质谱法测定大气颗粒物中多环芳烃的内标选择和质量控制
The Choice of Internal Standard and Quality Control for the Measurement of Polycyclic Aromatic Hydrocarbons in Airborne Particulates by Mass Spectrometry
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摘要: 以美国EPA TO-13A标准为基础,研究了气相色谱-质谱法测定大气颗粒物中18种多环芳烃(PAHs)的分析方法,对内标的选择、数据稳定性进行了探讨,对替代物回收率进行统计分析。从内标物和目标化合物的响应衰减相关性、响应因子等确定了各化合物的内标物,BghiP、DBahA、IP、COR的内标物由EPA方法TO-13A中的d10-AC改为d10-PYL,并考查了7天内测试数据的稳定性和365件分析样中替代物回收率。该分析方法的仪器检出限为8~12 pg,目标化合物日常校准测定平均误差为-11.21%~12.12%,相对标准偏差(RSD,n=7)为4.12%~14.27%。替代物的回收率为64.35%~127.94%,平均回收率为76.95%~79.71%,相对标准偏差(RSD,n=365)为7.15%~9.66%。方法数据的稳定性有较大的提高,替代物的回收率等参数符合美国EPA要求,可用于批量或连续分析大气颗粒物中的18种PAHs。Abstract: This paper reports a method to analyze as many as 18 polycyclic aromatic hydrocarbons (PAHs) in airborne particulates by gas chromatography mass spectrometry (GC-MS) based on US EPA TO-13A standard. The selectivity of internal standards, the stability of data and the recovery rate of substitute standards are discussed. The internal standards were selected according to the correlations of response attenuation and response factors between internal standards and target compounds. The internal standard for BghiP, DBahA, IP and COR was d10-PYL instead of d10-AC, which was used in TO-13A. The stability of data and the recovery rates of substitutes of 365 samples for 7 days were studied. The instrument detection limit was 8-12 pg, the average error of target compounds were -11.21%-12.12%, and relative standard deviation (RSD, n=7) were 4.12%-14.27%. The recovery rate of substitute standards ranged from 64.35% to 127.94%, the average recovery rate were from 76.95% to 79.71% with the RSD (n=365) from 7.15% to 9.66%. In this paper, the stability of data, the recovery rate of substitute standards, etc. all met the requirements of EPA. This method can be used for batch or continuous analysis of 18 PAHs in atmospheric particulates.
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Keywords:
- airborne /
- particulates /
- polycyclic /
- aromatic
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