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基于羧基化磁性石墨烯纳米粒子的环境水样中磺胺类抗生素的磁固相萃取。

Magnetic solid phase extraction of sulfonamides based on carboxylated magnetic graphene oxide nanoparticles in environmental waters.

机构信息

College of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou 215009, PR China; Jiangsu Key Laboratory of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou 215009, PR China.

College of Environmental Science and Engineering, Suzhou University of Science and Technology, No. 1 Kerui Road, Suzhou 215009, PR China.

出版信息

J Chromatogr A. 2018 Nov 9;1575:1-10. doi: 10.1016/j.chroma.2018.09.015. Epub 2018 Sep 8.

Abstract

A magnetic nano-adsorbent material was prepared by functionalizing carboxylic group onto the granule surface of magnetic graphene oxide nanoparticles (CMGO), using in-situ co-precipitating method. The surface morphology was characterized by SEM and TEM. The CMGO was selected as the adsorbent for the magnetic solid phase extraction (MSPE) of sulfonamides (SAs) from environmental water samples, and the eluted analytes were determined by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A series of experimental parameters were optimized to improve the extraction efficiency such as amount of CMGO, extraction time, pH, ionic strength of the sample solution and desorption conditions. When the pH of water sample was 4.00, the extraction recoveries (ERs) for SAs were over 82.0% with 15.0 mg CMGO adsorption for 20 min. Under the optimized extraction conditions, linear range was obtained with coefficients of determination (R)≥0.9983. The limits of detection for this proposed method were in the range of 0.49-1.59 ng/L, and the enrichment factors were 1320-1702 for eight SAs. The newly developed method was successfully applied to the analysis of trace SAs in real-world water samples, which provided satisfactory ERs in the range of 82.0-106.2% with RSDs less than 7.2%. Overall, it shows a great potential for the concentration of trace amine organic pollutions in complex matrices.

摘要

一种磁性纳米吸附剂材料是通过在磁性氧化石墨烯纳米颗粒(CMGO)的颗粒表面功能化羧酸基团,使用原位共沉淀法制备的。通过 SEM 和 TEM 对表面形态进行了表征。CMGO 被选为从环境水样中磁性固相萃取(MSPE)磺胺类药物(SAs)的吸附剂,洗脱的分析物通过超高效液相色谱-串联质谱法(UHPLC-MS/MS)进行测定。优化了一系列实验参数以提高萃取效率,例如 CMGO 的量、萃取时间、pH 值、样品溶液的离子强度和洗脱条件。当水样的 pH 值为 4.00 时,用 15.0mg CMGO 吸附 20min 后,SAs 的萃取回收率(ER)超过 82.0%。在优化的萃取条件下,得到了线性范围,相关系数(R)≥0.9983。该方法的检出限在 0.49-1.59ng/L 范围内,8 种磺胺类药物的富集因子为 1320-1702。新开发的方法成功应用于实际水样中痕量 SAs 的分析,在 82.0-106.2%的范围内提供了令人满意的 ER,相对标准偏差(RSD)小于 7.2%。总体而言,它在复杂基质中痕量胺类有机污染物的浓缩方面具有很大的潜力。

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