文章摘要
赵恂,袁耀佐,范青峰.尿素及其有关物质含量的HPLC-CAD分析研究[J].中国药品标准,2018,19(6):453-458
尿素及其有关物质含量的HPLC-CAD分析研究
Determination of Urea and Its Related Substances by HPLC-CAD
投稿时间:2018-10-22  修订日期:2018-11-30
DOI:
中文关键词: 尿素,HPLC-CAD,电喷雾检测器,含量测定,有关物质
英文关键词: Urea, HPLC-CAD, Charged Aerosol Detection, assay, related substances
基金项目:国家重大新药创制-化药制剂质量评价关键技术研究课题
作者单位E-mail
赵恂 江苏省食品药品监督检验研究院 zhaoxun9999@sina.com 
袁耀佐* 江苏省食品药品监督检验研究院 yyzyz7256@sina.cn 
范青峰 江苏省食品药品监督检验研究院  
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中文摘要:
      目的:建立尿素及其有关物质含量的HPLC-CAD分析测定法。 方法:采用Waters XBridge Amide(4.6mm×250 mm,3.5 μm),柱温25 ℃;以乙腈-水(88:12)为流动相,流速1.0 mL?min-1;检测器为电喷雾检测器(CAD),雾化温度LOW(35℃);幂率1.0;采样频率10 Hz;过滤常数3.6 s。结果:尿素与相邻杂质以及各杂质峰间的分离度均大于1.5;尿素在1.0~504.0μg?mL–1范围内线性关系良好,最小检出限为4.03ng,最小检出量为9.01ng。重复性RSD为0.71%。 6个批次样品含量测定结果在99.6%~100.7%范围内,与用现行标准测定结果一致。6个批次样品有关物质结果总杂质量在0.061%~0.072%范围内。 结论:本方法首次采用HPLC-CAD法对尿素的含量及其有关物质进行测定,优于现行国内外药典标准,可为尿素质量控制提供参考。
英文摘要:
      Objective: To establish an HPLC-CAD method for the determination of urea and its related substances. Methods: The determination was carried out on a Waters XBridge Amide(4.6mm×250 mm, 3.5 μm) column at 25℃, with acetonitrile-water(88:12) as mobile phase at a flow rate 1.0 mL?min-1.The detector of CAD was applied with at a low nebulization temperature at 35℃ and collection frequency at 10 Hz, filter constant at 3.6 s, and PFV at 1.0. Results: Urea and its impurities were well separated by this method. The linearity of urea was fine in the range of 1.0-504.0μg?mL–1 for the related substances determination. The LOD was 4.03ng and LOQ was 9.01ng. The RSD of repeatability was 0.71%. The results of determination of the sample content of the six batches ranged from 99.6% to 100.7%, which was consistent with the results of the current standard. The total impurity amount of the relevant substances in the six batch samples is in the range of 0.061% to 0.072%.Conclusion: The established method is first to use HPLC-CAD method to determine the content of urea and its related substances, which is better than the current domestic and international pharmacopoeia standards that can provide reference for urea quality control.
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