Abstract
Exposure to atmospheric particulate matter (PM) associated pollutants is a global concern due to the risk posed in human health after inhalation. In this study, a simple and sensitive multi-residue method is developed for the analysis of 50 organic pollutants, comprising 18 polycyclic aromatic hydrocarbons (PAHs), 12 phthalate esters (PAEs), 12 organophosphorus flame retardants (OPFRs), 6 synthetic musk compounds (SMCs) and 2 bisphenols in PM2.5 samples. The method consists of three cycles of ultrasonic assisted solvent extraction and vortex (UASE + vortex), followed by a vortex-assisted dispersive solid phase extraction (d-SPE) clean-up and a final determination step by using programmed temperature vaporization-gas chromatography-tandem mass spectrometry (PTV-GC-MS/MS). Experimental conditions concerning clean-up adsorbents (alumina, silica gel and Florisil®) and filters (glass fibre, PTFE and nylon), as well as PTV-GC-MS/MS conditions were studied. In addition, the use of SRM (selected reaction monitoring) mode in MS-MS, as well as matrix-matched calibration together with labelled subrogate standards, resulted in successfully validation results for most of the compounds due to the high sensitivity, minimization of matrix effects and recovering losses compensation. The proposed method was validated in terms of linearity, limits of detection and quantification (LODs and LOQs), analytical recoveries by analysing a spiked composite sample (PM2.5) at three spiking levels and intra-day and inter-day precision. Moreover, an urban particulate matter standard reference material (SRM 1648a) was analysed to assess PAHs determination accuracy. Furthermore, applicability of the method was proved by analysing 12 PM2.5 samples from an industrial area. Among all studied pollutants, bisphenol A (BPA) was the most predominant with an average concentration of 5000 pg m−3, followed by bis(2-ethylhexyl) phthalate (DEHP) and diisobutyl phthtalate (DiBP) with 1990 pg m−3 and 632 pg m-3, respectively. Concerning OPFRs, average concentrations between 345 – 253 pg m−3 were found for triphenyl phosphine oxide (TPPO), tris(chloropropyl) phosphate (TCPP), tri-iso-butyl phosphate (TiBP) and tris(2-butoxyethyl) phosphate (TBOEP). Finally, the highest PAHs levels were found for 5-6 ring-number PAHs (Σ5-6 rings PAHs) with an average concentration of 2680 pg m−3, while only 2 SMCs were quantitated accounting for 17.5 pg m−3 by average.
Highlights
The release of pollutants to the atmosphere due to anthropogenic activity represents an important impact on air quality, driving global climate change and posing an important risk on human health [1], and being considered to be responsible of approximately 3 million deaths worldwide every year [2]
Target compound extraction from PM2.5 samples was assessed following the ultrasonic assisted solvent extraction (UASE) + vortex method described by Cristale and Lacorte et al [58] and by Velaz quez-Gomez et al [63] with some modifications
GF filters were not tested for synthetic musk compounds (SMCs) due to the problem detected for bisphenols, showing averaged recoveries of 92 % and 95 % for nylon and PTFE filters, respectively
Summary
The release of pollutants to the atmosphere due to anthropogenic activity represents an important impact on air quality, driving global climate change and posing an important risk on human health [1], and being considered to be responsible of approximately 3 million deaths worldwide every year [2]. PAEs and bisphenols are considered endocrine disruptors, exhibiting similar health effects associated to reproductive developmental and neurological toxicity in humans [24,25,26,27,28,29,30,31,32,33]. PAHs are well-known air pollutants that are mainly emitted to the atmosphere as a result of incomplete combustion processes (e.g. biomass and fossil fuels) and their occurrence in atmospheric PM fractions (PM10 and PM2.5) has been studied in different areas by many researchers [34,35,36,37,38,39]. The occurrence in the environment of the remaining compounds (PAEs, OPFRs, SMCs and bisphenols) is primarily due to their wide application in many industries such as plastics, electronics, furniture and personal care [19,31,40,41], being many of them considered as high-production volume (HPV) chemicals by the USEPA [42]
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