title: Trace level analysis of corky off-flavor compounds: development of a new analytical method based on solid phase extraction and analysis by multidimensional gas chromatography with mass spectrometric detection.
abstract: This work describes the development of a trace level (<1 ngL(-1)) analysis of haloanisoles in complex wine matrix. The suggested method involves sample preparation based on solid phase extraction, a clean-up to remove acidic compounds, concentration of the haloanisole fraction and large volume on-column injection into a multidimensional GC-MS system. Mass spectrometric detection in the selected ion mode allowed reliable quantification of 2,4,6-trichloroanisole (TCA) or 2,4,6-tribromoanisole (TBA), via their highly deuterated ([(2)H5]) isotopologues as internal standards (stable isotope dilution analysis; SIDA), which had prior been synthesized in house. The development of this new method had become necessary, as a one-dimensional HS-SPME-GC-ECD method, routinely applied for analysis of TCA in cork soaks, had to be extended for TeCA and TBA determination, but failed due to co-elutions within wine matrices. The newly developed SPE//MDGC-MS method provided detection limits well below olfactory thresholds of the analytes with 0.05 ngL(-1) (LOD), 0.19 ngL(-1) (LOQ) for TCA, 0.06 ngL(-1) (LOD), 0.21 ngL(-1) (LOQ) for TeCA, and 0.09 ngL(-1) (LOD), 0.34 ngL(-1) (LOQ) for TBA.
authors: Dienstleistungszentrum Ländlicher Raum Rheinpfalz, Competence Centre for Wine Research, Breitenweg 71, D-67435 Neustadt an der Weinstraße, Germany. hans-georg.schmarr@dlr.rlp.de
authors: Hans-Georg
authors: HG
authors: Schmarr
authors: Stefan
authors: S
authors: Koschinski
authors: Wei
authors: W
authors: Sang
authors: Petra
authors: P
authors: Slabizki
mesh_terms: D000840:Anisoles / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007553:Isotope Labeling; D057230:Limit of Detection; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D014920:Wine / Q000032:analysis*
chemical_list: D000840:Anisoles