Abstract

Effects of temperature on the reversed-phase chromatographic behavior of PAHs were investigated on three columns. The first was the recent C18column (250 mm × 4.6 mm) packed with 5 µm core-shell particles while the others were more conventional C18columns (250 mm × 4.6 mm) packed with fully porous particles. Among the 16 PAHs studied, special attention has been paid to two pairs of PAHs, fluorene/acenaphthene and chrysene/benzo[a]anthracene, which often present coeluting problems. Due to the low surface area of the core-shell particles, lowest retention time of each PAH was highlighted and effects of the temperature on the separation of PAHs were negligible in regard to those using columns packed with fully porous particles. For each PAH studied, it was demonstrated that peaks were symmetrical and may be considered as Gaussian peaks when the column packed with core-shell particle was employed. In the best condition, the separation of PAHs was conducted at 16°C under very low pressure values (670–950 psi = 46–65 bars). Depending on PAHs, the limit of detection ranged from 0.88 to 9.16 μg L−1. Analysis of spiked acetonitrile samples with PAHs at 10 and 50 µg L−1and tap water at 10 µg L−1gave very good recoveries (94%–109.3%) and high precision (1.1%–3.5%).

Highlights

  • Laboratory experiments have shown that the genotoxic, mutagenic, and carcinogenic activity depended on the chemical structure of polycyclic aromatic hydrocarbons (PAHs) [1]

  • These PAHs are usually analyzed by gas chromatography coupled to mass spectrometry [3,4,5,6,7,8] and less frequently by liquid chromatography coupled to mass spectrometry [9,10,11]

  • Many studies reported that the efficiency in the separation of PAHs depended on the chain length of the stationary phase and on chemically bonded octadecylsilyl phases [15,16,17]

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Summary

Introduction

Laboratory experiments have shown that the genotoxic, mutagenic, and carcinogenic activity depended on the chemical structure of polycyclic aromatic hydrocarbons (PAHs) [1]. The stationary phase particles of these columns are composed of a solid silica core surrounded by a homogeneous and durable porous layer, allowing better efficiencies and faster analyses than totally porous particles of the same size This performance improvement is likely due to the package quality of the core-shell columns for which the eddy diffusion terms of these columns are significantly smaller (−40%) than that of the column packed with fully porous particles [21,22,23,24,25, 30]. The recent packed with the 5 μm core-shell particles were tested in the separation of the 16 PAHs recommended by the US EPA with the following main objectives: (i) the study of the retention with temperature, (ii) the characterization of peaks for each PAH, (iii) the determination of detection and quantification limits and the precision on the analytical method, and (iv) the validation of the method using spiked tap water samples

Materials and Methods
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