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目的建立反相高效液相色谱法测定依达拉奉原料药的含量及其有关物质。方法采用Hy-persil ODS C18色谱柱(150 mm×4.6 mm,5μm),柱温35℃,以50 mmol.L-1磷酸二氢钾(100 mL加三乙胺0.2 mL,用磷酸调pH值至3.0)-甲醇(体积比52∶48)为流动相等度洗脱,流速1.0 mL.min-1,检测波长243 nm。有关物质采用梯度洗脱,主成分自身对照法检查。结果含量测定色谱条件下,依达拉奉质量浓度在15～90 mg.L-1内与峰面积呈良好的线性关系(r=0.999 7,n=6),重复性好(RSD=0.2%),平均回收率为99.9%,RSD为0.2%(n=9),检测限(S/N=3)为22μg.L-1;经测定3批原料药的含量质量分数分别为100.0%、99.9%和100.3%,有关物质含量均低于限度(0.5%)。结论本法专属性强、准确、灵敏,能满足依达拉奉原料药的质量控制要求。
Objective To establish an RP-HPLC method for the determination of edaravone and its related substances. Methods Hy-persil ODS C18 column (150 mm × 4.6 mm, 5 μm) was used. The column temperature was 35 ℃, and 50 mmol·L-1 potassium dihydrogen phosphate (100 mL) plus 0.2 mL triethylamine To 3.0) -methanol (52:48 by volume) as the mobile phase. The flow rate was 1.0 mL.min-1 and the detection wavelength was 243 nm. Gradient-related substances were eluted, the main components of self-control test. Results The content of edaravone showed good linearity (r = 0.999 7, n = 6) and good reproducibility (RSD = 0.2%) in the range of 15-90 mg.L- ), The average recovery was 99.9%, the RSD was 0.2% (n = 9) and the limit of detection (S / N = 3) was 22μg.L-1. The mass fractions of three batches of raw drug were 100.0% 99.9% and 100.3%, the relevant substances are below the limit (0.5%). Conclusion This method is specific, accurate and sensitive and can meet the quality control requirements of edaravone.