title: In situ derivatization combined to automated microextraction by packed sorbents for the determination of chlorophenols in soil samples by gas chromatography mass spectrometry.
abstract: 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.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Rosa María
authors.initials: RM
authors.lastname: González Paredes
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain. Electronic address: cgp@usal.es.
authors.forename: Carmelo
authors.initials: C
authors.lastname: García Pinto
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: José Luis
authors.initials: JL
authors.lastname: Pérez Pavón
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Bernardo
authors.initials: B
authors.lastname: Moreno Cordero
mesh_terms: D000327:Adsorption; D001331:Automation; D002733:Chlorophenols / Q000737:chemistry* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D010575:Pesticides / Q000032:analysis / Q000302:isolation & purification*; D012989:Soil Pollutants / Q000032:analysis / Q000302:isolation & purification*; D052617:Solid Phase Microextraction / Q000295:instrumentation / Q000379:methods*
chemical_list: D002733:Chlorophenols; D010575:Pesticides; D012989:Soil Pollutants
keywords: Chlorophenols; In situ derivatization; Microextraction by packed sorbents (MEPS); Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS); Soil samples