摘要
目的:建立氨苄西林原料药中有机溶剂残留量的测定方法,测定乙醇、丙酮、异丙醇、二氯甲烷、三乙胺的残留量。方法:采用顶空毛细管气相色谱法,色谱柱为DB-624(长度30.0 m×内径0.53 mm,膜厚3.0μm),载气为高纯氮气,进样口、FID检测器温度分别为220℃与250℃;柱温为程序升温:起始温度为50℃保持3 min,以每分钟10℃的速率升温至200℃,保持8 min;顶空进样条件,溶剂为二甲基亚砜。结果:5种有机溶剂色谱峰分离度良好,各色谱峰峰面积与浓度线性关系良好,加样回收率为98.4%~102.1%。结论:该方法准确、可靠,可用于氨苄西林原料药中有机溶剂残留量的质量控制。
Objective:To establish a method for the determination of residual organic solvents in ampicillin,including ethanol,acetone,isopropanol,dichloromethane,triethylamine.Methods:The residual organic solvents in ampicillin were separated by DB-624 capillary column(30.0 m×0.53 mm,3.0μm).The carried gas was high-purity nitrogen,and the temperature of injection and flame ionization detector temperature were controlled at 220℃and 250℃,respectively.The column temperature was maintained at 50℃for 3 minutes,then raised at a rate of 10℃per minutes to 200℃and maintained 8 minutes.The samples were dissolved in dimethyl sulfoxide.Results:The measure five organic solvents were separated completely.There was a good linear relationship between peak area and concentration.The recoveries ranged from 98.4%to 102.1%.Conclusion:The eatablished method is accurate and reliable,and can be used for the quality control of in ampicillin.
作者
王琪
黄霖
WANG Qi;HUANG Lin(Jingdezhen Market and Quality Supervision and Management Comprehension,Jingdezhen Jiangxi 333000,China)
出处
《药品评价》
CAS
2021年第18期1105-1107,共3页
Drug Evaluation
关键词
氨苄西林
气相色谱法
有机溶剂
残留量
Ampicillin
Headspace capillary gas chromatography
Organic solvents
Residual
作者简介
王琪,本科,药师。研究方向:药品检验。E-mail:23418528@qq.com。
