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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20μl。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 1μg·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60.71~121.41μg·ml-1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 a method for the determination of related substances and contents of oxiracetam raw materials and their injections by high performance liquid chromatography. Methods: The column was Agilent Eclipse XDB C18 (250 mm × 4.6 mm, 5 μm). The related substances were determined by using 0.01 mol·L-1 potassium dihydrogen phosphate solution (adjusted to pH 2.5 with phosphoric acid) as mobile phase A, mobile phase A- Acetonitrile (50:50) was used as mobile phase B gradient elution method. The mobile phase A was eluted by isocratic elution. The detection wavelength was 214 nm, the flow rate was 0.5 ml · min-1, the column temperature was 30 ℃, Injection volume of 20μl. Results: The main peak and the adjacent impurity peak were completely separated. The impurity A concentration showed a good linear relationship with the peak area in the range of 0.734 0 ~ 9.787 1 μg · ml-1, r = 0.999 0 with an average recovery of 95.6% (RSD = 1.5%, n = 9). The oxiracetam showed a good linear relationship with the peak area in the range of 60.71 ~ 121.41μg · ml-1, r = 0.999 9 and the average recovery was 100.0% (RSD = 0.6% 9). Conclusion: This method is highly specific, can detect more impurities, high accuracy, effective control of raw materials and injection oxiracetam related substances and content.