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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.

Authors
  • González Paredes, Rosa María1
  • García Pinto, Carmelo2
  • Pérez Pavón, José Luis1
  • Moreno Cordero, Bernardo1
  • 1 Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain. , (Spain)
  • 2 Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain. Electronic address: [email protected] , (Spain)
Type
Published Article
Journal
Journal of chromatography. A
Publication Date
Sep 12, 2014
Volume
1359
Pages
52–59
Identifiers
DOI: 10.1016/j.chroma.2014.07.048
PMID: 25113872
Source
Medline
Keywords
Language
English
License
Unknown

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. Copyright © 2014 Elsevier B.V. All rights reserved.

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