色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 474-479.DOI: 10.3724/SP.J.1123.2011.12042

• 研究论文 • 上一篇    下一篇

静态顶空气相色谱-质谱联用法快速测定海水中13种苯系物

白红妍1,2, 韩彬1*, 陈军辉1, 郑立1, 杨东方2, 王小如1   

  1. 1. 国家海洋局第一海洋研究所, 山东 青岛 266061; 2. 上海海洋大学水产与生命学院, 上海 201306
  • 收稿日期:2011-12-19 修回日期:2012-02-10 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 韩彬,硕士,助理研究员. E-mail: hanbin@fio.org.cn.
  • 基金资助:

    国家自然科学基金项目(20905017)、海洋公益性行业科研专项(201005034-03)和国家海洋局第一海洋研究所基本科研业务费专项(2010G14).

Rapid determination of benzene series in seawater by gas chromatography-mass spectrometry with static headspace extraction

BAI Hongyan1,2, HAN Bin1*, CHEN Junhui1, ZHENG Li1, YANG Dongfang2, WANG Xiaoru1   

  1. 1. First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China; 2. College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, China
  • Received:2011-12-19 Revised:2012-02-10 Online:2012-05-28 Published:2012-06-07

PDF

370

被引次数

49

摘要： 建立了静态顶空萃取、气相色谱-质谱联用(HS-GC/MS)同时测定海水中常见的痕量13种苯系物(BTEX)方法。对影响分析效果的主要条件: 色谱柱类型、升温程序、顶空平衡温度、平衡时间以及气液体积比进行了详细的分析和优化。在优化条件下,该方法的线性相关系数大于0.999,线性范围为0.16～320 μg/L,检出限(按信噪比为3计)为0.019～0.033 μg/L;水样中3个加标水平(1.6、16和160 μg/L)的回收率为81.25%～103.73%,相对标准偏差(RSD, n=6)为0.3%～4.4%。将该方法应用于上海黄浦区海水样品中苯系物的测定,结果令人满意。该方法分析时间为12 min,操作简单快捷,灵敏度高,环境友好,定性、定量准确、可靠。

关键词: 苯系物, 海水, 静态顶空萃取, 气相色谱-质谱

Abstract: A method for the simultaneous determination of 13 benzene series (BTEX) in seawater using gas chromatography-mass spectrometry with static headspace extraction (HS-GC/MS) was developed. To carefully characterize the performance of this method, several factors affecting parameters were studied in detail, such as the type of column, heating procedure, equilibrium temperature, equilibrium time and the volume ratio of gas phase to liquid phase. The optimized conditions were as follows: the polar column of DB-WAX; heating procedure, 40 ℃ kept for 4 min, then raised to 120 ℃ at 10 ℃/min, to 180 ℃ at 25 ℃/min; equilibrium temperature, 80 ℃; equilibrium time, 10 min; and the volume ratio of gas phase to liquid phase, 1:1. Under the optimized conditions, the linear equations were obtained in the concentration range of 0.16~320 μg/L with correlation coefficients greater than 0.999. The limits of detection (S/N=3) were 0.019~0.033 μg/L. The recoveries at the three spiked levels of 1.6, 16 and 160 μg/L ranged from 81.25% to 103.73% with the relative standard deviations (RSD, n=6) from 0.3% to 4.4%. The analytical results of the practical seawater samples from Shanghai Huangpu District were satisfactory. The determination of the 13 benzene series can be finished in 12 min. The method is simple, accurate, reliable, efficient and environmental-friendly.

Key words: benzene series, gas chromatography-mass spectrometry （GC-MS）, seawater, static headspace extraction

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