| Title: | Comparison of extraction techniques and mass spectrometric ionization modes in the analysis of wine volatile carbonyls |
| Author(s): | Zapata J; Mateo-Vivaracho L; Cacho J; Ferreira V; |
| Address: | "Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, I3A, Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza, Spain" |
| DOI: | 10.1016/j.aca.2009.09.041 |
| ISSN/ISBN: | 1873-4324 (Electronic) 0003-2670 (Linking) |
| Abstract: | "This work presents a comparative study of the analytical characteristics of two methods for the analysis of carbonyl compounds in wine, both based on the derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). In the first method derivatives are formed in the solid phase extraction (SPE) cartridge in which the analytes have been previously isolated, while in the second method derivatives are formed in a solid phase microextraction (SPME) fibre saturated with vapors of the reagent and exposed to the sample headspace. In both cases detection has been carried out by electron impact (EI) or negative chemical ionization (NCI) mass spectrometry. The possibility of determining haloanisols simultaneously has been also considered. The method based on SPE presents, in general, better analytical properties than the SPME one. Although linearity was satisfactory for both methods (R(2)>0.99), repeatability of the SPE method (RSD<10%) was better than that obtained with SPME (9% < RSD < 20%). Detection limits obtained with EI are better for the SPE method except for trihaloanisols, while with NCI detection limits for both strategies are comparable, although the SPME strategy presents worse results for ketones and methional. Detection limits are always lower with NCI, being the improvement most notable for SPME. Recovery experiments show that in the case of SPE, uncertainties are lower than 12% in all cases, while with the SPME method the imprecision plus the existence of matrix effects make the global uncertainty to be higher than 15%" |
| Keywords: | Aldehydes/analysis/chemistry Gas Chromatography-Mass Spectrometry/*methods Hydroxylamines/chemistry Limit of Detection Solid Phase Extraction/*methods Solid Phase Microextraction/*methods Volatile Organic Compounds/*analysis/chemistry Wine/*analysis; |
| Notes: | "MedlineZapata, Julian Mateo-Vivaracho, Laura Cacho, Juan Ferreira, Vicente eng Comparative Study Research Support, Non-U.S. Gov't Netherlands 2010/01/28 Anal Chim Acta. 2010 Feb 15; 660(1-2):197-205. doi: 10.1016/j.aca.2009.09.041. Epub 2009 Oct 1" |
