中国药物警戒 ›› 2016, Vol. 13 ›› Issue (3): 143-145.

• 质量与工艺研究 • 上一篇    下一篇

电位滴定法和高效液相色谱法测定乌拉地尔含量的比较

耿庆光1,职雪莹2,郭欢迎1   

  1. 1陕西省食品药品检验所,陕西 西安 710065;
    2陕西中医学院,陕西 咸阳 712046
  • 收稿日期:2015-12-14 修回日期:2016-04-12 出版日期:2016-03-20 发布日期:2016-04-12
  • 作者简介:耿庆光,女,副主任药师,药物分析。
  • 基金资助:
    陕西省社会科学基金项目（13G020）。

Content Determination of Urapidil by Potentiometry Titration and HPLC

GENG Qing-guang1， ZHI Xue-ying2， GUO Huan-ying1，   

  1. 1. Shanxi Institute for Food and Drug Control, Shanxi Xi’an 710065, China;
    2. Shanxi University of Chinese Medicine, Shanxi Xianyang 712046, China
  • Received:2015-12-14 Revised:2016-04-12 Online:2016-03-20 Published:2016-04-12

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摘要： 目的 确定乌拉地尔原料更科学合理的含量测定方法 。方法 采用梅特勒DL-55型自动电位滴定仪,以冰醋酸和醋酐为溶剂,用高氯酸滴定液进行电位滴定。高效液相色谱法采用色谱柱为Syncronis C18（100 mm×2.1 mm, 1.7 μm）;流动相为乙腈-0.05 mol·L-1磷酸二氢钠溶液（20:80）,流速1.0 mL·min-1;检测波长268 nm;柱温35℃。结果 电位滴定法的平均回收率为99.98%, RSD为0.41%（n=3）。高效液相色谱法的平均回收率为100.93%, RSD为0.60%（n=3）。电位滴定法和高效液相色谱法的测定结果 在统计学上有显著性差异,电位滴定法回收率测定结果 更接近100%。结论 电位滴定法测定乌拉地尔的含量避免了对照品引起的误差,操作简单、快速,测定结果 准确度高,更适宜于乌拉地尔原料的含量测定。

关键词: 乌拉地尔, 含量测定, 电位滴定法, 高效液相色谱法

Abstract: Objective To confirm the content determination method of urapidil in raw materials more scientifically and reasonably. Methods Mettler DL-55 potentiometric titration was used to titrate the content of urapidil by perchloric acid. Acetic acid and acetic anhydride were used as solvent. HPLC method was performed on a Syncronis C18 column (100 mm×2.1 mm,1.7 μm). The mobile phase was acetonitrile-0.05 mol·L-1 NaH2PO4 (20:80) with the flowing rate of 1.0 mL·min-1. The detection wavelength was set at 268 nm and the column temperature at 35℃. Results The average recovery rate of potentiometry titration was 99.98% and RSD was 0.41% (n=3). The average recovery rate of HPLC was 100.93% and RSD was 0.60% (n=3). The results of potentiometry titration and HPLC had significant statistic difference, and the recovery rate of potentiometry titration was closer to 100%. Conclusion Potentiometry titration could avoid the error due to the standard substance. The method is simple, fast, accurate and can be used to determine the content of urapidil.

Key words: urapidil, content determination, potentiometry titration, HPLC

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