加速溶剂萃取/GC-MS-SIM法测定环境空气中16种多环芳烃 摘要:建立了环境空气中16种多环芳烃的监测方法。通过大流量采样装置,使环境空气中的目标化合物富集于石英纤维滤膜,PUF和XAD-2中,目标物用加速溶剂萃取技术萃取,以氟罗里硅土柱净化,质谱采用选择离子法(SIM)扫描,内标法定量。本方法的检出限为0.59 ng/m3~1.26 ng/m3,空白加标回收率为69.8%~126%,相对标准偏差为3.91%~15.0%。本方法简单、易操作,适用于环境空气中多环芳烃的监测。
关键词:多环芳烃; 环境空气; 加速溶剂萃取; 选择离子法
Abstract: An accelerated Solvent Extraction (ASE) coupled with gas chromatography-mass spectrometric method was established for the simultaneous determination of sixteen Polycyclic Aromatic Hydrocarbons (PAHs) in ambient air. Through the large flow sampling device, the target compounds were collected in quartz fiber filters, PUF and XAD-2. The PAHs were extracted by ASE, and purified by Florisil column. Mass spectrometry with Selected Ion Method for scanning and Internal Standard for quantitative calculation. The method limit was from 0.59 ng/m3 to 1.26 ng/m3, and spiked blank recovery rate was from 69.8% to 126%, the RSD was between 3.91% and 15.0%. The method was simple, easy to operate, and suitable for the determination of PAHs in ambient air.
Key words: PAHs; Ambient air; ASE; SIM
多环芳烃(Polycyclic Aromatic Hydrocarbons, PAHs)是两个或两个以上苯环连在一起的化合物,主要是煤、石油、天然气、烟草、高分子有机化合物等在不完全燃烧下形成的具有挥发性的碳氢化合物,具有高致毒、致癌和致突变性,对人体健康危害很大[1.2]。
大气中多环芳烃主要以气态和固态两种形式存在,其中分子量小的2环-3环PAHs主要以气态为主, 4环PAHs存在气态、颗粒态中,分子量较大的5环-7环PAHs则大多以颗粒态形式存在[3]。本文以美国EPA优先控制的16种PAHs为分析目标化合物,用加速溶剂萃取法提取石英纤维滤膜、聚氨酯泡沫(PUF)和XAD-2大孔树脂中的PAHs,气相色谱质谱选择离子法(SIM)测定。选择离子法具有定性准确,灵敏度高等特点,当以100L/min的流量采集环境空气24h,其检出限可达到0.59 ng/m3~1.26 ng/m3。
1、实验部分
1.1方法原理
当环境空气通过具有一定切割特性的采样器,以100 L/min流速,将环境空
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