反相高效液相色谱法测定阿德福韦酯及其降解产物

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Inertsil CN-3化学键合硅胶为固定相,以乙腈-25 mmol/L磷酸盐缓冲液(pH 4.0)(体积比为33∶67)为流动相,流速1.0 mL/min,检测波长260 nm。阿德福韦酯、阿德福韦的质量浓度分别为1.861~181.7 mg/L和2.018~197.2 mg/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%~10

Determination of Adefovir Dipivoxil and Its Degradation Products by Reversed-Phase High Performance Liquid Chromatography

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 = 0.9999 and 0.9998) 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.