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Determination of six sulfonylurea herbicides in environmental water samples by magnetic solid-phase extraction using multi-walled carbon nanotubes as adsorbents coupled with high-performance liquid chromatography

机译:磁性固相萃取-多壁碳纳米管作为吸附剂-高效液相色谱法测定环境水样中的六种磺酰脲类除草剂

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摘要

Magnetic solid-phase extraction (MSPE) using magnetic multi-walled carbon nanotubes (mag-MWCNTs) as adsorbents, coupled with high-performance liquid chromatography-diode-array detector (HPLC-DAD), was developed for the simultaneous separation and determination of six types of sulfonylurea herbicides (SUs) in environmental water samples. Several variables affecting MSPE efficiency were systematically investigated, including the type and volume of desorption solvent, sample solution pH, salt concentration, amount of mag-MWCNTs, and extraction and desorption time. Response surface was employed to assist in the MSPE optimization. Under optimized conditions, excellent linearity was achieved in the range of 0.05-5.0 mu g/L for all six SUs, with coefficients of correlation r > 0.9994, and preconcentration factors ranging from 178 to 210. Limits of detection and quantification were 0.01-0.04 mu g/L and 0.03-0.13 mu g/L, respectively. The intra-day and inter-day precision (relative standard deviations, n = 6, %) at three spiked levels were 2.0-11.0% and 2.1-12.9% in terms of peak area, respectively. The method recoveries at three fortified concentrations were obtained within 76.7-106.9% for reservoir water samples and 78.2-105.4% for tap water samples. The developed MSPE-HPLC method demonstrated high sensitivity, repeatability, simplicity, rapidity, and excellent practical applicability. (C) 2016 Elsevier B.V. All rights reserved.
机译:开发了以磁性多壁碳纳米管(mag-MWCNTs)为吸附剂的磁性固相萃取(MSPE)以及高效液相色谱-二极管阵列检测器(HPLC-DAD),用于同时分离和测定环境水样品中的六种磺酰脲类除草剂(SUs)。系统地研究了影响MSPE效率的几个变量,包括解吸溶剂的类型和体积,样品溶液的pH值,盐浓度,mag-MWCNT的数量以及萃取和解吸时间。响应面用于协助MSPE优化。在优化的条件下,所有六个SU的线性均在0.05-5.0μg / L的范围内,相关系数r> 0.9994,预浓系数范围为178至210。检测和定量限为0.01-0.04 μg / L和0.03-0.13μg / L。就峰值面积而言,三个加标水平的日内和日间精度(相对标准偏差,n = 6,%)分别为2.0-11.0%和2.1-12.9%。在三种强化浓度下,对于水库水样品的方法回收率在76.7-106.9%之间,对于自来水样品的方法回收率在78.2-105.4%之间。发达的MSPE-HPLC方法显示出高灵敏度,可重复性,简单性,快速性和出色的实用性。 (C)2016 Elsevier B.V.保留所有权利。

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