高效液相色谱法测定卡巴匹林钙产品与反应液中尿素的含量

Determination of Urea in Carbasalate Calcium and Reaction Solution by HPLC

建立了一种用于测定卡巴匹林钙产品及反应液中尿素含量的高效液相色谱法。确立了最佳色谱条件,色谱柱为Waters Xselect HSS T3 C18(4.6 mm×250 mm,5μm),流动相为甲醇-水(5∶95,V/V),检测波长为195 nm,流速为0.5 mL/min,柱温30℃,进样量10μL。结果显示,尿素浓度在0.12~120μg/mL范围内具有良好的线性关系(r>0.999);尿素的检出限为0.05μg/mL,定量限为0.1μg/mL;分离度R>1.5,重复性的相对标准偏差<1.0%(n=6);卡巴匹林钙产品中尿素的回收率范围为98.10%~100.46%,反应液中尿素的回收率范围为95.32%~101.20%。本方法操作简便、准确度高、重复性好、检测速度快,在合成工艺中对卡巴匹林钙产品及反应液中尿素的质量控制具有重要意义。

A new method for the determination of urea in carbasalate calcium and its reaction solution by HPLC was established,and the optimum chromatographic conditions were established.The determination was carried out with a Waters Xselect HSS T3 C18 column(250 mm×4.6 mm,5μm).Methanol-water(5∶95)was taken as mobile phase at a flow rate of 0.5 mL/min,and detection wavelength was 195 nm,column temperature was 30℃,the injection volume was 10μL.The results showed that a good linear relationship was accepted in the range of 0.12~120μg/mL(r>0.999).and limit of detection was 0.05μg/mL,limit of quantity was 0.1μg/mL.The resolution was more than 1.5,the relative standard deviation of this method was within 1.0%(n=6;the recovery rate of urea in carbasalate calcium were in the range of 98.10%~100.46%,the recovery rate of urea in its reaction solution were in the range of 95.32%~101.20%.The experimental results show that the method is simple,accurate,and fast,which provides the basis for the quality control of urea in carbasalate calcium and its reaction solution.