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Optimization of in situ derivatization SPME by experimental design for GC‐MS multi‐residue analysis of pharmaceutical drugs in wastewater
Author(s) -
de Lima Gomes Paulo Clairmont Feitosa,
Barletta Juliana Yamashita,
Nazario Carlos Eduardo Domingues,
SantosNeto Álvaro José,
Von Wolff Marya Anne,
Coneglian Cassiana Maria Reganhan,
Umbuzeiro Gisela Aragão,
Lancas Fernando Mauro
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000708
Subject(s) - derivatization , chromatography , wastewater , chemistry , residue (chemistry) , gas chromatography–mass spectrometry , gas chromatography , in situ , mass spectrometry , organic chemistry , environmental science , environmental engineering
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.