HPLC加校正因子的主成分自身对照法测定盐酸特拉唑嗪片中有关物质的含量

Determination of Related Substance in Terazosin Hydrochloride Tablets by HPLC and Principal Component Self-control with Correction Factor

目的:建立测定盐酸特拉唑嗪片中有关物质含量的方法。方法:采用高效液相色谱加校正因子的主成分自身对照法。色谱柱为Agilent Zorbax Eclipse XDB C18,流动相为乙腈-高氯酸溶液(20∶80,V/V),流速为1.0 mL/min,检测波长为246 nm,进样量为20μL,柱温为50℃;绘制盐酸特拉唑嗪和杂质A、B、C的线性方程,以斜率计算各杂质相对于盐酸特拉唑嗪的校正因子,用相对保留时间确定各杂质位置,测定3批盐酸特拉唑嗪片中杂质A、B、C的含量,并与杂质对照品法测得的结果进行比较。结果:盐酸特拉唑嗪杂质A、B、C的相对保留时间分别为0.39、0.74、2.77,检测质量浓度线性范围均为0.25～3.0μg/mL,校正因子分别为0.75、1.09、0.84,检测限分别为0.35、0.51、0.43 ng,定量限分别为0.70、1.02、0.86 ng。3批盐酸特拉唑嗪片中杂质A、B、C的含量分别为0.11%～0.13%、0.03%、0.09%～0.12%,杂质B未检出;与杂质对照品法测定结果一致。结论:该方法简便快速,可准确测定盐酸特拉唑嗪片中有关物质的含量。

OBJECTIVE:To establish the method for the content determination of related substance in Terazosin hydrochloride tablets.METHODS:HPLC and principal component self-control with correction factor were adopted.The determination was performed on Agilent Zorbax Eclipse XDB C18 column with mobile phase consisted of acetonitrile-perchloric acid solution(20∶80,V/V)at the flow rate of 1.0 mL/min.The detection wavelength was set at 246 nm,and sample size was 20μL.The column temperature was 50℃.The linear equations of terazosin hydrochloride,impurity A,B,C were drawn.The correction factors of each impurity related to terazosin hydrochloride were calculated by slope,and relative retention time was used to determine the position of impurities.The contents of impurity A,B and C in 3 batches of Terazosin hydrochloride tablets were determined and compared with the results of impurity control method.RESULTS:The relative retention time of impurity A,B,C was 0.39,0.74,2.77,respectively;the linear range of them were 0.25-3.0μg/mL,respectively.The correction factors were 0.75,1.09,0.84,respectively.The detection limits were 0.35,0.51,0.43 ng,and the limits of quantification were 0.70,1.02,0.86 ng,respectively.The contents of impurity A,B and C in 3 batches of Terazosin hydrochloride tablets were 0.11%-0.13%,0.03%and 0.09%-0.12%;impurity B did not detected.The results are consistent with the determination of impurity control method.CONCLUSIONS:The method is simple,rapid and accurate for the content determination of related substances A,B,C in Terazosin hydrochloride tablets.