加速溶剂萃取-气质联用同步测定土壤中17组分多溴二苯醚

建立了加速溶剂萃取-气相色谱-质谱法(ASE-GC/MS)同步定量分析土壤中17组分多溴二苯醚(PBDEs)的方法.选用正己烷和二氯甲烷混合液(体积比为1∶1)为萃取剂,样品经加速溶剂萃取后由氧化铝复合硅胶柱净化,气相色谱-负化学源-质谱法测定.结果表明:在32 min内,包括高溴代二苯醚在内的17组分PBDEs同族体在同一较短毛细管色谱柱上得到了较好的分离.该方法中BDE209的回收率为80.80%,其余BDE的回收率为86.39%～103.19%;BDE209的方法检出限为198.33 pg/g,其他16组分PBDEs同族体的方法检出限为0.85～114.33 pg/g.该方法检测土壤中多组分PBDEs的灵敏度高、重现性和回收率良好,可用于土壤样品PBDEs的分析. 

Simultaneous Determination of 17 Polybrominated Diphenyl Ethers in Soils by Accelerated Solvent Extracted-Gas Chromatography-Mass Spectrometry

An accelerated solvent extraction-gas chromatography-mass spectrometry method was developed for the simultaneous determination of 17 polybrominated diphenyl ethers(PBDEs) in soil.An n-hexane and dichloromethane mixture(V∶V=1∶1) was selected to extract the samples.The clean-up step was optimized using silica gel and alumina,and then the sample was analyzed by gas chromatography-negative chemical ionization-mass spectrometry.The results showed that all 17 components of PBDEs,including the high-brominated diphenyl ethers,could be well separated in a short capillary column in 32 minutes.The results also showed that the recovery of BDE209 was 80.80%,while that of the others ranged from 86.39% to 103.19%.The detection limit of BDE209 was 198.33 pg/g,while that of the other 16 polybrominated diphenyl ethers were in the range of 0.85-114.33 pg/g.With high sensitivity and good reproducibility and recovery,this method can be used well for the analysis of PBDEs in soils.