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采用涡旋辅助液液微萃取和气相色谱-质谱法分析水中和废水中的多氯联苯。

Analyses of polychlorinated biphenyls in waters and wastewaters using vortex-assisted liquid-liquid microextraction and gas chromatography-mass spectrometry.

机构信息

Department of Environmental Engineering, Selcuk University, Konya, Turkey.

出版信息

J Sep Sci. 2011 Mar;34(5):574-84. doi: 10.1002/jssc.201000623. Epub 2011 Jan 31.

Abstract

A method was developed for viable and rapid determination of seven polychlorinated biphenyls (PCBs) in water samples with vortex-assisted liquid-liquid microextraction (VALLME) using gas chromatography-mass spectrometry (GC-MS). At first, the most suitable extraction solvent and extraction solvent volume were determined. Later, the parameters affecting the extraction efficiency such as vortex extraction time, rotational speed of the vortex, and ionic strength of the sample were optimized by using a 2(3) factorial experimental design. The optimized extraction conditions for 5 mL water sample were as follows: extractant solvent 200 μL of chloroform; vortex extraction time of 2 min at 3000 rpm; centrifugation 5 min at 4000 rpm, and no ionic strength. Under the optimum condition, limits of detection (LOD) ranged from 0.36 to 0.73 ng/L. Mean recoveries of PCBs from fortified water samples are 96% for three different fortification levels and RSDs of the recoveries are below 5%. The developed procedure was successfully applied to the determination of PCBs in real water and wastewater samples such as tap, well, surface, bottled waters, and municipal, treated municipal, and industrial wastewaters. The performance of the proposed method was compared with traditional liquid-liquid extraction (LLE) of real water samples and the results show that efficiency of proposed method is comparable to the LLE. However, the proposed method offers several advantages, i.e. reducing sample requirement for measurement of target compounds, less solvent consumption, and reducing the costs associated with solvent purchase and waste disposal. It is also viable, rapid, and easy to use for the analyses of PCBs in water samples by using GC-MS.

摘要

建立了一种利用气相色谱-质谱法(GC-MS)通过涡旋辅助液-液微萃取(VALLME)快速测定水样中七种多氯联苯(PCBs)的方法。首先,确定了最适合的萃取溶剂和萃取溶剂体积。然后,通过使用 2(3)因子实验设计优化了影响萃取效率的参数,如涡旋萃取时间、涡旋转速和样品离子强度。对于 5 mL 水样的最佳萃取条件如下:萃取溶剂为 200 μL 氯仿;涡旋萃取时间为 3000 rpm 2 min;离心 4000 rpm 5 min,无需离子强度。在最佳条件下,7 种 PCBs 的检出限(LOD)范围为 0.36-0.73 ng/L。从三个不同的加标水平的加标水样中测定 PCBs 的平均回收率为 96%,回收率的 RSD 低于 5%。该方法成功应用于自来水和污水等实际水样中 PCBs 的测定,如水龙头水、井水、地表水、瓶装水、城市、处理后的城市和工业废水。与传统的实际水样液-液萃取(LLE)相比,对所提出方法的性能进行了比较,结果表明,该方法的效率与 LLE 相当。然而,与 LLE 相比,该方法具有减少测量目标化合物所需的样品量、减少溶剂消耗以及降低与溶剂购买和废物处理相关的成本等优点。它还适用于使用 GC-MS 分析水样中的 PCBs,快速、简单。

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