| View Larger Image | Validation of an analytical method for the solid phase extraction, in cartridge derivatization and subsequent gas chromatographic-ion trap tandem mass ... [An article from: Analytica Chimica Acta] | Digitalby L. Cullere (Author), J. Cacho (Author), V. Ferreira (Author)
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| | Binding: | Digital | | Publisher: | Elsevier |
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This digital document is a journal article from Analytica Chimica Acta, published by Elsevier in . The article is delivered in HTML format and is available in your Amazon.com Media Library immediately after purchase. You can view it with any web browser.Description: An analytical method for the quantification in wines of the strong-smelling compound, 1-octen-3-one, has been developed. 1-Octen-3-one is extracted by passing 90mL of wine through a solid phase extraction (SPE) cartridge packed with 90mg of LiChrolut-EN resins. Wine major volatiles and potential interferences are removed by washing up with 9mL of a 40% methanol-water solution containing 1% NaHCO"3. The ketone is subsequently derivatised with O-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine (PFBHA) to form its two isomeric oximes. Reaction takes place in the same cartridge at room temperature (25^oC) in 15min. The excess of reagent is then removed by washing with 20mL of a 0.05M sulphuric acid solution. The corresponding oximes are further eluted with pentane and determined by gas chromatography coupled with ion trap tandem mass spectrometry (GC-MS/MS) by non-resonant fragmentation of the m/z 140 parent ion and subsequent analysis of the corresponding daughter ions (m/z 77, 79, 94 for the trans and m/z 77 and 79 for the cis-isomer, respectively). The analytical signal is highly specific and in all samples the obtained MS spectrum are fully coincident with those from synthetic standards. Recoveries were in all the studied cases 100%. Precision (measured as R.S.D.) is better than 5%, linearity holds at least up to 900ngL^-^1 (r^2=0.9990), and the method detection limit is 0.75ngL^-^1, well below the olfactory threshold of the compound (15ngL^-^1). The range of concentrations found in normal, non-spoiled dry wines goes from 7 to 61ngL^-^1. Sensory experiments have shown, however, that such differences do not seem to be enough to explain sensory differences. |
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