全二维气相色谱/飞行时间质谱法定性筛查鱼肉组织中含卤有机污染物

采用全二维气相色谱/飞行时间质谱(GC×GC-TOFMS),建立了鱼肉样品中含卤有机污染物的定性和定量分析方法.鱼肉样品用正己烷丙酮(1∶1,V/V)提取,凝胶色谱和复合硅胶柱净化,浓缩富集,全二维气相色谱联用飞行时间质谱(DB-5MS毛细管色谱柱联HT-8色谱柱)检测.软件自动识别后,经三步筛查,共鉴定出含氯或溴化合物72种,其中包括33种多氯联苯,9种有机氯农药,4种多溴联苯醚,4种DDT代谢产物,2种氯代茴香醚,2种氯苯乙烯,1种氯代茴香硫醚及1种甲基三氯生.另外,从质谱信息上看,有16种化合物明显含氯或含溴,但是因为缺少必要的谱库信息不能准确识别.采用外标定量法,对鱼肉样品中检出的主要的10种多氯联苯和1种多溴联苯醚进行了准确定量分析.

Qualitative Analysis of Some Emerging Halogenous Pllutions in Fish Sample by Comprehensive Two-Dimensional Gas Chromatography/Time-of-Flight Mass Spectrometry

Numerous halogenated organic compounds have been identified as pollutants of concern.However,the release to the environment of many remains largely unrecognized.In this study,the comprehensive two dimensional gas chromatography/time of flight mass spectrometry(GC×GC-TOF-MS) was applied to no-target screening halogenous pollutions in fish sample.After extracting with hexane and actone(1:1,V/V),cleaning-up with gel permeation chromatography(GPC) and silica gel packed column,the residues were redissolved in the hexane and analyzed by GC×GC-TOF MS coupled with DB-5MS and column HT-8 column.In total,72 compounds were identified as organohalogens,including 33 polychlorinated biphenyls(PCBs),9 organochlorine pesticides,4 polybrominated diphenyl ethers(PBDEs),4 metabolites of diehlorodiphenyl-trichloroethane(DDT),2 chlorinated anisole,2 chlorostyrene,1 thioanisole,and methyl triclosan.In additional,another 16 compounds were tentatively identified as halogenous pllutions,however,these compounds could not be exactly identified due to the lack of authentic standard reference mass spectrum in the library.Using external standard method,10 dominating PCBs and 1 PBDE were quantified in 5 fish samples,Σ10PCBs and 2,2′,4,4′-tetrabromodiphenyl ether(BDE)-47 concentration ranged from 52.08-331.60 ng/g lipid and 4.75-17.03 ng/g lipid,respectively.