title: Determination of stale-flavor carbonyl compounds in beer by stir bar sorptive extraction with in-situ derivatization and thermal desorption-gas chromatography-mass spectrometry.
abstract: A method for the determination of stale-flavor carbonyl compounds including E-2-octenal, E-2-nonenal, E,Z-2,6-nonadienal and E,E-2,4-decadienal in beer was developed using stir bar sorptive extraction (SBSE) with in-situ derivatization followed by thermal desorption-GC-MS analysis. The derivatization conditions with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine and the SBSE conditions--sampling mode, salt addition, sample volume, polydimethylsiloxane volume (sample/polydimethylsiloxane phase ratio) and extraction time--were examined. The method showed good linearity over the concentration range from 0.1 to 10 ng ml(-1) for all analytes and the correlation coefficients were higher than 0.9993. The limits of detection ranged from 0.021 to 0.032 ng ml(-1) for all analytes. The recoveries (98-101%) and precision (RSD 2.4-7.3%) of the method were examined by analyzing beer samples fortified at the 0.5-ng ml(-1) level. The method was successfully applied to low-level concentration samples.
authors.affiliation: Application Development Department, Yokogawa Analytical Systems Inc., 2-11-13 Nakacho, Musashino-shi, Tokyo, 180-0006 Japan. nobuo_ochiai@agilent.com
authors.forename: N
authors.initials: N
authors.lastname: Ochiai
authors.forename: K
authors.initials: K
authors.lastname: Sasamoto
authors.forename: S
authors.initials: S
authors.lastname: Daishima
authors.forename: A C
authors.initials: AC
authors.lastname: Heiden
authors.forename: A
authors.initials: A
authors.lastname: Hoffmann
mesh_terms: D001515:Beer / Q000032:analysis*; D005421:Flavoring Agents / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D005421:Flavoring Agents