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以聚苯胺@SiO@Fe为吸附剂,采用磁性固相萃取法对环境水样中的典型酚类进行HPLC分析前的灵敏测定。

Sensitive determination of typical phenols in environmental water samples by magnetic solid-phase extraction with polyaniline@SiO @Fe as the adsorbents before HPLC.

作者信息

Zhou Qingxiang, Yuan Yongyong, Wu Yalin, Liu Yongli

机构信息

Beijing Key Laboratory of Oil and Gas Pollution Control, College of Geosciences, China University of Petroleum-Beijing, Beijing, China.

出版信息

J Sep Sci. 2017 Oct;40(20):4032-4040. doi: 10.1002/jssc.201700644. Epub 2017 Aug 31.

Abstract

A novel magnetic core-shell material polyaniline@SiO @Fe (PANI@SiO @Fe) has been successfully synthesized and investigated as an effective adsorbent for the magnetic solid-phase extraction of typical endocrine disrupting compounds such as bisphenol A, tetrabromobisphenol A, and 4-nonylphenol from water samples. The morphology of the as-prepared PANI@SiO @Fe was characterized by transmission electron microscopy and X-ray diffraction. The main parameters that influenced the enrichment performance such as the kind of eluent, amount of adsorbent, volume of eluent, adsorption time, elution time, ionic strength, pH, concentration of humic acid, and sample volume were investigated. Under the optimal conditions, a good linear relationship was found in the range of 0.05-100 μg/L for bisphenol A, 0.05-300 μg/L for tetrabromobisphenol A, and 0.05-250 μg/L for 4-nonylphenol, respectively. The correlation coefficients are all above 0.995. The limits of detection were in the range of 0.009-0.04 μg/L, and precisions were under 3.73% (n = 6). The real water analysis indicated that the spiked recoveries were in the range of 92.9-98.9% (n = 3). All these results indicated that the developed method was an efficient tool for the analysis of bisphenol A, tetrabromobisphenol A, and 4-nonylphenol.

摘要

一种新型的磁性核壳材料聚苯胺@二氧化硅@铁(PANI@SiO@Fe)已成功合成,并作为一种有效的吸附剂用于从水样中磁性固相萃取典型的内分泌干扰化合物,如双酚A、四溴双酚A和4-壬基酚。通过透射电子显微镜和X射线衍射对所制备的PANI@SiO@Fe的形貌进行了表征。研究了影响富集性能的主要参数,如洗脱剂种类、吸附剂用量、洗脱剂体积、吸附时间、洗脱时间、离子强度、pH值、腐殖酸浓度和样品体积。在最佳条件下,双酚A在0.05 - 100μg/L范围内、四溴双酚A在0.05 - 300μg/L范围内、4-壬基酚在0.05 - 250μg/L范围内均呈现良好的线性关系。相关系数均高于0.995。检测限在0.009 - 0.04μg/L范围内,精密度在3.73%以下(n = 6)。实际水样分析表明,加标回收率在92.9 - 98.9%范围内(n = 3)。所有这些结果表明,所建立的方法是分析双酚A、四溴双酚A和4-壬基酚的有效工具。

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