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采用多壁碳纳米管填充微柱的流动注射固相萃取法测定水中多环芳烃的气相色谱-质谱法。

Flow injection solid-phase extraction using multi-walled carbon nanotubes packed micro-column for the determination of polycyclic aromatic hydrocarbons in water by gas chromatography-mass spectrometry.

机构信息

Department of Chemistry, Xuzhou Normal University, Shanghai Road, Xuzhou 221116, China.

出版信息

J Chromatogr A. 2010 Apr 23;1217(17):2911-7. doi: 10.1016/j.chroma.2010.02.040. Epub 2010 Feb 25.

Abstract

A flow injection solid-phase extraction preconcentration system using a multi-walled carbon nanotubes (MWCNTs) packed micro-column was developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in water by gas chromatography-mass spectrometry (GC-MS). The preconcentration of PAHs on the MWCNTs was carried out based on the adsorption retention of analytes by on-line introducing the sample into the micro-column system. Methanol was introduced to elute the retained analytes for GC-MS analysis using selected ion monitoring (SIM) mode. Important influence factors were studied in detail, such as sample acidity, sample flow rate, eluent flow rate and volume, dimensions of MWCNTs and amounts of packing material. Limits of detection of 16 PAHs for an extraction of 50 mL water sample were in the range of 0.001-0.15 microg L(-1), and the precisions (RSD) were in the range of 4-14%. The optimized method was successfully applied to the determination of 16 PAHs in surface waters, with recoveries in the range of 72-93% for real spiked sample.

摘要

建立了一种基于多壁碳纳米管(MWCNTs)填充微柱的流动注射固相萃取预浓缩系统,用于通过气相色谱-质谱联用(GC-MS)测定水中的 16 种多环芳烃(PAHs)。PAHs 在 MWCNTs 上的预浓缩是基于在线将样品引入微柱系统时分析物的吸附保留来进行的。甲醇被引入以洗脱保留的分析物,然后进行 GC-MS 分析,采用选择离子监测(SIM)模式。详细研究了重要的影响因素,例如样品酸度、样品流速、洗脱液流速和体积、MWCNTs 的尺寸和填充材料的量。对于 50 mL 水样的萃取,16 种 PAHs 的检测限在 0.001-0.15 μg L(-1)范围内,精密度(RSD)在 4-14%范围内。优化后的方法成功应用于地表水 16 种 PAHs 的测定,实际加标样品的回收率在 72-93%范围内。

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