摘要
目的:建立毛细管气相色谱方法测定阿德福韦酯有机溶剂残留量。方法:采用气相色谱法测定,色谱柱为 DB-624石英毛细管柱(75m×0.53 mm,3.0μm),载气为氮气。检测器温度:300℃;进样口温度:200℃;程序升温:初始温度60℃,保持8 min,以20℃·min^(-1)升温至200℃,保持8 min。顶空进样,平衡温度为80℃,平衡时间为45 min,分流比为0.5:1,N,N-二甲基甲酰胺为溶剂,正丙醇为内标物。结果:被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论:该法可用于阿德福韦酯原料药中有机溶剂残留量的检测。
Objective：To establish a method of head- space capillary gas chromatography（CGC） for the determination of residual solvents in adefovir dipivoxil. Methods：The residual solvents in adefovir dipivoxil were separated by DB-624 capillary column（75 m ×0. 53 ram,3.0 μm） with an FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature were controlled at 200 ℃ and 300 ℃, respectively. The programmed column temperature was set as follows ： maintained at 60 ℃ for 8 rain and then raised to 200 ℃ at the rate of 20 ℃ · min ^-1 followed by holding for 8 min. The sample was dissolved in N,N - dimethylformamide and n - propanol was used as the internal standard. The containers of head - space injector were in equilibrium at 80 ℃ for 45 min, the splitting - ratio was 0. 5： 1. Results： The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. Conclusion：The established method was accurate and reliable. It can be used for the determination of residual solvents in adefovir dipivoxil.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第11期1357-1359,共3页
Chinese Journal of Pharmaceutical Analysis
关键词
阿德福韦酯
残留溶剂
毛细管气相色谱
adefovir dipivoxil
residual solvent
capillary gas chromatography （ CGC ）
