O acoplamento do extrator por "purge and trap" com a cromatografia gasosa foi utilizado para quantificar o dimetilssulfeto em bebidas alcoólicas. Muito boa performance foi obtida usando-se uma coluna HP-FFAP e um detector seletivo de massas operando em modo SIM (m/z 62): limite de detecção de 8 x 10 -9 mol L -1 ; boa repetibilidade e tempo total de análise de 25 minutos. O método foi aplicado em 60 amostras de bebidas alcoólicas (cachaça, tiquira, grapa, uísque, brandy, vodca, rum e uma tequila). As amostras de cachaças exibiram a maior concentração de dimetilssulfeto (mediana de 3.16 x 10 -4 mol L -1 ) seguidas pelas amostras de grapa (mediana de 1.45 x 10 -4 mol L -1 ). Não foi observada a presença de dimetilssulfeto nas amostras de rum analisadas.A purge and trap concentrator coupled to gas chromatography was used to quantify dimethylsulphide in distilled beverages. A very good performance was obtained using a HP-FFAP column and a mass selective detector operating in SIM mode (m/z 62): detection limit 8 x 10 -9 mol L -1 ; good repeatability and total time of analysis 25 minutes. The method has been applied for sixty samples of alcoholic beverages (cachaças, tiquiras, grappas, whiskies, brandies, vodkas, rum and a tequila). The cachaças exhibit the highest content of dimethylsulphide (median 3.16 x 10 -4 mol L -1 ), followed by grappa (median 1.45 x 10 -4 mol L -1 ). The presence of dimethylsulphide was not observed in the samples of rum.Keywords: cachaça, chromatography, purge and trap, dimethylsulphide, GC-MS
IntroductionBrazilian sugar cane spirit, also called "cachaça", is a distilled alcoholic beverage from fermented sugar cane juice. Although cachaça production is around 1.5 -2 x 10 9 liters per year, only 2.6 x 10 6 liters are exported. Significant improvements can be obtained from knowledge of the cachaça chemical composition; however this subject has only been thoroughly investigated in the last decade. [1][2][3][4][5] Flavor and aroma are the most important sensory characteristics of a beverage. The presence of sulphur compounds in beverages makes the sensorial profile worse as these compounds are known to be responsible for the so-called "off-flavors". [5][6][7][8][9] Sulphur compounds in beverages exhibit different olfactory characteristics, depending on the position of the sulphur atom in the molecule, 5 and probably originate from the degradation of sulphur-containing amino acids. 5 Previous studies carried out in our laboratory indicated that dimethylsulphide (DMS) is the major volatile sulphur component in cachaça and can strongly influence the beverage sensory qualities. 11 The reported analytical methods 5-9,12-15 for DMS determination, based on chromatographic analysis, are laborious, show a low detection limit, and are subject to interferences.As part of our efforts aiming at improving Brazilian cane sugar spirit quality, we describe here a simple and rapid method for the quantitative analysis of DMS in cachaça and other alcoholic matrices, employing the purge and trap technique 16 coupled ...