New HPLC Method to Determine Ethyl Carbamate in Alcoholic Beverages Using Fluorescence Detection

Abstract

A new methodology to the quantification of ethyl carbamate (EC) has been developed. This method allows the analysis by HPLC of ethyl carbamate in samples of wine, fortified wine, and wine brandy, by a precolumn derivatization with 9-xanthydrol, and fluorescence detection. This does not require previous sample extraction or concentration. The method presents an average recovery of 96% among samples studied, a detection limit of 4.2 µg/L, and an average intermediate precision of 6.3%. The comparison of the results obtained for EC analysis on the same wine brandy samples by GC/MS and HPLC are statistically indistinguishable with 97.5% probability. The results of the analysis of 42 samples are presented.

Effect of light on the concentration of ethyl carbamate in cachaça stored in glass bottles

“…The values were 3.81 and 11.53 μg L À1 , respectively. Values shown are in the range of other studies that have applied the same technique, with detection limits ranging from 0.02 to 4.20 μg L À1 and quantification limits varying from 0.05 to 4.00 mg L À1 (16,17,25,26). The concentrations of EC encountered in samples of cachaça stored in the presence and absence of light and analysed every 2 months for 6 months are described in Table 1.…”

Identificação do carbamato de etila durante o armazenamento da cachaça em tonel de carvalho (quercus sp) e recipiente de vidro

“…Alguns trabalhos realizados com diferentes bebidas alcoólicas têm apresentado valores que variam de 1,64 a 4,2 μg L -1 , para o limite de detecção, e de 3,56 μg L -1 a 4 mg L -1 , para o limite de quantificação. 6,12,13 A Tabela 1 mostra os resultados obtidos para a quantificação do CE nas frações "cabeça", "coração" (cachaça nova) e "calda".…”

“…[12][13][14] Os reagentes empregados para análise foram padrão de carbamato de etila (Acros Organics), etanol, propanol, hexano, ácido clorídrico (HCl), acetato de etila, acetato de sódio, acetonitrila grau HPLC (Merck), água ultrapura e 9-xantidrol (Acros Organics). Para as análises, foi realizada a purificação do 9-xantidrol por meio de sucessivas recristalizações em hexano.…”

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

“…Under these conditions, many reactions can occur leading to significant changes in wine, some are crucial to the final remarkable characteristics of Madeira wine, however it may also cause production of ethyl carbamate (EC). According to Stevens and Ough [2], under fairly normal storage temperatures (13)(14)(15)(16)(17)(18)(19)(20)(21)(22)(23)(24) • C), and not uncommon concentrations of urea (1-10 mg/L), a significant amount of EC will accumulate in wine.…”

“…Several extraction methodologies have been used, such as continuous liquid-liquid extraction [13], and solid phase extraction [7,14,15], combined with one-dimensional gas chromatography coupled with mass spectrometry detection (GC-MS). EC has been determined in fortified Madeira wines by SPE followed by GC-MS [15,16], and by derivatization with 9-xanthydrol, followed by high performance liquid chromatography (HPLC) [17]. More recently, a solvent-free methodology was used: solid phase microextraction (SPME) [9,18,19].…”