摘要
目的:建立毛细管气相色谱方法测定阿奇霉素中的残留溶剂。方法:采用气相色谱法测定,色谱柱为 HP-5(5%苯基~95%甲基聚硅氧烷固定液)石英毛细管柱(30.0 m×0.32 mm×0.25 μm),载气为氮气。进样口温度为200℃,FID 检测器温度为250℃,柱温为40℃;顶空进样,平衡温度为50℃,平衡时间为30 min,分流比为1:1;0.25 mol·L^(-1)硫酸溶液为溶剂;丁酮为内标物。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,精密度和回收率良好。结论:该法可用于阿奇霉素原料药中残留溶剂的检测。
Objective: To establish a method of head - space capillary gas chromatography (CGC) for the nation of residual solvents in azithromycin. Methods:The residual solvents in azithromycin were separated determiby HP - 5 capillary colunm(30. 0 m ×0. 32 mm ×0. 25 μm) with an FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature was controlled at 200 ℃ and 250 ℃, respectively. The column temperature was 40 ℃, The sample was dissolved in 0. 25 mol· L^- 1 sulfuric acid and methylethyl ketone was used as the internal standard. The containers of head - space injector were in was 1: 1. Results:The measured solvents were se good linear relationship with good precision and parated equilibrium at 50 ℃ for 30 min,the splitting - ratio completely. The calibration curve of each solvent showed a accuracy. Conclusion: The established method was accurate and reliable. It can be used for the determination of residual solvents in azithromycin.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第11期1827-1831,共5页
Chinese Journal of Pharmaceutical Analysis
关键词
阿奇霉素
残留溶剂
毛细管气相色谱
azithromycin
residual solvent
capillary gas chromatography (CGC)