Optimization of in situ derivatization SPME by experimental design for GC-MS multi-residue analysis of pharmaceutical drugs in wastewater
✍ Scribed by Paulo Clairmont Feitosa de Lima Gomes; Juliana Yamashita Barletta; Carlos Eduardo Domingues Nazario; Álvaro José Santos-Neto; Marya Anne Von Wolff; Cassiana Maria Reganhan Coneglian; Gisela Aragão Umbuzeiro; Fernando Mauro Lancas
- Publisher
- John Wiley and Sons
- Year
- 2011
- Tongue
- English
- Weight
- 306 KB
- Volume
- 34
- Category
- Article
- ISSN
- 1615-9306
No coin nor oath required. For personal study only.
✦ Synopsis
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.