RP-HPLC法测定瑞格列奈原料药含量及其有关物质  

Determination Related Substances and Content of Repaglinide by RP-HPLC

作　　者：张婷 陈淑娴 吴司琪 彭红[3] ZHANG Ting;CHEN Shuxian;WU Siqi;PENG Hong(Pingxiang Health Vocational College,Pingxiang Jiangxi 337000,China;Xinghua Hospital of Traditional Chinese Medicine,Xinghua Jiangsu 225700,China;Jiangxi University of Traditional Chinese Medicine,Nanchang Jiangxi 330004,China.)

机构地区：[1]萍乡卫生职业学院,江西萍乡337000 [2]兴化市中医院,江苏兴化225700 [3]江西中医药大学,江西南昌330004

出　　处：《药品评价》2024年第1期36-40,共5页Drug Evaluation

摘　　要：目的通过RP-HPLC法对瑞格列奈原料药的含量和其有关物质进行分析。方法采用J&K WpHC18色谱柱(4.6 mm×250 mm,5μm),使用0.1%甲酸溶液-甲醇(32∶68)作为流动相,流速为1.0 mL/min,检测波长为243 nm,柱温为20℃,进样量为20μL。结果瑞格列奈浓度在10.06~80.72μg/mL范围内线性相关性良好(Y=0.0121X+0.0107,r=0.9997),重复性试验RSD值为1.01%(n=6),平均回收率为99.2%,检测限为4.0 ng,定量限为11.5 ng。外标法测定瑞格列奈原料药平均含量为99.6%。主峰和其他杂质峰明显区别,三个批次的瑞格列奈样品有关物质的含量分别为0.17%、0.14%和0.15%。结论RP-HPLC法操作便捷、专属性好、精密度高、结果可靠,可用于瑞格列奈原料药的检测。Objective To analyze the content of repaglinide and its related substances by RP-HPLC.Methods J&K WpHC18 column(4.6 mm×250 mm,5μm)was used with 0.1%formic acid solution-methanol(32∶68)as mobile phase,flow rate was 1.0 mL/min,detection wavelength was 243 nm,column temperature was 20℃,and sample size was 20μL.Results The linear correlation of repaglinide was good in the range of 10.06-80.72μg/mL(Y=0.0121X+0.0107,r=0.9997),RSD of repeatability test was 1.01%(n=6),recovery was 99.2%,detection limit was 4.0 ng,and quantitation limit was 11.5 ng.The average content of repaglinide by external standard method was 99.6%.The main peak and other impurity peaks were obviously different.The content of related substances in three batches of repaglinide samples were 0.17%,0.14%and 0.15%,respectively.Conclusion RP-HPLC method is convenient,specific,highly precise and reliable,and can be used for the determination of repaglinide.

关 键 词：瑞格列奈原料药 HPLC法 含量 有关物质 

分 类 号：R927.2[医药卫生—药学]