顶空气相色谱法测定盐酸头孢替安酯原料药中残留溶剂含量

发布时间：2018-02-21 10:01

  本文关键词： 头孢替安酯 盐酸 色谱法 气相 顶空采样 残留溶剂　出处：《医药导报》2016年02期 　论文类型：期刊论文

【摘要】：目的建立顶空气相色谱法同时测定盐酸头孢替安酯原料药中丙酮、乙酸乙酯、异丙醇、二氯甲烷、乙腈5种残留溶剂。方法采用Agilent DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定相)石英毛细管柱(30 m×0.53 mm,3.0μm),火焰离子化检测仪(FID)检测器,N,N-二甲基甲酰胺(DMF)为溶剂。结果 5种残留溶剂在各自的浓度范围内呈现良好的线性关系(r=0.999 6~0.999 9,n=5),最低检出限范围为0.071~0.847μg;5种残留溶剂检测的稳定性RSD为0.40%~2.12%(n=3),平均加样回收率为99.03%~104.79%,RSD为0.54%~3.41%(n=3)。结论该方法简单、灵敏、可靠,适用于盐酸头孢替安酯原料药中残留溶剂的分析检测。
[Abstract]:Objective to establish a headspace gas chromatography method for the simultaneous determination of acetone, ethyl acetate, isopropanol and dichloromethane in ceftianil hydrochloride. Five residual solvents of acetonitrile were used. Methods Agilent DB-624A6% cyanopropyl phenyl 94% dimethyl polysiloxane stationary phase) quartz capillary column (30 m 脳 0.53 mm ~ (3) 渭 m) and flame ionization detector (FID) were used as solvent. There was a good linear relationship between the residual solvents in their respective concentration ranges. The lowest detection limit was 0.071 ~ 0.847 渭 g ~ (-1) 渭 g ~ (-1). The RSD was 0.40 ~ 2.12% and the average recovery was 99.03 ~ 104.79 ~ 0.54 ~ 3.41 渭 g ~ (-1) 渭 g ~ (-1). Conclusion the method is simple, and the relative standard deviation is 0.54 ~ (3.41) 渭 g ~ (-1) for the determination of residual solvents. It is sensitive, reliable and suitable for the determination of residual solvent in ceftiamil hydrochloride.
【作者单位】： 抗生素研究与再评价四川省重点实验室成都大学四川抗菌素工业研究所;成都军区总医院药剂科;
【基金】：成都大学自然科学青年基金(2080515057)
【分类号】：R927.2;O657.71
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