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

J Chromatogr A. 2007 Sep 14;1164(1-2):248-61. doi: 10.1016/j.chroma.2007.06.059. Epub 2007 Jul 3.


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.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Phthalic Acids / analysis
  • Phthalic Acids / chemistry*
  • Reproducibility of Results
  • Solid Phase Microextraction / methods*
  • Wine / analysis*


  • Phthalic Acids