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[固相萃取-高效液相色谱-质谱法测定卤水中的烷基酚和烷基酚聚乙氧基化物]

[Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry].

作者信息

Wang Jincheng, Xiong Li, Zhang Haijun, Chen Jiping

机构信息

Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.

出版信息

Se Pu. 2011 Dec;29(12):1160-4.

Abstract

A simple method based on solid phase extraction (SPE) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of octylphenol (OP), nonylphenol (NP), octylphenol ethoxylates (OPEOs) and nonylphenol ethoxylates (NPEOs) in brine. The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges. The complete separation among OP, NP, OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase. The determination was achieved using HPLC-MS with electrospray ionization (ESI) in selected ion monitoring mode. The results showed that the average recoveries of target compounds were 59.6% - 104.4% and the corresponding relative standard deviations (RSDs, n = 3) were 1.0% - 13.5%. The instrumental limits of detection for the compounds were 0.08 - 3 microg/L. This method was applied to the analysis of the samples of seawater near Dalian coast. The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.

摘要

建立了一种基于固相萃取(SPE)结合高效液相色谱 - 质谱联用(HPLC - MS)的简单方法,用于测定盐水中的辛基酚(OP)、壬基酚(NP)、辛基酚聚氧乙烯醚(OPEOs)和壬基酚聚氧乙烯醚(NPEOs)。盐水样品的萃取和净化在C18固相萃取柱上进行。以甲醇 - 水为流动相,在Hypersil GOLD分析柱上实现了OP、NP、OPEOs和NPEOs的完全分离。采用HPLC - MS在电喷雾电离(ESI)的选择离子监测模式下进行测定。结果表明,目标化合物的平均回收率为59.6% - 104.4%,相应的相对标准偏差(RSDs,n = 3)为1.0% - 13.5%。该方法对化合物的仪器检测限为0.08 - 3μg/L。该方法应用于大连海岸附近海水样品的分析。结果表明,所有样品中均检测到NP和NPEOs,其在海港和油港的浓度远高于其他采样点。

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