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

Autor(es)

Feitosa de Lima Gomes, Paulo Clairmont ^[1] ; Barletta, Juliana Yamashita ^[1] ; Domingues Nazario, Carlos Eduardo ^[1] ; Santos-Neto, Alvaro Jose ^[1] ; Von Wolff, Marya Anne ^[2] ; Reganhan Coneglian, Cassiana Maria ^[2] ; Umbuzeiro, Gisela Aragao ^[2] ; Lancas, Fernando Mauro ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Inst Chem Sao Carlos, BR-13560970 Sao Carlos, SP - Brazil

^[2] Univ Estadual Campinas, Fac Technol, Limeira, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF SEPARATION SCIENCE; v. 34, n. 4, p. 436-445, FEB 2011.
• Citações Web of Science: 20

Resumo

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 mu g/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. (AU)

• Processo FAPESP: 05/59360-0 - Miniaturização de instrumentação analítica para técnicas de separação: do preparo de amostra a impressão do resultado
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 07/03844-4 - Análise simultânea de multi-resíduos de antibióticos em água e sedimentos por extração sorptiva em barra no modo headspace com derivatização "in situ" acoplado a GC/MS
• Beneficiário: Paulo Clairmont Feitosa de Lima Gomes
• Modalidade de apoio: Bolsas no Brasil - Doutorado Direto