Solid-phase microextraction on-fiber derivatization for the analysis of some polyphenols in wine and grapes using gas chromatography-mass spectrometry

J Chromatogr A. 2009 Feb 27;1216(9):1279-84. doi: 10.1016/j.chroma.2008.12.058. Epub 2008 Dec 27.


The present study describes a new environmentally friendly sample pretreatment system based on solid-phase microextraction (SPME) for the sensitive determination of polyphenols. A derivatization process was necessary to convert the polar non-volatile compounds into volatile derivatives. Direct immersion (DI) SPME was used for the adsorption of polyphenols, and then the fiber was placed in the headspace of the derivatizing reagent, bis(trimethylsilyl)trifluoroacetamide (BSTFA). The separation was carried out by coupling gas chromatography with mass spectrometry in the selected ion monitoring mode, after silylation. Optimal extraction conditions were 25 degrees C for 10 min under continuous stirring using DI and a polyacrylate fiber. After extraction, the fiber was inserted into the headspace of BSTFA (10 microL) and the polyphenols were derivatized for 15 min at 50 degrees C. Desorption was carried out at 280 degrees C for 5 min. The method allowed the determination of both isomers cis- and trans-resveratrol, piceatannol, catechin and epicatechin in wine and grapes, and it was validated for linearity, detection and quantitation limits, selectivity, accuracy and precision. Detection limits ranged from 0.05 to 0.9 ng mL(-1) at a signal-to-noise ratio of 3, depending on the compound. Recoveries obtained for spiked samples were satisfactory for all compounds.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Analysis of Variance
  • Flavonoids / analysis*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Green Chemistry Technology / methods
  • Least-Squares Analysis
  • Phenols / analysis*
  • Polyphenols
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Solid Phase Microextraction / methods*
  • Stereoisomerism
  • Vitis / chemistry*
  • Wine / analysis*


  • Flavonoids
  • Phenols
  • Polyphenols