Wilson Walter B, Hayes Hugh V, Sander Lane C, Campiglia Andres D, Wise Stephen A
Chemical Sciences Division, Material Measurement Laboratory, National Institute of Standards and Technology, 100 Bureau Drive, Mail Stop 8390, Gaithersburg, MD, 20899, USA.
Department of Chemistry, University of Central Florida, Orlando, FL, 32816, USA.
Anal Bioanal Chem. 2017 Aug;409(21):5171-5183. doi: 10.1007/s00216-017-0464-x. Epub 2017 Jun 29.
A normal-phase liquid chromatography (NPLC) fractionation procedure was developed for the characterization of a complex mixture of polycyclic aromatic hydrocarbons (PAHs) from a coal tar sample (Standard Reference Material (SRM) 1597a). Using a semi-preparative aminopropyl (NH) LC column, the coal tar sample was separated using NPLC based on the number of aromatic carbons; a total of 14 NPLC fractions were collected. SRM 1597a was analyzed before and after NPLC fractionation by using gas chromatography/mass spectrometry (GC/MS) with a 50% phenyl stationary phase. The NPLC-GC/MS method presented in this study allowed for the identification of 72 PAHs and 56 MePAHs. These identifications were based on the NPLC retention times for authentic reference standards, GC retention times for authentic reference standards, and the predominant molecular ion peak in the mass spectrum. Most noteworthy was the determination of dibenzo[a,l]pyrene, which could not be measured directly by GC/MS because of low concentration and co-elution with dibenzo[j,l]fluoranthene. The NPLC-GC/MS procedure also allowed for the tentative identification of 74 PAHs and 117 MePAHs based on the molecular ion peak only. This study represents the most comprehensive qualitative characterization of SRM 1597a to date. Graphical abstract NPLC-GC/MS analysis for the six-ring MM 302 Da PAH isomers in SRM 1597a.
开发了一种正相液相色谱（NPLC）分级程序，用于表征煤焦油样品（标准参考物质（SRM）1597a）中多环芳烃（PAH）的复杂混合物。使用半制备型氨丙基（NH）液相色谱柱，基于芳香碳的数量，通过NPLC对煤焦油样品进行分离；共收集了14个NPLC级分。在NPLC分级前后，使用具有50%苯基固定相的气相色谱/质谱（GC/MS）对SRM 1597a进行分析。本研究中提出的NPLC-GC/MS方法能够鉴定出72种PAH和56种甲基化多环芳烃（MePAH）。这些鉴定基于真实参考标准品的NPLC保留时间、真实参考标准品的GC保留时间以及质谱图中的主要分子离子峰。最值得注意的是二苯并[a,l]芘的测定，由于其浓度低且与二苯并[j,l]荧蒽共洗脱，无法通过GC/MS直接测量。NPLC-GC/MS程序还仅基于分子离子峰初步鉴定出74种PAH和117种MePAH。本研究代表了迄今为止对SRM 1597a最全面的定性表征。图形摘要SRM 1597a中六环MM 302 Da PAH异构体的NPLC-GC/MS分析。
