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目的建立一种快速、简便和准确的高效液相色谱法,用于测定艾拉莫德片的有关物质。方法使用Agilent HC-C18色谱柱(250 mm×4.6 mm,5μm),乙腈-50 mmol·L-1磷酸二氢钾溶液(体积分数50%磷酸溶液调节pH值至3.0)(体积比10∶90)作为流动相,流速1.0 mL·min-1,检测波长为270 nm,柱温25℃。结果方法学研究结果表明,片剂辅料对艾拉莫德有关物质的测定没有干扰;杂质1和杂质2质量浓度均在5.0~50 mg·L-1内与峰面积呈良好的线性关系(r=0.999 6和0.999 8);平均回收率分别为99.77%和99.89%,RSD分别为1.3%和1.0%(n=9)。经测定艾拉莫德片中2种主要杂质的总含量为0.107%。结论所建立的艾拉莫德片有关物质测定方法,简单可靠、准确有效,为艾拉莫德片有关物质检测提供了参考方法。
Objective To establish a rapid, simple and accurate HPLC method for the determination of related substances of ralumuide tablets. Methods The sample was separated on an Agilent HC-C18 column (250 mm × 4.6 mm, 5 μm), acetonitrile-50 mmol·L-1 potassium dihydrogen phosphate solution (50% phosphoric acid solution to adjust the pH value to 3.0) ) As the mobile phase, the flow rate was 1.0 mL · min-1, the detection wavelength was 270 nm and the column temperature was 25 ℃. Results The results of the methodological study showed that tablet adjuvant had no interference with the determination of related substances of Iramodine. The concentrations of impurity 1 and impurity 2 in the range of 5.0 ~ 50 mg · L-1 showed a good linear relationship with the peak area (r = 0.999 6 and 0.999 8). The average recoveries were 99.77% and 99.89%, respectively, with RSDs of 1.3% and 1.0%, respectively (n = 9). The total content of the two major impurities in the iguratimod was 0.107%. Conclusion The established method for the determination of ouramide tablets is simple, reliable, accurate and effective and provides a reference method for the detection of related substances of iguratimod.