Optimization of in situ derivatization SPME by experimental design for GC-MS multi-residue analysis of pharmaceutical drugs in wastewater.

Autor: de Lima Gomes PC; Institute of Chemistry of Sao Carlos, University of Sao Paulo, São Carlos, SP, Brazil., Barletta JY, Nazario CE, Santos-Neto AJ, Von Wolff MA, Coneglian CM, Umbuzeiro GA, Lancas FM
Jazyk: angličtina
Zdroj: Journal of separation science [J Sep Sci] 2011 Feb; Vol. 34 (4), pp. 436-45.
DOI: 10.1002/jssc.201000708
Abstrakt: This paper presents the development of a procedure, which enables the analysis of nine pharmaceutical drugs in wastewater using gas chromatography-mass spectrometry (GC-MS) associated with solid-phase microextraction (SPME) for the sample preparation. Experimental design was applied to optimize the in situ derivatization and the SPME extraction conditions. Ethyl chloroformate (ECF) was employed as derivatizing agent and polydimethylsiloxane-divinylbenzene (PDMS-DVB) as the SPME fiber coating. A fractional factorial design was used to evaluate the main factors for the in situ derivatization and SPME extraction. Thereafter, a Doehlert matrix design was applied to find out the best experimental conditions. The method presented a linear range from 0.5 to 10 μg/L, and the intraday and interday precision were lower than 16%. Applicability of the method was verified from real influent and effluent samples of a wastewater treatment plant, as well as from samples of an industry wastewater and a river.
(Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)
Databáze: MEDLINE
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