Optimization of the matrix solid-phase dispersion sample preparation procedure for analysis of polycyclic aromatic hydrocarbons in soils: Comparison with microwave-assisted extraction

Abstract

A fast and simple preparation procedure based on the matrix solid-phase dispersion (MSPD) technique is proposed for the first time for the isolation of 16 polycyclic aromatic hydrocarbons (PAHs) from soil samples. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[ a]anthracene, chrysene, benzo[ e]pyrene, benzo[ b]fluoranthene, benzo[ k]fluoranthene, benzo[ a]pyrene, dibenzo[ a, h]anthracene, benzo[ g, h, i]perylene, and indeno[1,2,3- c, d]pyrene were considered in the study. Extraction and clean-up of samples were carried out in a single step. The main parameters that affect extraction yield, such as dispersant, type and amount of additives, clean-up co-sorbent and extractive solvent were evaluated and optimized. The addition of an alkali solution in MSPD was required to provide quantitative recoveries. Analytical determinations were carried out by high performance liquid chromatography (HPLC) with fluorescence detection. Quantification limits (between 0.01 and 0.6 ng g −1 dry mass) were well below the regulatory limits for all the compounds considered. The extraction yields for the different compounds obtained by MSPD were compared with the yields obtained by microwave-assisted extraction (MAE). To test the accuracy of the MSPD technique, the optimized methodology was applied to the analysis of standard reference material BCR-524 (contaminated industrial soil), with excellent results.