Department of Food Quality Assurance, Institute of Food Sciences, Faculty of Agricultural and Food Sciences, University of West Hungary, Lucsony u. 15-17, H-9200 Mosonmagyaróvár, Hungary.
Food Chem. 2013 Nov 15;141(2):1301-5. doi: 10.1016/j.foodchem.2013.04.011. Epub 2013 Apr 18.
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.
采用柱前衍生-高效液相色谱荧光检测法分析酒中氨基甲酸乙酯（EC），本文对该方法中 9-芴酮衍生化反应动力学进行了研究和进一步发展。文中系统考察了衍生化产物的寿命及其激发/吸收光谱。采用低酸度（通过磷酸盐缓冲液设定 pH=2.5），只有 3%的 9-芴基乙基氨基甲酸酯（XEC）在约 48 小时内分解，从而使衍生化 EC 具有更长的储存时间，更有利于大样本批次的准确测定。该方法的检测限为 3μg/L，平均回收率为 98.5±4.9%。校准曲线在 400μg/L 范围内呈线性。33 份匈牙利葡萄酒样品中 EC 的含量范围为 4.9 至 39.9μg/L（平均值：17.7μg/L，中位数：16.7μg/L），其中只有三份样品的 EC 含量略高于 30μg/L，而这一数值是已经制定相关法规的国家所允许的最大浓度。
