[关键词]
[摘要]
目的 建立高效液相色谱法(HPLC)-二极管阵列检测器(DAD)法测定2-氨基吡啶原料药中的有关物质。方法 使用Waters XBridge C18色谱柱(250mm×4.6mm,5μm),流动相为10mmol/L磷酸氢二钾(磷酸调pH值至7.5)–甲醇,梯度洗脱;检测波长为225 nm(2,4-二氨基吡啶、2,6-二氨基吡啶)、260 nm(4-氨基吡啶);体积流量1.0mL/min;柱温为35℃;进样量:10μL。结果 4-氨基吡啶、2,4-二氨基吡啶、2,6-二氨基吡啶在0.01~2.00、0.01~2.00、0.06~2.00μg/mL线性关系良好。4-氨基吡啶、2,4-二氨基吡啶、2,6-二氨基吡啶的平均回收率分别为99.6%、97.5%、102.7%,RSD值分别为4.6%、2.6%、3.5%。结论 建立的方法操作简便、准确、灵敏度高、专属性强,可用于2-氨基吡啶原料药的质量控制。
[Key word]
[Abstract]
Objective To establish an HPLC-DAD method for the determination of related substances in 2-aminopyridine active pharmaceutical ingredients. Methods The analysis was performed on an Waters XBridge C18 column (250 mm×4.6 mm, 5 μm). The mobile phase was 10 mmol/L dipotassium phosphate (pH value was adjusted to 7.5 with phosphoric acid) - methanol with gradient elution. The detection wavelength was 225 nm (2,4-diaminopyridine and 2,6-diaminopyridine) and 260 nm (4- aminopyridine), the flow rate was 1.0 mL/min, column temperature was 35 ℃, and injection volume was 10 μL. Results The calibration curves of 4-aminopyridine, 2,4-diaminopyridine, and 2,6-diaminopyridine were linear within the concentration ranges of 0.01 — 2.00, 0.01 — 2.00, and 0.06 — 2.00 μg/mL, respectively. The average recoveries for 4-aminopyridine, 2,4-diaminopyridine, and 2,6-diaminopyridine were 99.6%, 97.5%, and 102.7% with RSD values of 4.6%, 2.6%, and 3.5%, respectively. Conclusion The method is simple, accurate, sensitive, and specific, and can be used for the quality control for 2-aminopyridine active pharmaceutical ingredients.
[中图分类号]
R927.2
[基金项目]
淮安市科技项目(HAP201901)