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运用气相色谱-离子阱质谱(ion trap mass spectrometry,ITMS)建立了大气中8种多溴二苯醚的二级质谱(MS/MS)检测方法。优化后的MS/MS方法对7种三溴至七溴二苯醚(BDE28、-47、-99、-100、-153、-154、-183)和十溴二苯醚(BDE209)的仪器检出限分别为0.04~0.23 pg和9.38 pg;方法检出限为6.0~27.1 pg/m3和211.6 pg/m3;6点标准曲线相关系数(r)为0.9980~0.9999。方法对8种目标物的加标回收率为79.1%~101.0%,相对标准偏差(RSD)为4.3%~14.3%(n=6)。对6份南京实际大气样品的检测结果表明:离子阱质谱的选择反应监测(selected reaction monitoring,SRM)技术能有效的降低背景干扰。优化后的MS/MS方法对目标化合物有较高的灵敏度,可应用于大气中痕量多溴二苯醚的定量检测。
A two-phase mass spectrometry (MS / MS) detection method for eight PBDEs in the atmosphere was established by ion trap mass spectrometry (ITMS). The optimized MS / MS method was applied to seven instruments for the determination of tribromo to heptabromodiphenyl ether (BDE28, -47, -99, -100, -153, -154, -183) and decabromodiphenyl ether (BDE209) The detection limits were 0.04 ~ 0.23 pg and 9.38 pg respectively. The detection limits were 6.0 ~ 27.1 pg / m3 and 211.6 pg / m3, respectively. The correlation coefficients (r) of 6 standard curves were 0.9980 ~ 0.9999. The recoveries of eight target compounds were 79.1% ~ 101.0% with relative standard deviations (RSDs) of 4.3% -14.3% (n = 6). The results of six real atmospheric samples in Nanjing show that the selected reaction monitoring (SRM) technique of ion trap mass spectrometry can effectively reduce the background interference. The optimized MS / MS method has high sensitivity to the target compounds and can be applied to the quantitative detection of trace levels of polybrominated diphenyl ethers in the atmosphere.