色谱

色谱 ›› 2014, Vol. 32 ›› Issue (9): 971-974.DOI: 10.3724/SP.J.1123.2014.05031

• 特别策划：新型污染物色谱分析专栏 • 上一篇    下一篇

生物样品二恶英分析中两个常见干扰峰的鉴定

任代卫1, 梁韬2, 黎刚1, 张海东1, 王璞1, 肖珂1, 李英明1, 张庆华1   

  1. 1. 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085;
    2. 台州市路桥污水处理有限公司, 浙江 台州 318050
  • 收稿日期:2014-05-22 修回日期:2014-07-16 出版日期:2014-09-08 发布日期:2014-08-30
  • 通讯作者: 张庆华
  • 作者简介:张庆华，qhzhang@rcees.ac.cn.
  • 基金资助:

    国家自然科学基金项目（41276195，21277165，21107121）.

Identification of two interference peaks during dioxin analysis for biological samples

REN Daiwei1, LIANG Tao2, LI Gang1, ZHANG Haidong1, WANG Pu1, XIAO Ke1, LI Yingming1, ZHANG Qinghua1   

  1. 1. State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China;
    2. Taizhou Luqiao Sewage Treatment Corporation, Taizhou 318050, China
  • Received:2014-05-22 Revised:2014-07-16 Online:2014-09-08 Published:2014-08-30

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摘要：

利用高分辨气相色谱/高分辨质谱联用仪（HRGC/HRMS）和高分辨气相色谱/低分辨质谱仪（HRGC/LRMS）对实际生物样品中二恶英（polychlorinated dibenzo-p-dioxins and dibenzofurans，PCDD/Fs）的分析过程中13C标记的2，3，7，8-四氯代二苯并呋喃（13C12-2，3，7，8-TCDF）监测碎片离子通道的两个常见干扰峰进行了分析鉴定。通过实际样品分析结果首先推测这两个干扰峰可能为有机氯农药类化合物滴滴涕（DDT）降解产物滴滴伊（DDE）的两个异构体，其次采用DDE的标准溶液（包括o，p’-DDE和p，p’-DDE）进行分析确认。通过HRGC/HRMS的色谱峰分离效果分析、色谱保留时间匹配以及与DDE碎片离子的理论丰度比进行比较，最终确认实际样品分析中的两个干扰峰依次为o，p’-DDE和p，p’-DDE。本文可为生物样品中二恶英的准确识别提供重要参考。

关键词: 滴滴伊（DDE）, 二恶英, 干扰物, 高分辨气相色谱/低分辨质谱, 高分辨气相色谱/高分辨质谱, 生物样品

Abstract:

Two interference peaks which generally appeared in company with 13C labeled 2,3,7,8-tetrachlorodibenzofuran (13C12-2,3,7,8-TCDF) in the same ion channel during dioxin analysis for biological samples were identified using high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) and high resolution gas chromatography/low resolution mass spectrometry (HRGC/LRMS). It was firstly inferred that the interference peaks should be the two isomers of dichlorodiphenyldichloroethylene (DDE), which was a breakdown product of dichlorodiphenyltrichloroethane (DDT), one of the typical organic chlorine pesticides (OCPs). Thereafter, the standard solution of DDE including o,p'-DDE and p,p'-DDE was analyzed for confirmation. By evaluation of the peak separation in HRGC/HRMS, comparison of the GC retention times and ion abundance ratios of the two interference peaks in real samples with the two DDE isomers in standard solution, the interference peaks were finally confirmed as o,p'-DDE and p,p'-DDE in sequence on a DB-5MS column. This study provided valuable information for accurate identification of dioxin compounds during the biological sample analysis.

Key words: biological samples, dichlorodiphenyldichloroethylene (DDE), high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS), high resolution gas chromatography/low resolution mass spectrometry (HRGC/LRMS), interferences, polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs)

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