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采用冷纤维固相微萃取气相色谱-质谱法测定环境空气中颗粒物中的多环芳烃。

Determination of polycyclic aromatic hydrocarbons from ambient air particulate matter using a cold fiber solid phase microextraction gas chromatography-mass spectrometry method.

机构信息

Departamento de Química, Universidade Federal de Minas Gerais, Avenida Antonio Carlos, Pampulha - Belo Horizonte/MG 31270901, Brazil.

出版信息

J Chromatogr A. 2011 May 27;1218(21):3300-5. doi: 10.1016/j.chroma.2010.10.105. Epub 2010 Nov 3.

DOI:10.1016/j.chroma.2010.10.105
PMID:21093868
Abstract

Polycyclic aromatic hydrocarbons (PAH) from ambient air particulate matter (PM) were analyzed by a new method that utilized direct immersion (DI) and cold fiber (CF) SPME-GC/MS. Experimental design was used to optimize the conditions of extraction by DI-CF-SPME with a 100μm polydimethylsiloxane (PDMS) fiber. The optimal conditions included a 5min equilibration at 70°C time in an ultrasonic bath with an extraction time of 60min. The optimized method was validated by the analysis of a NIST standard reference material (SRM), 1649b urban dust. The results obtained were in good agreement with certified values. PAH recoveries for reference materials were between 88 and 98%, with a relative standard deviation ranging from 5 to 17%. Detection limits (LOD) varied from 0.02 to 1.16ng and the quantification limits (LOQ) varied from 0.05 to 3.86ng. The optimized and validated method was applied to the determination of PAH from real particulate matter (PM10) and total suspended particulate (TPS) samples collected on quartz fiber filters with high volume samplers.

摘要

多环芳烃(PAH)来自环境空气颗粒物(PM),采用直接浸入(DI)和冷纤维(CF)SPME-GC/MS 的新方法进行分析。实验设计用于通过 DI-CF-SPME 优化萃取条件,采用 100μm 聚二甲基硅氧烷(PDMS)纤维。最佳条件包括在超声波浴中于 70°C 下平衡 5min,萃取时间为 60min。通过对 NIST 标准参考物质(SRM)1649b 城市灰尘的分析验证了优化方法。获得的结果与认证值吻合良好。参考物质的 PAH 回收率在 88%至 98%之间,相对标准偏差在 5%至 17%之间。检测限(LOD)范围从 0.02 到 1.16ng,定量限(LOQ)范围从 0.05 到 3.86ng。优化和验证后的方法应用于测定高容量采样器采集的石英纤维滤纸上的真实颗粒物(PM10)和总悬浮颗粒物(TPS)样品中的 PAH。

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