Optimization of Modern Analytical SPME and SPDE Methods for Determination of <Emphasis Type="Italic">Trans</Emphasis>-2-nonenal in Barley,Malt and Beer |
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Authors: | Zdenek Svoboda Renata Mikulíková Sylvie Běláková Karolína Bene?ová Ivana Márová Zdenek Nesvadba |
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Institution: | 1.Research Institute of Brewing and Malting,Malting Institute,Brno,Czech Republic;2.Faculty of Chemistry,Brno University of Technology,Brno,Czech Republic;3.Agrotest Fyto,Kromě?í?,Czech Republic |
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Abstract: | Trans-2-nonenal is an aldehyde contributing to an unpleasant off-flavor and odor of rancid butter in stored beer. The automated solid-phase microextraction technique (SPME) coupled with gas chromatography (GC) and solid-phase dynamic extraction (SPDE) coupled with gas chromatography were optimized and introduced to determine trans-2-nonenal in barley, malt and beer. Five types of SPME fibers coated with different stationary phases (100 μm PDMS, 65 μm PDMS/DVB, 85 μm CAR/PDMS, 50/30 μm DVB/CAR/PDMS, 85 μm PA) and two needles (PDMS, PDMS/AC) were compared and tested for their efficiencies in the headspace (HS) SPME and SPDE determination of trans-2-nonenal in barley, malt and beer. The highest extraction efficiency of HS-SPME was achieved with the PDMS/DVB fiber, and addition of 1.5 g of NaCl, extraction time was 20 min at 60 °C. The highest extraction efficiency of HS-SPDE was obtained with the PDMS needle, 15 extraction strokes at 60 °C and addition of 1.5 g of NaCl. Trans-2-nonenal was identified with the method of HS-SPME coupled gas chromatography-mass spectrometry (GC–MS); the samples were analyzed using the HS-SPME-GC-coupled gas chromatography-flame ionization detector (GC-FID) technique. |
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