Apparatus and Procedure for Reproducible, High-Resolution Gas Chromatographic Analysis of Alcoholic Beverage Headspace Volatiles

Abstract

A readily established method is reported for concentrating headspace volatiles on a bed of the porous polymer, Chromosorb 105. The trapped components are transferred by a desorption tech nique onto a small plug of SF96 coated support material. The volatiles can then be injected onto a high-resolution gas chromatographic column by a simple process.The apparatus required and the steps involved in the procedure are discussed in detail. The precision of the method for the quantitative determination of alcoholic beverage headspace volatiles is assessed for a range of typical compounds.Examples are given of applications of the technique to the analysis of alcoholic spirits and beverages.

Contributions of mass spectrometry in the Australian Wine Research Institute to advances in knowledge of grape and wine constituents

“…This can increase the signal-to-noise ratio in instrumental analyses (Simpson 1978b). Unfortunately, conventional headspace concentration procedures can present various problems, especially with repeatability, although in the early days (Rankine et al 1969) static headspace extraction facilitated quicker and more accurate diacetyl determination than the corresponding chemical method, and Williams and Strauss (1977) demonstrated precise determination of volatiles in the headspace of wine and spirits. More recently, we have used static headspace with some success for the analysis of volatile compounds linked to the spicy 'black pepper' aroma of Shiraz (Pollnitz et al 2004b) and in the sensitive quantitative analysis of low molecular weight sulfur compounds (Siebert et al, manuscript in preparation).…”

“…The resulting ions, molecular ions and/or their fragment ions, are subsequently introduced into a mass analyser to separate them according to their mass to charge ratio (m/z), before they are detected and recorded as a mass spectrum. Distillation of spirits Connell and Strauss (1974); Williams (1976); Strauss and Williams (1983); Strauss (1975, 1978a,b,e) Flor sherry volatiles Williams and Strauss (1978c,d) Method development in distillation ; Williams et al(1981a) Method development in wine aroma ; Williams and Strauss (1977); Simpson (1979b); Williams (1982) compounds Wine aroma compounds Simpson et al (1977); Simpson (1978aSimpson ( ,b, 1979aSimpson ( ,c, 1980; Miller (1983, 1984) Off flavours in wine Craig and Heresztyn (1984); Strauss and Heresztyn (1984); Strauss et al (1985a,d); Heresztyn (1986a); Simpson et al (1986); Amon et al (1987Amon et al ( , 1989 Grape flavour Williams et al (1980aWilliams et al ( ,b,c, 1981bWilliams et al ( , 1982aWilliams et al ( ,b, 1983aWilliams et al ( ,b, 1985a; Dimitriadis and Williams (1984a,b); Wilson et al (1984aWilson et al ( ,b, 1986; Strauss et al (1985bStrauss et al ( ,c, 1986Strauss et al ( , 1987aStrauss et al ( ,b, 1988; Sefton et al (1989); Williams (1989) For involatile molecules, typically analysed by LC-MS (bottom half of Figure 2) an overview of the process is given in the following steps.…”

Assessment of aroma impact compounds in a cashew apple-based alcoholic beverage by GC-MS and GC-olfactometry

“…The understanding of the aroma profile will help technologists to enhance the sensory quality of this beverage. Dynamic headspace techniques are widely used for alcoholic beverages analysis (Williams & Strauss, 1977;Shimoda, Shibamoto, & Noble, 1993 Cela-Torrijos, 1995) because the porous polymers, specially Porapak Q, show low retention for ethanol which often obliterates a large part of the chromatograms.…”

The Influence of Film Yeast Activity on the Aroma Volatiles of Flor Sherries-a Study of Volatiles Isolated by Headspace Sampling

“…The wine was then hcadspace sampled according to the standard procedure, the precision of which has been repor ted. 22 The normalized peak ratio for each compound (i.e. the quotient of the GC peak height or area to the peak height of the internal standard) was determined.…”