全二维气相色谱/飞行时间质谱法快速定性分析飞灰样品中的二噁英

Fast Qualitative Analysis of Dioxins in Fly Ash by Comprehensive Two Dimensional Gas Chromatography Coupled Time of Fight Mass Spectrometry

建立了全二维气相色谱/飞行时间质谱法(GC×GC-TOFMS)快速定性分析飞灰样品中17种二噁英的方法。实验证明,采用GC×GC二维特征谱图、TOFMS谱图库检索(自建谱库和NIST库)以及丰度比的定性手段,能在42.5min内快速分离和定性17种二英的同分异构体。本方法对大于0.5pg/μL(TCDD)的样品有较好的灵敏度。因此,在二噁英分析领域,GC×GC/TOFMS技术可以作为高分辨气相色谱/质谱(HRGC/HRMS)技术的补充和替代。

Comprehensive two dimensional gas chromatography （GC×GC-TOFMS） has been applied to fast qualitative analysis of 17 polychlorinated dibenzo-p-dioxins and dibenofurans （PCDD/Fs）.GC×GC-TOFMS parameters were evaluated and optimized to yield complete separation for 17 PCDD/Fs from interference,and to attain the high sensitivity.After optimization,all 17 PCDD/Fs were separated in 42.5 min.The critical and most toxic tetrachloro-dibenzo-p-dioxin （TCDD） detection was up to 0.5 pg/μL.The method was used to analyze a real fly ash sample.Accurate identification and determination of all analytes were by GC×GC,mass spectrum library and ion ratio.The technique could be a substitute and supplement for high resolution gas chromatography/high resolution mass spectrometry in the field of dioxin analysis.