论文部分内容阅读
目的采用加校正因子的主成分自身对照法测定培哚普利片中有关物质的含量。方法采用GL Inertsil C8-3色谱柱(4.0 mm×150 mm,5μm),以流动相A(用50%高氯酸调节pH至2.5的水溶液)和流动相B(0.03%的高氯酸乙腈溶液)进行梯度洗脱,流速为1.0 mL·min~(-1),检测波长为215 nm,进样量为20μL,柱温60℃,测定培哚普利叔丁胺和杂质B、E、F的线性方程,以斜率计算杂质相对于培哚普利叔丁胺的校正因子,用相对保留时间确定各杂质位置。并进行了方法学验证。用相对校正因子计算培哚普利片中杂质B、E和F的含量,并与杂质对照品法测得的结果进行比较。结果培哚普利杂质B、E和F的相对保留时间分别为0.68,1.14,1.61;校正因子分别为0.77,1.02,1.24;检出限分别为2.24,0.52,1.02 ng;定量限为6.73,1.57,3.06 ng;采用校正因子的主成分自身对照法和外标法测得的结果无显著性差异。结论该方法简便快速,可准确测定培哚普利片中杂质B、E和F含量。
Objective To determine the content of perindopril tablets by using the principal component self-control method with correction factor. Methods A GL Inertsil C8-3 column (4.0 mm × 150 mm, 5 μm) was used with mobile phase A (aqueous solution adjusted to pH 2.5 with 50% perchloric acid) and mobile phase B (0.03% perchloric acid in acetonitrile ) At a flow rate of 1.0 mL · min -1 with a detection wavelength of 215 nm, an injection volume of 20 μL and a column temperature of 60 ° C. The linearity of perindopril tert-butylamine with impurities B, E and F Equation, the slope is used to calculate the correction factor for impurity relative to perindopril tert-butylamine, and the relative retention time is used to determine the position of each impurity. And conducted methodological verification. The relative calibration factors were used to calculate the contents of impurities B, E and F in perindopril tablets and compared with the results of the impurity reference substance method. Results The relative retention times of perindopril impurities B, E and F were 0.68, 1.14 and 1.61, respectively. The calibration factors were 0.77, 1.02 and 1.24, respectively. The detection limits were 2.24, 0.52 and 1.02 ng, respectively. The limits of quantification were 6.73, 1.57, 3.06 ng respectively; there was no significant difference between the results of self-control method and external standard method using the principal component of correction factor. Conclusion The method is simple and rapid and can accurately determine the contents of B, E and F in perindopril tablets.