Title page for ETD etd-04032003-195302

Type of Document Master's Thesis
Author Hartmann, Peter J
Author's Email Address Peter_Hartmann@vt.edu
URN etd-04032003-195302
Title The Effect of Wine Matrix Ingredients on 3-Alkyl-2-methoxypyrazines Measurements by Headspace Solid-Phase Microextraction (HS-SPME)
Degree Master of Science
Department Chemistry
Advisory Committee
Advisor Name Title
McNair, Harold M. Committee Chair
Zoecklein, Bruce W. Committee Co-Chair
Taylor, Larry T. Committee Member
  • Alkyl-methoxypyraxines
  • Gas Chromatography
  • Headspace Solid-phase Microextraction
  • Wine
Date of Defense 2002-12-02
Availability unrestricted
The effect of wine matrix ingredients and conditions on the headspace (HS) sampling of 3-alkyl-2-methoxypyrazines was investigated with solid-phase microextraction (SPME) and capillary gas chromatography, using a nitrogen phosphorus detector. Changes in the recovery of 3-ethyl-, isopropyl-, sec-butyl-, and isobutyl-2-methoxypyrazines from the static headspace of synthetic wine matrices spiked with 5mg/L of each analyte were investigated and reported as a function of SPME fiber type, extraction time, and temperature. The influence of pH, ethanol, phenolics, and ground oak was studied.

DVB/Carboxen?/PDMS SPME fibers at an extraction temperature of 50°C for 30 minutes with 30% (w/v) added sodium chloride resulted in the highest analyte recoveries. Although, PDMS (100 micron) SPME fibers at an extraction temperature of 35°C for 30 minutes with 30% (w/v) added sodium chloride resulted in the lower analyte recoveries, the fiber remained functional after 50 to 75 analyses after other coatings deteriorated. Changing the sample ethanol concentration from 0 to 20% (v/v) resulted in an exponential decrease in the recovered analytes. Below pH 2, there was extensive loss of the analytes in the headspace. No measurable impact on alkylmethoxypyrazine headspace concentrations was observed with exposures to selected phenolics and to ground oak.

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