Zhou Jinsen, Liu Cimin, Chen Yong, Luo Xiaoyan, Deng Dongsheng
Laboratory Department, Guangzhou Huangpu Center for Disease Control and Prevention, Xinyang West Road 23, Guangzhou 510530, P. R. China.
Guangdong Provincial Engineering Research Center for Reverse Engineering of Industrial Additives, Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology, Institute of Analysis, Guangdong Academy of Sciences (China National Analytical Center,Guangzhou), Xianlie Middle Road 100, Guangzhou 510070, P. R. China.
J Chromatogr Sci. 2023 Apr 24;61(4):339-346. doi: 10.1093/chromsci/bmac025.
A reversed-phase isocratic elution high-performance liquid chromatography method coupled with fluorescence detection has been developed to determine urea concentration via online postcolumn derivatization. Swimming pool water samples were filtered through 0.20 μm syringe filters. When the temperature of reaction coil was 40°C, urea was derivatized well with xanthydrol methanol solution (0.1 g/L) containing 0.50% hydrochloric acid with a flow rate of 0.20 mL/min. Successful separation was achieved by using Shim-pack VP-ODS C18 (250 mm × 4.6 mm, 5 μm) column, with a mobile phase containing phosphoric acid solution (0.01 mol/L) at a flow rate of 0.80 mL/min. Retention time and external standard method were used for qualitative and quantitative urea analysis, respectively. Under the established conditions, the limit of detection, linear range, correlation coefficient, recovery and relative standard deviation was 0.09 mg/L, 1.0-100.0 mg/L, 0.9998, 87.0-105.3% and 0.95-4.8%, respectively. Ammonia, thiourea and trichloroisocyanuric acid did not interfere with urea analysis. The method showed satisfactory results with high precision, accuracy, recovery, as well as sensitivity, for the determination of urea in swimming pool water.
建立了一种反相等度洗脱高效液相色谱法结合荧光检测，通过在线柱后衍生来测定尿素浓度。游泳池水样通过0.20μm的注射器滤膜过滤。当反应盘管温度为40℃时，尿素能与含0.50%盐酸的0.1g/L茚三酮甲醇溶液以0.20mL/min的流速良好衍生。使用Shim-pack VP-ODS C18（250mm×4.6mm，5μm）色谱柱，以含0.01mol/L磷酸溶液的流动相，流速为0.80mL/min，实现了成功分离。分别采用保留时间和外标法对尿素进行定性和定量分析。在既定条件下，检测限、线性范围、相关系数、回收率和相对标准偏差分别为0.09mg/L、1.0 - 100.0mg/L、0.9998、87.0 - 105.3%和0.95 - 4.8%。氨、硫脲和三氯异氰尿酸不干扰尿素分析。该方法在测定游泳池水中尿素时，具有高精度、准确性、回收率以及灵敏度，结果令人满意。
