气相色谱／离子阱串联质谱法检测大气中的多溴二苯醚

Gas Chromatography-Ion Trap Tandem Mass Spectrometry for the Determination of Polybrominated Biphenyl Ethers in Air

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0．04～0．23pg和9．38pg；方法检出限为6．0～27．1pg／m^3和211．6pg／m^3；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 gas chromatography-ion trap tandem mass spectrometric （GC-ITMS） method was developed for the determination of 8 primary polybrominated biphenyl ethers （PBDEs） in air. ITMS/MS parameters were optimized to achieve the best sensitivity and selectivity. A 15-m GC column, tandem mass spectrometry with selected reaction monitoring along with the internal standard method were used to analyze from tri- to hepta- BDEs and deca-BDE, The detection limits of PBDEs were 0. 04 -0. 23 pg and 9. 38 pg. The cleaned blank PUF samples were spiked with surrogates before using Soxhlet extraction and silica column chromatographic cleanup. The average recoveries of 6 spiked PUF samples were 79. 1% - 101.2% , relative standard deviation was 4. 3% （14. 3% ）. The method detection limits ranged from 6.0 -211.6 pg/m^3 for the PBDEs in the air. Results show that GC-ITMS/MS method appeared to be suitable for the measurement of PBDEs in air under reliable quality assurance and quality control.