Determination of ethyl carbamate in wine by high performance liquid chromatography

摘要

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 ～48 h, allowing a prolonged storage time of the derivatized EC conferring more accurate determination for large sample batches. Detection limit of this method is 3 μg L~(-1), while its average recovery is 98.5 ±4.9%. Calibration is linear up to 400 μg L~(-1). The EC content in 33 Hungarian wine samples ranges from 4.9 to 39.9 μg L~(-1) (average: 17.7 μg L~(-1) median: 16.7 μg L(-1)), while only three of them was slightly over 30 μg L~(-1) EC, it being the maximum allowed concentration in countries already having legislation.