title: Development, validation and application of a method to analyze phenols in water samples by solid phase micro extraction-gas chromatography-flame ionization detector.
abstract: In this work the development, validation and application of method using Solid Phase Microexctration (SPME) for the analyses of five pollutants (phenol, 2-nitrophenol, 2,4-dimethylphenol, 2,4-dichlorophenol and 4-chloro, 3-methyl phenol) in supplying water, using gas chromatography (GC) with flame ionization detector (FID) is described. The optimal conditions obtained for SPME were: fiber type: Poliacrylate (PA); extraction time: 40 minutes; extraction temperature: 70 degrees C; amount of salt added to sample (NaCl): 15%; desorption temperature: 8 minutes. The parameters studied in the method validation were: limit of detection (0.3 and 3.5 microg.L(- 1)); precision, measured by the variation coefficient (between 2.1 and 8.8%); calibration curve and linearity, by using the external standardization method (between 1 and 50 50 microg.L(- 1)). After the methodology development, samples of water collected in Atibaia River (São Paulo - Brazil) were analyzed, using the optimized methodology. Three water samples collected in the rain season showed a peak with retention time close to 4-chloro, 3 methyl phenol further analyzed by Gas Chromatography-Mass Spectrometry for the identity confirmation. In spite of the fact that none target compounds were found in the river water samples analyzed, the presence of two phenols different from those investigated (p-terc butyl phenol; butylated hydroxytoluene) were detected. These results together with the results of the limit of detection (that showed to be lower than the maximum concentration of phenols demanded by different environment control agencies), and the results of the validation, indicate the applicability of this method for the analysis of selected phenols in river water samples.
authors.affiliation: São Paulo University, Institute of Chemistry at São Carlos, São Paulo University, São Carlos, SP, Brazil. flancas@iqsc.usp.br
authors.forename: Fernando M
authors.initials: FM
authors.lastname: Lanças
authors.forename: Igor R B
authors.initials: IR
authors.lastname: Olivares
authors.forename: Priscila M
authors.initials: PM
authors.lastname: Alves
mesh_terms: D000327:Adsorption; D001938:Brazil; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods / Q000592:standards*; D010636:Phenols / Q000032:analysis* / Q000737:chemistry; D011891:Rain; D015203:Reproducibility of Results; D012621:Seasons; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods / Q000592:standards*; D013696:Temperature; D013997:Time Factors; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D010636:Phenols; D014874:Water Pollutants, Chemical