高效液相色谱-荧光检测器法测定白酒中尿素含量方法研究  

Measurement of Urea Content in Baijiu(Liquor) by HPLC-FLD

作　　者：申世刚[1] 李国辉[1,2] 钟其顶[2] 王道兵[2] 崔战友[2] 高红波[2] 熊正河[2] 

机构地区：[1]河北大学化学与环境科学学院,河北省分析科学技术重点实验室,"药物化学与分子诊断"省部共建重点实验室,河北保定071002 [2]中国食品发酵工业研究院,北京100015

出　　处：《酿酒科技》2015年第3期111-114,共4页Liquor-Making Science & Technology

基　　金：国家自然基金(31101333);国家科技支撑计划(编号:2012BAK17B11);质检公益项目(编号:201210104)

摘　　要：建立一种利用高效液相色谱结合荧光检测器准确、快速测定白酒中微量尿素的方法。白酒样品经9-羟基吨在酸性、避光条件下衍生30 min后,直接进样分析。采用C18色谱柱分析,流动相为乙腈和0.02 mol/L乙酸钠溶液(p H7.2),检测器波长为λex=213 nm,λem=308 nm。方法在线性范围内相关系数R2=0.9999;检测限和定量限分别为0.021 mg/L和0.071 mg/L;平均回收率及回收率相对标准偏差(RSD)分别为97.71%和3.61%;日内和日间精密度分别为1.63%和1.98%。该方法方便快速,精度高、分离度好,适合于白酒中微量尿素的测定。A rapid,sensitive,reproducible and inexpensive method for the measurement of urea content in Baijiu（liquor） had been developed by HPLC-FLD. Liquor samples were derivated with 9-xanthydrol in acidic photophobic conditions, 30 min later, direct sample injection analysis was done. C18 column was used and the mobile phase were acetonitrile and 0.02 mol/L sodium acetate solution （pH 7.2）.Theλex andλem of flu-orescence detector were 213 nm and 308 nm respectively.The correlation coefficient of this method was above 0.9998, the limits of detection and quantification were 0.021 mg/L and 0.071 mg/L respectively, the relative standard deviations of both the in-day and inter-day precision were 1.63%and 1.98%, the average recovery rate and the average RSD were 97.71%and 3.61%respectively. Such method was suitable for the determination of trace urea in Baijiu（liquor）.

关 键 词：高效液相色谱-荧光检测器 尿素 白酒 9-羟基吨 衍生化 

分 类 号：O657[理学—分析化学] TS262.3[理学—化学]