title: Optimization of in situ derivatization SPME by experimental design for GC-MS multi-residue analysis of pharmaceutical drugs in wastewater.
abstract: 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.
authors.affiliation: Institute of Chemistry of Sao Carlos, University of Sao Paulo, São Carlos, SP, Brazil.
authors.forename: Paulo Clairmont Feitosa
authors.initials: PC
authors.lastname: de Lima Gomes
authors.forename: Juliana Yamashita
authors.initials: JY
authors.lastname: Barletta
authors.forename: Carlos Eduardo Domingues
authors.initials: CE
authors.lastname: Nazario
authors.forename: Alvaro José
authors.initials: AJ
authors.lastname: Santos-Neto
authors.forename: Marya Anne
authors.initials: MA
authors.lastname: Von Wolff
authors.forename: Cassiana Maria Reganhan
authors.initials: CM
authors.lastname: Coneglian
authors.forename: Gisela Aragão
authors.initials: GA
authors.lastname: Umbuzeiro
authors.forename: Fernando Mauro
authors.initials: FM
authors.lastname: Lancas
mesh_terms: D004350:Drug Residues / Q000032:analysis* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry; D012722:Sewage / Q000032:analysis*; D052617:Solid Phase Microextraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification*
chemical_list: D012722:Sewage; D014874:Water Pollutants, Chemical