摘要
建立了一快速、简单地测定阿德福韦酯及其降解产物阿德福韦单特戊酸甲基酯、阿德福韦的反相高效液相色谱方法。以InertsilCN 3化学键合硅胶为固定相,以乙腈 25mmol/L磷酸盐缓冲液(pH4 0)(体积比为33∶67)为流动相,流速1 0mL/min,检测波长260nm。阿德福韦酯、阿德福韦的质量浓度分别为1 861～181 7mg/L和2 018～197 2mg/L时与峰面积呈良好的线性关系(r分别为0 9999和0 9998);阿德福韦酯及阿德福韦平均加样回收率分别为99 5%～101 0%和99 1%～99 6%,相对标准偏差(RSD)均低于1 0%,阿德福韦的最小检测量(以信噪比为3计)为1ng。该方法能同时测定阿德福韦酯及其降解产物,可用于阿德福韦酯降解产物的检测。
A rapid and simple reversed-phase high performance liquid chromatographic (HPLC) method has been developed and validated for the routine analysis of adefovir dipivoxil and its degradation products (adefovir and mono-POM PMEA). The influences of pH, concentrations of buffer and acetonitrile to the retention of adefovir dipivoxil and its related substances have been investigated. The separation between adefovir dipivoxil and its degradation products was performed on a CN-3 column and the quantitation was achieved with UV detection at 260 nm. A mixture of acetonitrile and 25 (mmol/L) phosphate buffer (to adjust the pH to 4.0 with phosphoric acid) (33∶67, v/v) was used as the mobile phase for isocratic elution with a flow rate of 1.0 mL/min. This method demonstrated the baseline separation of the three analytes free of interference within 8 min. The calibration curves were linear (r=(0.999 9) and (0.999 8)) in the concentration range of 1.861-181.7 (mg/L) and 2.018-197.2 (mg/L) of adefovir dipivoxil and adefovir respectively. The average recoveries of adefovir dipivoxil and adefovir were 99.5%-101.0% and 99.1%-99.6% respectively, and the relative standard deviation was less than 1.0%. The minimum detectable quantity of adefovir was 1 ng (S/N=3). The method is simple, reproducible and can be applied to the determination of adefovir dipivoxil and its degradation products simultaneously.
出处
《色谱》
CAS
CSCD
北大核心
2004年第3期248-251,共4页
Chinese Journal of Chromatography
关键词
高效液相色谱法
阿德福韦酯
降解产物
high performance liquid chromatography
adefovir dipivoxil
degradation products
