针对环境监测的特点和要求，建立了同位素稀释-高分辨气相色谱／高分辨质谱测定大气中多溴联苯醚（ PBDEs）和多溴联苯153（ BB153）的方法。采用正己烷／二氯甲烷（1：1，v／v）及正己烷分别对 PBDEs 和 BB153进行快速溶剂萃取，并通过复合硅胶柱净化。在校准曲线最高浓度的10％和90％加标水平下得到的天然内标的平均回收率分别为100％和104％，平均相对标准偏差（ n=7）分别为5％和6％；二至十溴代联苯醚和BB153相应的13 C同位素标准物质回收率在36.5％~133％之间；而一溴代联苯醚13 C同位素标准物质回收率较差，可能是由于物化性质与其他化合物不同。在实际采样体积为300 m 3的情况下，未发生污染物穿透现象；分析物检出限低于2×10－4 ng／Nm3，提取内标回收率在56％~126％之间（一溴代联苯醚除外）。实验结果表明该方法能对化合物准确定量，适用于大气中二至十溴代联苯醚和 BB153的分析。
Considering the features and demands of the environmental monitoring,an isotope dilution-high resolution gas chromatography/high resolution mass spectrometry method was developed for the determination of polybrominated diphenyl ethers( PBDEs)and polybrominat-ed biphenyls 153( BB153)in the ambient air. PBDEs and BB153 were extracted using an accel-erated solvent extraction apparatus with a mixture of hexane-dichloromethane( v/v,1:1)and hexane,respectively. The concentrated extracts were loaded on the composite silica gel column for cleanup. The mean recoveries of native compounds at 10% and 90% of the highest levels of calibration curves were 100% and 104% with 5% and 6% of the mean relative standard devia-tions(n=7),respectively. The recoveries of 13C labeled surrogates for di- to deca-brominated diphenyl ethers and BB153 were in the range of 36. 5%-133%. However,the recoveries of 13C-monobrominated diphenyl ethers were relatively low ,maybe due to the different physicochemi-cal properties compared with the other homologues. No breakthrough of pollutants was esti-mated under real sampling volume of 300 m 3 . The limits of detection were lower than 2 × 10-4 ng/Nm3. The recoveries of 13C labeled surrogates were between 56% and 126%, except monoBDEs. The results demonstrated that the method is suitable for the analysis of di- to deca-brominated diphenyl ethers and BB153 in the ambient air with precise quantification.
参考文献
| [1] | La Guardia MJ;Hale RC;Harvey E.Detailed polybrominated diphenyl ether (PBDE) congener composition of the widely used penta-, octa-, and deca-PBDE technical flame-retardant mixtures[J].Environmental Science & Technology: ES&T,200620(20):6247-6254. |
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