摘要
目的：建立用高效液相色谱法测定奥拉西坦原料及其注射剂中有关物质和含量的方法.方法：色谱柱为Agilent Eclipse XDB C18（250 mm×4.6 mm,5μm）,有关物质测定采用0.01 mol·L-1磷酸二氢钾溶液（磷酸调节pH至2.5）为流动相A,流动相A-乙腈（50∶ 50）为流动相B的梯度洗脱法,含量测定采用流动相A的等度洗脱法,检测波长为214 nm,流速为0.5ml·min-1,柱温为30℃,进样量为20 μl.结果：主峰和相邻杂质峰能完全分离,杂质A浓度在0.734 0 ～9.787 1 μg·ml-1范围内与其峰面积呈良好的线性关系,r =0.999 0,平均回收率为95.6％（RSD =1.5％,n=9）;奥拉西坦在60.71 ～121.41 μg·ml-范围内与峰面积呈良好线性关系,r =0.999 9,平均回收率为100.0％（RSD =0.6％,n=9）.结论：本方法专属性强,能检出更多的杂质,准确度高,能有效质控奥拉西坦原料及注射剂中的有关物质和含量.
Objective：To establish an HPLC method for the determination of oxiracetam and its related substances in the raw material and the injections.Methods：An Agilent Eclipse XDB C18 （250 mm × 4.6 mm,5 μμm） column at the temperature of 30℃ was adopted.For the determination of related substances,the mobile phase was composed of mobile phase A （0.01 mol · L-1 potassium dihydrogen phosphate solution,adjusting pH to 2.5 with phosphoric acid） and acetonitrile （50∶ 50） with gradient elution,and the mobile phase Awith isocratic elution was used in the content determination of oxiracetam in the raw material and the injections.The flow rate was 0.5 ml · min-1,the UV detection wavelength was set at 214nm and the injection volume was 20μl.Results：The related substances were completely separated from the main component.The standard curve of impurity A was linear over the range of 0.734 0-9.787 1 μg · ml-1（r =0.999 0） with the average recovery of 95.6％ （RSD =1.5％,n =9）.The standard curve of oxiracetam was linear over the range of 60.71-1 21.41 μg · ml-1 （r =0.999 9） with the average recovery of 100.0％ （RSD =0.6％,n =9）.Conclusion：The method with high precision,accuracy,sensitivity and specificity can satisfy the requirements and can be used in the quality control of oxiracetam in the raw material and the injections.
出处
《中国药师》
CAS
2014年第7期1112-1116,共5页
China Pharmacist
