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伏安法测定河水中阿莫西林的方法开发与验证

Development and validation of voltammetric method for determination of amoxicillin in river water.

作者信息

Valenga Marcia Gabriela Pianaro, Felsner Maria Lurdes, de Matos Carolina Ferreira, de Castro Eryza Guimarães, Galli Andressa

机构信息

Universidade Estadual Do Centro-Oeste, Departamento de Química, Guarapuava, Paraná, 85040-080, Brazil.

Universidade Estadual Do Centro-Oeste, Departamento de Química, Guarapuava, Paraná, 85040-080, Brazil.

出版信息

Anal Chim Acta. 2020 Nov 22;1138:79-88. doi: 10.1016/j.aca.2020.09.020. Epub 2020 Sep 14.

Abstract

Amoxicillin is an antibiotic that can accumulate in aquatic environments and lead to the development of resistant bacteria; thus, its determination is of great importance. In this study, a glassy carbon electrode modified with reduced graphene oxide and Nafion was used as a sensor in a square-wave voltammetry method for determination of amoxicillin in river water samples from Guarapuava city, Brazil. The method was validated, using parameters and statistical tools recommended by the validation guidelines, in the range of 1.8-5.4 μmol L (r = 0.922 and R = 85.1%). The analytical curve was constructed using external standard calibration in pure electrolyte, since the matrix effect was not significant. Results of linear regression analysis, lack of fit test and analysis of the residual plots pointed that the linear regression was significant, without lack of fit of linear model and that the variances had homoscedastic distribution. Both coefficients of regression curve were significant and, thus, they were included in the regression equation: Response = 7.0 + 3.5C. The limits of detection and quantification were 0.36 and 1.2 μmol L, respectively. The method was selective towards interferents such as humic acids and benzylpenicillin. The relative standard deviations for repeatability and intermediate precision were adequate according to the limits established in literature. The mean recoveries were statistically equal to those obtained through a comparative chromatography method, so, the accuracy of the method was also adequate. Therefore, the method can be applied to the voltammetric determination of amoxicillin in river water, affording reliable and consistent measurements.

摘要

阿莫西林是一种抗生素,它会在水生环境中蓄积并导致耐药菌的产生;因此,对其进行测定非常重要。在本研究中,采用还原氧化石墨烯和Nafion修饰的玻碳电极作为传感器,运用方波伏安法测定巴西瓜拉普瓦市河水样品中的阿莫西林。按照验证指南推荐的参数和统计工具,在1.8 - 5.4 μmol/L范围内对该方法进行了验证(r = 0.922,R = 85.1%)。由于基质效应不显著,在纯电解质中采用外标校准构建分析曲线。线性回归分析、失拟检验和残差图分析结果表明,线性回归显著,线性模型不存在失拟,且方差具有同方差分布。回归曲线的两个系数均显著,因此将它们纳入回归方程:响应值 = 7.0 + 3.5C。检测限和定量限分别为0.36和1.2 μmol/L。该方法对腐殖酸和苄青霉素等干扰物具有选择性。根据文献规定的限度,重复性和中间精密度的相对标准偏差是合适的。平均回收率在统计学上与通过比较色谱法获得的回收率相等,因此该方法的准确度也合适。所以,该方法可用于河水中阿莫西林的伏安测定,能提供可靠且一致的测量结果。

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