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In situ derivatization combined to automated microextraction by packed sorbents for the determination of chlorophenols in soil samples by gas chromatography mass spectrometry A

González Paredes, Rosa María, García Pinto, Carmelo, Pérez Pavón, José Luis, Moreno Cordero, Bernardo
Journal of chromatography 2014 v.1359 pp. 52-59
2,4-dichlorophenol, 2-chlorophenol, acylation, automation, derivatization, detection limit, gas chromatography-mass spectrometry, liquids, microextraction, soil, sorbents
A method based on the coupling of in situ extraction and derivatization of chlorophenols (CPs) (2-chlorophenol, 4-chloro-3-methylphenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) from soils, accomplishing their preconcentration by means of automated microextraction by packed sorbent (MEPS), is proposed. After extraction and acylation of the chlorophenols in aqueous medium, the liquid phase obtained is subjected to the MEPS procedure. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and MEPS techniques were compared and the results confirmed the preconcentration carried out with MEPS.The existence of a matrix effect was checked and the analytical characteristics of the method were determined in a soil sample. The method provided good linearity (from 1 to 12μgkg⁻¹), together with good repeatability and reproducibility values (RSD equal to or less than 10%). The limits of detection were in the 0.118–0.894μgkg⁻¹ range. A certified reference material was applied to validate the proposed methodology.