The method describes a rapid and accurate procedure for the analysis of ethyl carbamate in wines. The separation of the ethyl carbamate (EC), the target analyte, from alcohol and the sample matrix is a challenge to many analytical chemists. After alcohol removal from the sample, EC was extracted and concentrated by solid-phase extraction. For analysis of EC, large-volume injection on a programmable temperature vaporization (PTV) inlet was used followed by multidimensional gas chromatography/mass spectrometry (MDGC/MS) using electron-impact ionization (EI). For quantitation, the ratio of ions produced during EI at m/z 62 (EC) and 64 (isotopically labeled EC) was monitored. The use of solid-phase extraction and MDGC/MS removes the majority of the matrix interference encountered in other methods. A linear dynamic range was established from 0.387 to 1160 ng/mL, with a limit of detection at 0.1 ng/mL and limit of quantitation at 1 ng/mL.

Bureau of Alcohol, Tobacco and Firearms regulations require that a straight whiskey be aged in a freshly charred oak barrel for a minimum of 2 years and that it not be colored with added caramel. The regulations, however, permit addition of caramel in blended whiskeys. Blended whiskeys are usually produced by mixing a straight whiskey with neutral spirits which causes loss of color intensity. Caramel addition is permitted to compensate for this loss. Thus, it is not possible to authenticate the standard of identity of a straight whiskey by measurement of color intensity. Our investigations suggest that furfural (2-furaldehyde) and 5-hydroxymethyl-2-furaldehyde are imparted into a straight whiskey during aging in a freshly charred oak barrel. Caramel, on the other hand, imparts only 5-hydroxymethyl-2-furaldehyde. Thus, the measurement of the concentrations of furfural and 5-hydroxymethyl-2-furaldehyde and their ratio could effectively authenticate the standard of identity of straight whiskeys. This study shows that straight whiskeys aged in freshly charred oak barrels for a period of 2 years or more have a 2:1 or higher ratio of furfural to 5-hydroxymethyl-2-furaldehyde. A high-performance liquid chromatographic method for the determination of furfural and 5-hyroxy- methyl-2-furaldehyde at low parts-per-million levels is described.

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Two direct sample injection methods using liquid chromatography (LC) and gas chromatography coupled with mass spectrometry (GC/MS) were used to determine phthalate residues in grain neutral spirits and vodka. Six reported phthalates were quantitated at concentrations as low as 20 μg/L (20 ppb) with no sample preparation or sample enrichment.