A simple and sensitive method for the analysis of volatile and semi-volatile sulphur compounds in beer at trace levels was developed using headspace solid-phase microextraction (SPME) and gas chromatography with pulsed flame photometric detection. Different SPME fibres were tested and a Carboxen-polydimethylsiloxane coated fibre was found to be the most appropriate. The adsorption and desorption conditions were optimised. The effect of ethanol concentration in the sample on the extraction of analytes was examined. A 60 m non-polar capillary column preceded by a 10 m length of a polar column was found to be capable of separating a wide range of C1-C6 sulphur compounds. The pulsed flame photometric detector enabled increased sensitivity to be obtained over previous methods, such as dynamic headspace followed by conventional flame photometric detection or sulphur chemiluminescent detection, with high sulphur selectivity. Two sulphur compounds, 2-methyl-1-butanethiol and 3-methylthiophene, were identified in beer for the first time.
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