Determination of ethyl carbamate in wine by high performance liquid chromatography

•Ethyl carbamate (EC) in wine by HPLC with fluorescence detection is quantified.•The kinetics of pre-column derivatization of EC with 9-xanthydrol is studied.•Phosphate buffers at pH=2.5 provide a long-term storage of derivatized samples.•The UV–Vis emission/absorption spectra of xanthyl EC are reco...

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Published in:Food chemistry Vol. 141; no. 2; pp. 1301 - 1305
Main Authors: Ajtony, Zsolt, Szoboszlai, Norbert, Bencs, László, Viszket, Erna, Mihucz, Victor G.
Format: Journal Article
Language:English
Published: Kidlington Elsevier Ltd 15-11-2013
Elsevier
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Summary:•Ethyl carbamate (EC) in wine by HPLC with fluorescence detection is quantified.•The kinetics of pre-column derivatization of EC with 9-xanthydrol is studied.•Phosphate buffers at pH=2.5 provide a long-term storage of derivatized samples.•The UV–Vis emission/absorption spectra of xanthyl EC are recorded.•The EC content of 33 Hungarian wine samples is analysed and evaluated. Kinetics of pre-column derivatization with 9-xanthydrol for the determination of ethyl carbamate (EC) in wine by a previous high performance liquid chromatographic method with fluorescence detection was studied and further developed. The life-time of the derivatized product and its excitation/absorption spectra were systematically investigated. Using low acidity (pH=2.5 set by phosphate buffers) only 3% of 9-xanthyl ethyl carbamate (XEC) decomposes in ∼48h, allowing a prolonged storage time of the derivatized EC conferring more accurate determination for large sample batches. Detection limit of this method is 3μgL−1, while its average recovery is 98.5±4.9%. Calibration is linear up to 400μgL−1. The EC content in 33 Hungarian wine samples ranges from 4.9 to 39.9μgL−1 (average: 17.7μgL−1, median: 16.7μgL−1), while only three of them was slightly over 30μgL−1 EC, it being the maximum allowed concentration in countries already having legislation.
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ISSN:0308-8146
1873-7072
DOI:10.1016/j.foodchem.2013.04.011