离子对色谱法检测阿德福韦酯中降解产物的含量  

Determination of degradation products of adefovir dipivoxil by ion-pair HPLC

作　　者：李小兵 王勇军 蒋飞英 朱峰 毛白杨 陈再新 

机构地区：[1]江苏亚邦药业集团技术中心,常州213200

出　　处：《药物分析杂志》2013年第6期1007-1011,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立阿德福韦酯主要的降解产物阿德福韦单特戊酸甲酯、阿德福韦及其他杂质的检测方法。方法:采用WelchMaterials XB-C8柱(250 mm×4.6 mm,5μm),以0.05 mol.L-1的磷酸氢二钾和0.01 mol.L-1四丁基硫酸氢铵缓冲溶液(磷酸调pH至3.0)-乙腈(65∶35)为流动相,检测波长为260 nm,流速为1.0 mL.min-1。结果:阿德福韦酯主峰与临近杂质峰可达到基线分离,主要降解产物阿德福韦、阿德福韦单特戊酸甲酯及9-(2-二乙氧基膦酰甲氧基乙基)腺嘌呤分离度均在2.0以上。阿德福韦、阿德福韦单特戊酸甲酯及阿德福韦酯分别在0.109～21.8μg.mL-1、0.111～22.2μg.mL-1、0.105～21.0μg.mL-1的浓度范围内呈良好的线性;阿德福韦和阿德福韦单特戊酸甲酯的回收率分别为98.8%、99.7%。结论:该方法简便,准确,专属性好,可适用于阿德福韦酯的有关物质检查及质量控制。Objective：To establish a method for the determination of main degradation products including mono - POM PMEA, adefovir and other impurities in adefovir dipivoxil. Methods：The Welch Materials XB - C8 column （250 mm×4.6 mm,5μm） was adopted with the mobile phase consisting of buffer solution - acetonitrile （65： 35）, the buffer solution contained 50 mol·L^-1 potassium phosphate dibasic and 10mol·L^-1 tetrabutylammonium hydrogen sulfate, and was adjusted to pH 3.0 with phosphate acid. The detection wavelength was 260 nm, and the flow rate was 1.0mL·min^-1. Results： The baseline separation was achieved between the main peak of adefovir dipivoxil and the near peak of impurities, and the resolutions among the main degradation products （ i. e. , adefovir, mono - POM PMEA and 9 - [ 2 - （ diethyl - phosphonomethoxy） ethyl ] adenine） were above 2. 0. The good linearity was obtained over the range of 0. 109-21.8 μg·mL^-1 for adefovir,0. 111 -22.2 μg·mL^-1 for mono -POM PMEA,and 0. 105 -21.0 μg·mL^-1 for adefovir dipivoxil. The average recoveries were 98.8% for adefovir and 99.7 % for mono - POM PMEA, respectively. Conclusion： This method is simple, accurate, with well specificity, and can be applied to determination of the relative substances in adefovir dipivoxil and quality control.

关 键 词：阿德福韦酯 降解产物 阿德福韦 阿德福韦单特戊酸甲酯 离子对色谱法 

分 类 号：R917[医药卫生—药物分析学]