【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. 5μm）,柱温25℃;以乙腈-水（88∶12）为流动相,流速1. 0 m L·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·m L^-1范围内线性关系良好,最小检出限为4. 03 ng,最小检出量为9. 01 ng。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。更多还原

【Abstract】 Objective: To establish an HPLC-CAD method for determination of urea and its related substances.Methods: The determination was carried out on a Waters XBridge Amide column（ 4. 6 mm × 250 mm,3. 5 μm） at 25 ℃ with acetonitrile-water（ 88∶ 12） as the mobile phase and the flow rate as 1. 0 m L·min^-1. The detector of CAD was applied with a low nebulization temperature as 35 ℃ and collection frequency as 10 Hz,filter constant as3. 6 s,and PFV as 1. 0. Results: The resolutions between urea and its adjacent impurities peaks,and other impurities peaks were more than 1. 5. The linearity of urea was good in the range of 1. 0-504. 0 μg·mL^-1. The LOD and LOQ of urea were 4. 03 ng 9. 01 ng respectively. The RSD of repeatability was 0. 71%. The contents results of six batches ranged from 99. 6% to 100. 7%,which were consistent with that obtained with the current standard.The total impurities contents of the related substances in six batch samples were from 0. 061% to 0. 072%.Conclusion: The established method adopts HPLC-CAD to determine the content of urea and its related substancesfirstly. It is better than the current domestic and international pharmacopoeia methods,and can provide the reference for urea quality control.更多还原