Analysis of corky off-flavour compounds at ultra trace level with multidimensional gas chromatography-electron capture detection

A robust method for routine quality control of corky off-flavour compounds in wine and cork soak matrices has been established. Based on an automated headspace solid phase microextraction (HS-SPME), the method needs only marginal sample preparation and achieves low (sub-ng L−1) trace level detection limits (LODs) for the most relevant off-flavour compounds, such as 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA) and 2,4,6-tribromoanisole (TBA). Particularly for wine matrix, reliable trace level quantification had only been achieved after applying heart-cutting multidimensional gas chromatography (MDGC). Using a halogen-sensitive electron capture detector (ECD) and quantification with a stable isotope dilution assay (SIDA), LODs of 0.1 ng L−1 for TCA, TeCA and TBA could be obtained. Since a SIDA based quantification method is used with a non-mass spectrometric detector, the necessary chromatographic resolution of internal standard and target analyte peaks resulted from the use of highly deuterated [2H5]-isotopologues.

► Analysis of cork off-flavour haloanisole compounds at sub-ng L−1 level in wine matrix.
► Improved method developed for routine analysis with HS-SPME as sample preparation.
► Matrix problems in wine at trace level could be overcome by applying MDGC.
► Necessary sensitivity was achieved using the sensitive ECD as detector.
► Reliable quantification was with a non-MS SIDA approach.