title: Determination of phthalates in wine by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry: fibre comparison and selection.
abstract: This paper describes the development of a headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for determining phthalates in wine. The HS-SPME conditions were thoroughly studied: first, the performance of six fibres at three temperature values and two sample volumes was surveyed by means of a 6 x 3 x 2 multi-factor categorical experimental design. From this study, three fibres - carbowax-divinylbenzene (CW-DVB), polyacrylate (PA) and polydimethylsiloxane-divinylbenzene (PDMS-DVB) - were selected. Then, temperature, sample volume and sodium chloride concentration were optimised using a central composite design and the overall desirability function for each fibre. The optimal values were 70 degrees C, a NaCl concentration of 2.6, 3.6 and 5.5M for PA, CW-DVB and PDMS-DVB fibres, respectively, and sample volumes of 4.0, 3.5 and 3.0 mL. Next, the performance characteristics of the three fibres were obtained and compared. PDMS-DVB fibre showed the best repeatability values followed by CW-DVB. PA fibre was not suitable for diethylhexylphthalate extraction and showed poor repeatability for the heavier phthalates, and was therefore discarded. Finally, the performance of CW-DVB and PDMS-DVB fibres was checked for red, white and rosé wines.
authors.affiliation: Department of Chemistry, University of La Rioja, C/Madre de Dios, 51, E-26006 Logroño (La Rioja), Spain.
authors.forename: J D
authors.initials: JD
authors.lastname: Carrillo
authors.forename: C
authors.initials: C
authors.lastname: Salazar
authors.forename: C
authors.initials: C
authors.lastname: Moreta
authors.forename: M T
authors.initials: MT
authors.lastname: Tena
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010795:Phthalic Acids / Q000032:analysis / Q000737:chemistry*; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D014920:Wine / Q000032:analysis*
chemical_list: D010795:Phthalic Acids