Abstract
The objective of this study was to develop a novel analytical chemistry method, comprised of a coupled high-performance liquid chromatography–gas chromatography/mass spectrometry system (LC–GC/MS) with low detection limits and high selectivity, for the identification and determination of oxygenated polycyclic aromatic hydrocarbons (OPAHs) and polycyclic aromatic hydrocarbons (PAHs) in urban air and diesel particulate matter. The linear range of the four OPAHs, which include 9,10-anthraquinone, 4H-cyclopenta[def]phenanthrene-4-one, benzanthrone, and 7,12-benz[a]anthraquinone, was 0.7 pg–43.3 ng with limits of detection (LODs) and limits of quantification (LOQs) on the order of 0.2–0.8 and 0.7–1.3 pg, respectively. The LODs in this study are generally lower than values reported in the literature, which can be explained by using large-volume injection. The recoveries of the OPAHs spiked onto glass fiber filters using two different pressurized liquid extraction (PLE) methods were in the ranges of 84–107 and 67–110 %, respectively. The analytical protocols were validated using the following National Institute of Standards and Technology standard reference materials: SRM 1649a (Urban Dust), SRM 1650b (Diesel Particulate Matter), and SRM 2975 (Diesel Particulate Matter, Industrial Forklift). The measured mass fractions of the OPAHs in the standard reference materials (SRMs) in this present study are higher than the values from the literature, except for benzanthrone in SRM 1649a (Urban Dust). In addition to the OPAHs, 44 PAHs could be detected and quantified from the same particulate extract used in this protocol. Using data from the literature and applying a two-sided t test at the 5 % level using Bonferroni correction, significant differences were found between the tested PLE methods for individual PAHs. However, the measured mass fractions of the PAHs were comparable, similar to, or higher than those previously reported in the literature.Electronic supplementary materialThe online version of this article (doi:10.1007/s00216-014-8304-8) contains supplementary material, which is available to authorized users.
Highlights
A vast body of scientific studies has shown associations between human exposure to urban air particulate matter (PM) pollution and severe health outcomes such as lung cancer, diseases of the respiratory and cardiovascular systems, premature mortality, and an increase in infant mortality [1–4]
Extraction procedure E1 is an exhaustive extraction protocol previously developed by our research group [35], and it has previously been used for the determination of Polycyclic aromatic hydrocarbons (PAHs) in diesel standard reference materials (SRMs) [34, 36], whereas extraction procedures E2 and E3 are adopted from a recent paper from NIST using pressurized liquid extraction (PLE) for the extraction of PAHs and nitro PAHs from air and diesel PM SRMs [36]
Mirivel and co-workers determined the PLE recoveries of various oxygenated polycyclic aromatic hydrocarbons (OPAHs) spiked onto filters to be in the order of 79–107 % (PLE with methanol and one 8-min static cycle at 100 °C) [24], and Walgraeve and co-workers obtained recoveries of 99 ± 4 % and 101±4 % for BAQ at ambient temperature and at 40 °C, respectively (PLE with ethyl acetate and three 5-min static cycles)
Summary
A vast body of scientific studies has shown associations between human exposure to urban air particulate matter (PM) pollution and severe health outcomes such as lung cancer, diseases of the respiratory and cardiovascular systems, premature mortality, and an increase in infant mortality [1–4]. Polycyclic aromatic hydrocarbons (PAHs) constitute a group of ubiquitous environmental pollutants present in air PM derived from different sources, and they are considered to play an important part in the adverse health outcomes due to PM exposure [6, 10]. A group of less-studied PAH derivatives are oxygenated polycyclic aromatic hydrocarbons (OPAHs), which have recently been noted as being reactive compounds with the potential of causing adverse biological effects. Due to their direct mutagenic potency, OPAHs may be more toxic to humans compared to their parent PAHs [11, 12]. PLE has been shown to give an equivalent or higher extraction efficiency compared to Soxhlet extraction for PAHs from air and diesel PM standard reference materials (SRMs) and recently for OPAHs from a diesel PM SRM [26]
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