加校正因子的主成分自身对照法测定复方依折麦布瑞舒伐他汀钙片的有关物质

发布时间：2018-10-24 21:54

【摘要】：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。
[Abstract]:Objective to establish a method for the simultaneous determination of the related substances of ezeimebuterol (EZT) and resuvastatin calcium (ROS) in ezebrisuvastatin calcium compound tablets (105 mg). Methods Reversed-phase high performance liquid chromatography was used. The chromatographic column was Kromasil 100-5 C18Dimensions column (4.6 mm 脳 150 mm,5 渭 m), 0.05 mol L-1 (p H 4.0) -acetonitrile-methanol (60:30:10) as mobile phase, and 0.05 mol L-1 potassium dihydrogen phosphate (p H 4.0, acetonitrile-tetrahydrofuran (40:50:10) as mobile phase for gradient elution. The flow rate was 1.0 mL min-1,. The detection wavelength was 242 nm,. The injection rate was 20 渭 L. The linear equation for the determination of EZT,ROS and ROS impurity 1H Ros impurity 2EZT impurity 4EZT impurity 5EZT impurity 6EZT impurity 7 is obtained. The correction factor of impurity relative to EZT or ROS is calculated by slope, and the position of impurity is determined by relative retention time. Results the relative retention time (relative to ROS) of ROS impurity 1, Ros impurity 2, Ros impurity 3, Ros impurity 4 EZT impurity 2EZT impurity 5EZT impurity 6 EZT impurity 7 was 1.51.92.11.11.72.5n 2.92.92.93.00.The correction factor was 1.1cu 1.1a 1.01.01.01.01.31.31.4kg 1.0.3. the relative retention time of ROS 4 in the batch samples was 1.31.40.0.0.3. The total impurity is 0.270.270.27 and 0.26. Conclusion the method is simple, rapid and accurate for the determination of the related substances in ezebrisulfastatin calcium compound tablets.
【作者单位】：南京优科生物医药有限公司;
【分类号】：R927;O657.72

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