HPLC-DAD法测定2-氨基吡啶原料药中有关物质  

Determination of related substances in 2-aminopyridine active pharmaceutical ingredients by HPLC-DAD

作　　者：张绿茵 兰为环 刘朋[2] 王歆 唐海 ZHANG Lü-yin;LAN Wei-huan;LIU Peng;WANG Xin;TANG Hai(Jiangsu Tasly Diyi Pharmaceutical Co.Ltd,Huai’an 223001,China;Tasly Holding Group Co.Ltd,Tianjin 300410,China)

机构地区：[1]江苏天士力帝益药业有限公司,江苏淮安223001 [2]天士力控股集团有限公司,天津300410

出　　处：《现代药物与临床》2022年第11期2490-2494,共5页Drugs & Clinic

基　　金：淮安市科技项目(HAP201901)。

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(250 mm×4.6 mm,5μm),流动相为10 mmol/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1.0 mL/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。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 C18column(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.

关 键 词：2-氨基吡啶 4-氨基吡啶 2 4-二氨基吡啶 2 6-二氨基吡啶 有关物质 HPLC-DAD 

分 类 号：R927.2[医药卫生—药学]