色谱

色谱

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加速溶剂萃取-流体控制系统净化-高分辨气相色谱/高分辨质谱定量测定底泥中的二噁英

李翔,张垚,孙毅之,仲维科,邱月明,陈彦长,王大宁

  

  1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China

  • 收稿日期:2005-08-17 修回日期:2006-01-05 出版日期:2006-07-30 发布日期:1986-12-25
  • 通讯作者: 王大宁

Determination of Polychlorinated Dibenzo-p-Dioxins and Dibenzo-Furans in Sediment by Accelerated
Solvent Extraction,Fluid Management Systems and High Resolution Gas Chromatography/High Resolution
Mass Spectrometry

LI Xiang, ZHANG Yao, SUN Yizhi, ZHONG Weike, QIU Yueming, CHEN Yanzhang, WANG Daning

  

  1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China

  • Received:2005-08-17 Revised:2006-01-05 Online:2006-07-30 Published:1986-12-25
  • Contact: Wang Daning

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摘要：

采用高分辨气相色谱/高分辨质谱(HRGC/HRMS)定量测定了底泥中的17种2,3,7,8位多氯代二噁英和呋喃(PCDD/Fs)
,并测定了四至八氯取代的二噁英和呋喃总量。样品经加速溶剂萃取,然后通过流体控制系统（FMS）自动过硅胶柱、氧化
铝柱和碳柱净化，最后浓缩。以HRGC/HRMS电压选择离子检测模式对样品中的PCDD/Fs进行了定性分析,采用同位素稀释
技术定量,该方法可精确定量到pg/g水平。结果表明该方法分析的17种二噁英和呋喃异构体的检出限可达0.1 pg/g。同
位素标准的回收率为49.8%～85.3%,样品中各异构体的回收率为93.2%～115.6%。该方法不但满足国际标准的要求,还大
大提高了分析速度,使分析周期从原来的2周缩短到2 d以内。

关键词: 底泥 , 二噁英, 高分辨气相色谱, 高分辨质谱, 加速溶剂萃取, 流体控制系统

Abstract:

A rapid, sensitive and accurate method has been developed for the determination of
seventeen 2,3,7,8-substituted congeners of polychlorinated dibenzo-p-dioxins and dibenzo-furans
(PCDD/Fs) in sediment using isotope dilution high resolution gas chromatography/high resolution mass
spectrometry (HRGC/HRMS). Dibenzo-p-dioxins and dibenzo-furans were extracted from samples by
accelerated solvent extraction (ASE) and then purified by fluid management systems (FMS) with silica
column, alumina column and carbon column. Confirmation and quantitative analysis at pg/g level of
PCDD/Fs were performed by HRGC/HRMS using voltage selective ion record (VSIR) mode. Recoveries of
fifteen isotopically labeled compound solutions (LCS) and the precision and recovery standards
(PAR) were found to be in the range of 49.8%-85.3% and 93.2%-113.8%, respectively. The detection
limits of the method for both 2,3,7,8-tetrachloro-dibenzo-furan (TCDF) and
2,3,7,8-tetrachloro-dibenzo-p-dioxin (TCDD) were determined to be 0.1 pg/g. This method not only
meets the requirements of international standards, but also shortens analysis time from 2 weeks to 2
days.

Key words: dioxin, fluid management systems (FMS), high resolution gas
chromatography (HRGC), high resolution mass spectrometry (HRMS), sediment , accelerated solvent extraction (ASE)