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目的建立同时测定依折麦布瑞舒伐他汀钙复方片(10,5 mg)中依折麦布(EZT)和瑞舒伐他汀钙(ROS)有关物质的方法。方法采用反相高效液相色谱法。色谱柱为Kromasil 100-5 C18Dimensions柱(4.6 mm×150 mm,5μm),以0.05 mol·L-1磷酸二氢钾(p H 4.0)-乙腈-甲醇(60∶30∶10)为流动相A,以0.05 mol·L-1磷酸二氢钾(p H 4.0)-乙腈-四氢呋喃(40∶50∶10)为流动相B,进行梯度洗脱。流速为1.0 m L·min-1,检测波长为242 nm,进样量为20μL。测定EZT、ROS和ROS杂质1、ROS杂质2、ROS杂质3、EZT杂质1、EZT杂质2、EZT杂质3、EZT杂质4、EZT杂质5、EZT杂质6、EZT杂质7的线性方程,以斜率计算杂质相对于EZT或ROS的校正因子,用相对保留时间确定各杂质位置。结果 ROS杂质1、ROS杂质2、ROS杂质3、ROS杂质4、EZT杂质1、EZT杂质2、EZT杂质3、EZT杂质4、EZT杂质5、EZT杂质6、EZT杂质7的相对保留时间(相对于ROS)分别为1.5,1.9,2.1,1.1,1.7,2.5,2.6,2.8,2.9,3.0,4.0,校正因子分别为1.1,1.1,1.0,1.0,1.3,1.1,1.0,1.3,1.4,0.5,1.0。3批样品中ROS杂质4的含量均为0.15%,其他杂质均小于0.1%,总杂质分别为0.27%,0.27%,0.26%。结论方法简便快速,可准确测定依折麦布瑞舒伐他汀钙复方片中有关物质的含量。
Objective To establish a method for simultaneous determination of ezrinib (EZT) and rosuvastatin calcium (ROS) -related substances in ezetimibe and rosuvastatin calcium complex tablets (10,5 mg). Methods Using reversed-phase high performance liquid chromatography. The column was a Kromasil 100-5 C18Dimensions column (4.6 mm × 150 mm, 5 μm) with 0.05 mol·L -1 potassium phosphate monobasic (p H 4.0) -acetonitrile-methanol (60:30:10) as mobile phase A The mobile phase B was eluted with 0.05 mol·L-1 potassium phosphate monobasic (p H 4.0) -acetonitrile-tetrahydrofuran (40:50:10). The flow rate was 1.0 m L · min-1, the detection wavelength was 242 nm and the injection volume was 20 μL. The linear equations for EZT, ROS and ROS impurities 1, ROS impurity 2, ROS impurity 3, EZT impurity 1, EZT impurity 2, EZT impurity 3, EZT impurity 4, EZT impurity 5, EZT impurity 6, and EZT impurity 7 were measured with a slope Calculate the correction factor for impurities relative to EZT or ROS and use relative retention time to determine each impurity location. Results The relative retention time of ROS impurity 1, ROS impurity 2, ROS impurity 3, ROS impurity 4, EZT impurity 1, EZT impurity 2, EZT impurity 3, EZT impurity 4, EZT impurity 5, EZT impurity 6, EZT impurity 7 At ROS) were 1.5,1.9,2.1,1.1,1.7,2.5,2.6,2.8,2.9,3.0,4.0, the correction factors were 1.1,1.1,1.0,1.0,1.3,1.1,1.0,1.3,1.4,0.5 In 1.0.3 batches of samples, the content of ROS impurity 4 was 0.15%, the other impurities were less than 0.1%, the total impurities were 0.27%, 0.27% and 0.26% respectively. Conclusion The method is simple and rapid and can accurately determine the content of related substances in ezetimibe and rosuvastatin calcium compound tablets.