Preparation and application of 2,4,6-tribromo-[¹³C₆]-anisole for the quantitative determination of 2,4,6-tribromoanisole in wine
2009
Giannikopoulos, Georgina | Whitfield, F. B. (Frank B)
An expedient preparation of 2,4,6-tribromo-[¹³C₆]-phenol (¹³C₆-TBP) and its conversion to 2,4,6-tribromo-[¹³C₆]-anisole (¹³C₆-TBA) is described. The method involves the bromination of an aqueous solution of ¹³C₆-phenol and subsequent methylation of the corresponding tribromophenol with methyl iodide. Mass spectrometric and nuclear magnetic resonance analyses of ¹³C₆-TBP and ¹³C₆-TBA confirm that their chemical and isotopic purities were better than 99%. The application of ¹³C₆-TBA to the quantitative analysis of the known musty taint 2,4,6-tribromoanisole (TBA) in wine using solid phase microextraction coupled to gas chromatography-mass spectrometry, operated in the selected ion monitoring mode, is described. The detection limit for TBA was 2ngl⁻¹, based on a minimum signal response greater than three times the background noise.
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