Determination of phthalates in wine by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry: Fibre comparison and selection

作者：Carrillo J D; Salazar C; Moreta C; Tena M T^*

来源：Journal of Chromatography A, 2007, 1164(1-2): 248-261.

DOI：10.1016/j.chroma.2007.06.059

• phthalates
• wine
• solid-phase microextraction
• gas chromatography-mass spectrometry
• multi-factor categorical experimental design

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 (FA) 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 5.5 M 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 rose wines.

• 出版日期2007-9-14