摘要
目的:建立测定苯唑嗪胶囊中主成分及有关物质含量的方法。方法:采用高效液相色谱法测定主成分含量,采用主成分自身对照法计算有关物质(已知杂质1、已知杂质2、总杂质)的含量。色谱柱为Inertsil ODS-2 C18,流动相为乙腈-水(55∶45,V/V),流速为1.0 m L/min,检测波长为223 nm,柱温为25℃,进样量为20μL。结果:苯唑嗪主成分与杂质分离度良好,苯唑嗪检测质量浓度线性范围为20.04~60.12μg/mL(r=1.000 0);精密度、稳定性(24 h)、重复性试验的RSD均≤0.5%(n=6);平均回收率为97.50%(RSD=0.36%,n=3);苯唑嗪的检测限和定量限分别为0.91、3.04 ng。在3批样品中,苯唑嗪、已知杂质1、已知杂质2、总杂质含量的平均值分别为106.68%、0.002 1%、0.044 0%、0.046 2%。结论:建立的苯唑嗪胶囊中主成分及有关物质的含量测定方法简便、专属性强、灵敏度高,结果准确,适用于苯唑嗪胶囊的质量控制。
OBJECTIVE:To establish a method for content determination of main components and its related substances in Phenzolzine capsules. METHODS:HPLC method was adopted for content determination of main components. The contents of related substance(known impurity 1,known impurity 2,total impurity) were calculated with principle component self-control method. The determination was performed on Inertsil ODS-2 C18 column with mobile phase consisted of acetonitrile-water(55∶45,V/V)at the flow rate of 1.0 m L/min. The detection wavelength was set at 223 nm,and column temperature was 25 ℃. The sample size was 20 μL. RESULTS:The main component phenzolzine and other impurity peaks were well separated. The liner range of phenzolzine was 20.04-60.12 μg/mL(r=1.000 0). RSDs of precision,stability(24 h)and reproducibility tests were all ≤0.5%(n=6). Average recovery was 97.50%(RSD=0.36%,n=3). The detection limit and quantification limit of phenzolzine were0.91 ng and 3.04 ng. In 3 batches of samples,average value of phenzolzine,known impurity 1,known impurity 2 and total impurity were 106.68%,0.002 1%,0.044 0% and 0.046 2%,respectively. CONCLUSIONS:Established method is simple,specific,sensitive and accurate for content determination of main component and related substance in Phenzolzine capsules. It is suitable for quality control of Phenzolzine capsules.
作者
张英华
高佳
陈人萍
刘卫
王清
张炜煜
ZHANG Yinghua;GAO Jia;CHEN Renping;LIU Wei;WANG Qing;ZHANG Weiyu(School of Pharmaceutical Sciences,Changchun University of TCM,Changchun 130117,China;Basic Institute of TCM,Jilin Provincial Academy of TCM,Changchun 130012,China)
出处
《中国药房》
CAS
北大核心
2019年第19期2613-2617,共5页
China Pharmacy
基金
国家科技重大专项重大新药创制项目(No.2011-ZX09102-003-03)
吉林省科技发展计划项目(No.20170201003YY)
