摘要
目的:建立加校正因子的主成分自身对照法测定马来酸依那普利片有关物质的含量。方法:用辛烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲溶液(0.01 mol·L^(-1)磷酸二氢钾溶液,用磷酸调pH值为2.2)-乙腈(75∶25)为流动相;检测波长215 nm;柱温为50℃。测定依那普利拉(杂质Ⅰ)和依那普利双酮(杂质Ⅱ)相对于依那普利的校正因子,并进行定量分析。结果:各色谱系统中依那普利与相邻杂质及各已知杂质间分离良好,依那普利和杂质Ⅰ、杂质Ⅱ在0.5~30μg·mL^(-1)浓度范围内线性关系良好(r>0.999);杂质Ⅰ、杂质Ⅱ校正因子分别为0.71、0.92;杂质Ⅰ的定量方式以加校正因子的主成分自身对照法为宜,加校正因子的主成分自身对照法和外标法测得结果无显著性差异。结论:该方法简便快速,可准确测定马来酸依那普利片的有关物质。
Objective:To establish the method of main component self-control corrected with calibration factor to determine the related substances in Enalapril Maleate Tablets.Methods:The test was performed in octyl silane bonded silica gel column under the elution of phosphate buffer solution(adjusting pH to 2.2 with phosphoric acid)-acetonitrile(75∶25).The column temperature was 50℃,and the detection wavelength was 215 nm.The calibration factors of Enalaprilat(impurityⅠ)and enalapril diketopiperazine(impurityⅡ)relative to enalapril were determined,then the quantitative analysis of the impurities was made.Results:The resolutions between Enalapril and the adjacent peaks as well as the known impurities all met the requirements.The calibration curves of Enalapril and impuritiesⅠ,Ⅱwere linear in the range of 0.5-30μg·mL^(-1)(r>0.999).The calibration factors of impuritiesⅠandⅡwere 0.71 and 0.92,respectively.The main component self-control method with calibration factor should be used for quantitative analysis of impurityⅠ.There were no significant differences between the results determined by the external standard method and the main component self-control method with calibration factor.Conclusion:The established method is simple and accurate,and it is suitable for the determination of related substances in Enalapril Maleate tablets.
作者
魏凯
李欣
WEI Kai;LI Xin(Heilongjiang Timehome Pharmaceutical Co.,Ltd.,Harbin 150025,China;Harbin Institute for Food and Drug Control,Harbin 150001,China)
出处
《中国药品标准》
CAS
2021年第1期26-31,共6页
Drug Standards of China
