色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1160-1164.DOI: 10.3724/SP.J.1123.2011.01160

• 研究论文 • 上一篇    下一篇

固相萃取高效液相色谱质谱法测定海水中烷基酚和烷基酚聚氧乙烯醚

王金成1, 熊力2, 张海军1, 陈吉平1*   

  1. 1. 中国科学院大连化学物理研究所, 辽宁 大连 116023; 2. 大连工业大学, 辽宁 大连 116034
  • 收稿日期:2011-08-05 修回日期:2011-09-26 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 陈吉平,博士,研究员,博士生导师,主要从事分析化学、环境化学及相关领域的基础和应用研究. Tel: (0411)84379562,
  • 基金资助:

    科技部重大专项课题(No. 2009ZX07527-001).

Determination of Alkylphenol and Alkylphenolpolyethoxylates in Brine by SPE and LC – MS

WANG Jincheng1, XIONG Li2, ZHANG Haijun1, CHEN Jiping1*   

  1. 1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; 2. Dalian Polytechnic University, Dalian 116034, China
  • Received:2011-08-05 Revised:2011-09-26 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了固相萃取-高效液相色谱-电喷雾质谱分析海水中辛基酚、壬基酚、辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的方法。海水样品经C18固相萃取柱富集净化后,以甲醇-水为流动相,在Hypersil GOLD色谱柱上分离,电喷雾质谱在选择离子监测模式下分析目标化合物,采用外标法定量。结果表明,4种化合物的平均加标回收率为59.6%～104.4%,相对标准偏差(RSD, n=3)为1.0%～13.5%；仪器检出限为0.08～3 μg/L。将本方法用于大连海岸6个采样点海水中辛基酚、壬基酚、辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的检测发现,样品中壬基酚和壬基酚聚氧乙烯醚均有检出,且油港和海港附近海水中的含量较高。

关键词: 高效液相色谱-质谱, 固相萃取, 海水, 烷基酚, 烷基酚聚氧乙烯醚

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 μg/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.

Key words: alkylphenol, alkylphenolpolyethoxylate, high performance liquid chromatography-mass spectrometry (HPLC-MS), brine, solid phase extraction (SPE)