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超声辅助萃取与在线液相色谱-气相色谱-质谱联用测定城市灰尘和柴油颗粒物中的多环芳烃(PAH)

Ultrasound-assisted extraction and on-line LC-GC-MS for determination of polycyclic aromatic hydrocarbons (PAH) in urban dust and diesel particulate matter.

作者信息

Christensen Anders, Ostman Conny, Westerholm Roger

机构信息

Department of Analytical Chemistry, Arrhenius Laboratory, Stockholm University, 106 91, Stockholm, Sweden.

出版信息

Anal Bioanal Chem. 2005 Mar;381(6):1206-16. doi: 10.1007/s00216-005-3065-z. Epub 2005 Feb 25.

Abstract

A method has been developed for determination of polycyclic aromatic hydrocarbons (PAH) in particulate matter from ambient air and diesel exhaust emissions. It is reproducible and accurate and, compared with similar methods for analysis of individual PAH components in complex matrices, it is relatively fast and simple. Single PAH components can be determined in samples of particulate matter from ambient air and diesel exhaust emissions with LOD of approximately 1 pg/sample. Further, sample throughput is high, because more than 20 samples can be extracted and prepared for analysis in one working (8-h) day. The particulate matter is subjected to ultrasound-assisted extraction, a technique that is shown to extract PAH from particulate material with efficiencies fully comparable with those of Soxhlet extraction. An aliphatic/PAH-enriched fraction is obtained by solid-phase extraction before isolation, separation, and identification/quantification of PAH by on-line liquid chromatography-gas chromatography-mass spectrometry. The method was validated by analysis of US National Institute of Standards and Technology (NIST) Standard Reference Materials (SRM) 1649a, Urban Dust, and 2975, Diesel Particulate Matter. Results from the method are in good agreement with the NIST-certified PAH concentrations and with NIST reference PAH concentrations.

摘要

已开发出一种测定环境空气和柴油废气排放颗粒物中多环芳烃(PAH)的方法。该方法具有可重复性和准确性,与分析复杂基质中单个PAH成分的类似方法相比,相对快速且简单。可测定环境空气和柴油废气排放颗粒物样品中的单个PAH成分,检测限约为1 pg/样品。此外,样品通量高,因为在一个工作日(8小时)内可提取并制备20多个样品用于分析。颗粒物采用超声辅助萃取,该技术从颗粒物质中萃取PAH的效率与索氏萃取法完全相当。在通过在线液相色谱 - 气相色谱 - 质谱法对PAH进行分离、鉴定/定量之前,通过固相萃取获得富含脂肪族/PAH的馏分。通过分析美国国家标准与技术研究院(NIST)标准参考物质(SRM)1649a(城市灰尘)和2975(柴油颗粒物)对该方法进行了验证。该方法的结果与NIST认证的PAH浓度以及NIST参考PAH浓度高度吻合。

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