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  

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

作　　者：李翔[1] 张垚[1] 孙毅之[1] 仲维科[1] 邱月明[1] 陈彦长[1] 王大宁[1] 

机构地区：[1]中国检验检疫科学研究院,北京100025

出　　处：《色谱》2006年第4期347-350,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(No.20475051)

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0．1pg／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2d以内。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 dibenzofurans （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.

关 键 词：加速溶剂萃取 流体控制系统 高分辨气相色谱 高分辨质谱 二噁英 底泥 

分 类 号：O658[理学—分析化学]