高效液相色谱-荧光检测器法测定黄酒中尿素含量  

Determination of Urea Content in Yellow Rice Wine by High-performance Liquid Chromatography Combined with Fluorescence Detection after Pre-column Derivatisation

作　　者：邢江涛[1,2] 钟其顶[1,2] 熊正河[1] 邹慧君 周建弟 谢广发 

机构地区：[1]中国食品发酵工业研究院,北京100027 [2]全国食品发酵标准化中心,北京100027 [3]中国绍兴黄酒集团有限公司,浙江绍兴312000

出　　处：《酿酒科技》2011年第3期104-106,共3页Liquor-Making Science & Technology

摘　　要：建立了柱前衍生高效液相色谱荧光检测器(HPLC-FLD)测定黄酒中尿素含量的检测方法。采用9-羟基吨为柱前衍生试剂,尿素在酸性环境下与其反应产生具有荧光特性的吨基脲(N-9H-xanthen-9-ylurea),经HPLC分离后在λex=213nm,λem=308nm下荧光检测。方法学指标检测结果表明,方法线性良好(R^2>0.999)、重复性好(RSD=1.5%,n=5)、日间变异试验良好(RSD<5%,n=3),回收率高(平均回收率>90%,n=3);尿素检出限为0.024mg/L,定量限为0.086mg/L。A determination method of urea content in yellow rice wine by using high performance liquid chromatography with fluorescence detection （HPLC-FLD） has been developed. Urea will react with xanthydrol under hydrochloric acid solution to produce fluorescent characteristicN-9H-xanthen-9-ylurea, which could be quantified by using fluorescence detection （λex=213 nm,Xem=308 nm） after chromatographic separation from interferences. The determination results proved that such method had good linear relationship （R2〉0.999）, good repeatability（RSD=1.5 %,n=5）, good stability（RSD 〈 5 %, n=3） and good recovery（〉 90 %,n=3）. The limit of the detection for urea is 0.024 mg/L and the limit of quantification is 0.086 mg/L.

关 键 词：分析检测 尿素 柱前衍生 高效液相色谱-荧光检测器(HPLC—FLD) 黄酒 

分 类 号：O657.7[理学—分析化学] TS261.7[理学—化学]