantification of endocrine disruptors and pesticides in water by gas chromatography-tandem mass spectrometry. Method validation using weighted linear regression schemes

机译:气相色谱-串联质谱法定量分析水中的内分泌干扰物和农药。使用加权线性回归方案进行方法验证

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摘要

A multi-residue methodology based on a solid phase extraction followed by gas chromatography-tandem mass spectrometry was developed for trace analysis of 32 compounds in water matrices, including estrogens and several pesticides from different chemical families, some of them with endocrine disrupting properties. Matrix standard calibration solutions were prepared by adding known amounts of the analytes to a residue-free sample to compensate matrix-induced chromatographic response enhancement observed for certain pesticides. Validation was done mainly according to the International Conference on Harmonisation recommendations, as well as some European and American validation guidelines with specifications for pesticides analysis and/or GC-MS methodology. As the assumption of homoscedasticity was not met for analytical data, weighted least squares linear regression procedure was applied as a simple and effective way to counteract the greater influence of the greater concentrations on the fitted regression line, improving accuracy at the lower end of the calibration curve. The method was considered validated for 31 compounds after consistent evaluation of the key analytical parameters: specificity, linearity, limit of detection and quantification, range, precision, accuracy, extraction efficiency, stability and robustness.
机译:建立了一种基于固相萃取然后气相色谱-串联质谱的多残留方法,用于痕量分析水中的32种化合物,包括雌激素和不同化学家族的几种农药,其中一些具有内分泌干扰特性。通过将已知量的分析物添加到无残留样品中以补偿某些农药所观察到的基质诱导的色谱响应增强,从而制备了基质标准校准溶液。验证主要根据国际协调会议的建议进行,以及根据农药分析和/或GC-MS方法规范指定的一些欧美验证指南进行。由于分析数据未满足均方差的假设,因此采用加权最小二乘线性回归程序作为一种简单有效的方法来抵消较大浓度对拟合回归线的较大影响,从而提高了校准下限的准确性曲线。在对关键分析参数进行一致评估之后,认为该方法已对31种化合物进行了验证:特异性,线性,检测和定量限,范围,精度,准确度,提取效率,稳定性和鲁棒性。

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