| 摘要: |
| 建立了一种高效液相色谱法测定卡巴匹林钙及其反应液中尿素的新方法，确立了最优色谱条件，色谱柱为C18（4.6mm×250mm,5μm），流动相为甲醇-水（5:95，V/V），检测波长为195nm，流速为0.5mL/min，柱温30℃，进样量10μL。该方法的尿素浓度在0.12μg/mL～123.86μg/mL范围内线性关系良好，相关系数r＞0.999，检出限为0.5μg/mL，定量限为1.0μg/mL；分离度R≥1.5，相对标准偏差RSD＜1.0% (n=6)，卡巴匹林钙加标回收率在98.10%～100.46%之间，反应液加标回收率在95.32%-100.79%之间。实验结果表明该法操作简便、准确度高、重复性好，检测速度快，为合成工艺中卡巴匹林钙及其反应液中尿素的质量控制提供依据。 |
| 关键词: 高效液相色谱法 卡巴匹林钙 反应液 尿素 |
| DOI： |
| 投稿时间：2019-10-17修订日期：2020-01-15 |
| 基金项目:山东省“泰山学者”建设工程基金项目 |
|
| Determination of Urea in Carbasalate calcium and Reaction Solutions by HPLC |
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| (1. Qingdao University of Science & Technology, Shandong Chemical Industry Research Institute, Jinan 250014, Shandong，China; 2. Chemical Technology Academy of Shandong Province, Organic Reaction in Aqueous Engineering Research Center of Shandong Province, Jinan 250014，Shandong，China) |
| Abstract: |
| 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 C18 column(250 mm×4.6 mm,5μm). Methanol-water(5:95) was taken as mobile phase at a flow rate of 0.5mL/min, and detection wavelength was 195nm, column temperature was 30℃, the injection volume was 10μL.The calibration curve was linear in the range of 0.12μg/mL～123.86μg/mL, the linear correlation coefficient r>0.999, and limit of detection was 0.5μg/mL, limit of quantity was 1.0μg/mL. The resolution was more than 1.5,the relative standard deviation of this method was within 1% (n=6), and the standard addition recoveries were in the range of 98.6%～102.3%. 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. |
| Key words: HPLC Urea Carbasalate calcium Reaction solution |
