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直接洗脱-同位素稀释气相色谱/质谱法测定空气中颗粒物中 43 种多环芳烃

Determination of 43 polycyclic aromatic hydrocarbons in air particulate matter by use of direct elution and isotope dilution gas chromatography/mass spectrometry.

机构信息

Centers for Disease Control and Prevention, 4770 Buford Highway F-53, Atlanta, GA 30341, USA.

出版信息

Anal Bioanal Chem. 2010 Feb;396(3):1321-30. doi: 10.1007/s00216-009-3297-4. Epub 2009 Nov 21.

DOI:10.1007/s00216-009-3297-4
PMID:19936717
Abstract

We are reporting a method for measuring 43 polycyclic aromatic hydrocarbons (PAH) and their methylated derivatives (Me-PAHs) in air particulate matter (PM) samples using isotope dilution gas chromatography/high-resolution mass spectrometry (GC/HRMS). In this method, PM samples were spiked with internal standards, loaded into solid phase extraction cartridges, and eluted by dichloromethane. The extracts were concentrated, spiked with a recovery standard, and analyzed by GC/HRMS at 10,000 resolution. Sixteen (13)C-labeled PAHs and two deuterated Me-PAHs were used as internal standards to account for instrument variability and losses during sample preparation. Recovery of labeled internal standards was in the range of 86-115%. The proposed method is less time-consuming than commonly used extraction methods, such as sonication and accelerated solvent extraction (ASE), and it eliminates the need for a filtration step required after the sonication extraction method. Limits of detection ranged from 41 to 332 pg/sample for the 43 analytes. This method was used to analyze reference materials from the National Institute of Standards and Technology. The results were consistent with those from ASE and sonication extraction, and these results were also in good agreement with the certified or reference concentrations. The proposed method was then used to measure PAHs on PM(2.5) samples collected at three sites (urban, suburban, and rural) in Atlanta, GA. The results showed distinct seasonal and spatial variation and were consistent with an earlier study measuring PM(2.5) samples using an ASE method, further demonstrating the compatibility of this method and the commonly used ASE method.

摘要

我们报告了一种使用同位素稀释气相色谱/高分辨率质谱 (GC/HRMS) 测量空气中颗粒物 (PM) 样品中 43 种多环芳烃 (PAH) 及其甲基化衍生物 (Me-PAHs) 的方法。在该方法中,将 PM 样品与内标物混合,加载到固相萃取小柱中,然后用二氯甲烷洗脱。提取物浓缩后,加入回收率标准品,在 10000 分辨率下用 GC/HRMS 进行分析。十六个 (13)C 标记的 PAH 和两个氘代 Me-PAH 被用作内标物,以说明仪器变化和样品制备过程中的损失。标记内标物的回收率在 86-115%之间。与常用的提取方法(如超声提取和加速溶剂提取 (ASE))相比,该方法耗时更少,并且消除了超声提取方法后所需的过滤步骤。43 种分析物的检出限范围为 41-332pg/样品。该方法用于分析来自美国国家标准与技术研究院的标准物质。结果与 ASE 和超声提取的结果一致,这些结果也与认证或参考浓度非常吻合。然后,该方法用于测量佐治亚州亚特兰大市三个地点(城市、郊区和农村)采集的 PM(2.5) 样品中的 PAHs。结果显示出明显的季节性和空间变化,与使用 ASE 方法测量 PM(2.5) 样品的早期研究结果一致,进一步证明了该方法与常用的 ASE 方法的兼容性。

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