高效液相色谱法测定面粉及其制品中的硫脲

Determination of thiourea in flour and flour products by high performance liquid chromatography

目的建立一种测定面粉及其制品中硫脲含量的高效液相色谱检测方法。方法样品经水超声提取、过滤后,经Inertsil CX阳离子交换色谱柱进行分离,流动相为乙腈和含1%乙酸及0.2%乙酸铵的水溶液,二极管阵列检测器检测,检测波长为240 nm,外标法定量。结果硫脲在0.5~50.0 mg/L浓度范围内线性关系良好,相关系数为r=0.9996;方法检出限(S/N=3)为2.0 mg/kg;平均回收率在85.1%~97.8%之间,相对标准偏差(relative standard deviation,RSD)为0.95%~1.5%。结论本研究建立的方法快速、准确,适用于面粉及其制品中硫脲的检测。

Objective To establish a method for determination of thiourea in flour and flour products by high performance liquid chromatography（HPLC）. Methods Samples were extracted and filtered ultrasonically with water as the solvent. An Inertsil CX cation ion exchange column（4.6 mm×250 mm, 5 μm） was used with the mobile phase which consisted of acetonitrile and water with 0.1%acetic acid＋0.2%ammonium acetate. The UV detection wavelength was 240 nm. The external standard method was applied for the quantification. Results Thiourea had a good linear relationship at the range of 0.5~50.0 mg/mL, and the correlation coefficient（r） was 0.9996. The limit of detection（LOD） was 2.0 mg/kg（S/N=3）. The average recoveries were 85.1%~97.8%, and the relative standard deviations were 0.95%~1.5%. Conclusion The established method is simple and accurate, which can be used for determination of thiourea in flour and flour products.