摘要
目的:建立顶空毛细管气相色谱法测定红古豆醇酯原料药中甲醛酯、乙醇和丙酮等残留溶剂的检测方法。方法:以DB-624为色谱柱,进样口220℃,柱载气为氮气,柱流速3. 0 m L/min,分流比10∶1,色谱柱起始40℃,保持15 min,再以40℃/min升至200℃,保持5 min,FID检测器温度250℃。80℃顶空进样,检测红古豆醇酯原料药中甲醛酯、乙醇和丙酮溶剂残留。结果:甲醛酯、乙醇和丙酮得到了良好分离,线性关系、精密度、准确度、耐用性符合标准要求,检测4批红古豆醇酯原料药有机残留均达到了《中国药典》2015版中残留溶剂限量规定的测定要求。结论:建立的方法能快速准确地检测3种有机溶剂,并可用于药物质量控制中的有机残留溶剂检查。
Objectives:To establish a GC method for the determination of three residue organic solvent(Formaldehyde ester,ethanol,acetone)in Cuscohygrinolisα-Acetylbenzoacetate.Methods:DB-624 was used as chromatographic column,the inlet was 220℃,the carrier gas was nitrogen,the flow rate was 3.0 mL/min,the split ratio was 10:1,the column was kept at 40℃for 15 minutes,then at 40℃/min to 200℃,the temperature of FID detector was 250℃.The method of injection was headspace,the temperature of headspace injection was 80℃.The residual formaldehyde ester,ethanol and acetone solvents in actie pharmaceutical ingredient of Cuscohygrinolisα-Acetylbenzoacetate were determined.Results:Formaldehyde ester,ethanol and acetone were well separated.The linear relationship,precision,accuracy and durability met the requirements of the standard.The organic residues of four batches of Cuscohygrinolisα-Acetylbenzoacetate actie pharmaceutical ingredient met the requirements of the limit of residual organic in China Pharmacopoeia 2015.Conclusions:The method can be used to detect three kinds of organic solvents quickly and accurately,and can be used for the determination of residual organic solvents in drug quality control.
作者
田金磊
罗斌
熊城
马建强
Tian Jinlei;Luo Bin;Xiong Cheng;Ma Jianqiang(Chengdu First Pharmaceutical of Active Pharmaceutical Ingredient Co.,Ltd,Chengdu,611930,China)
出处
《成都中医药大学学报》
2018年第4期17-19,共3页
Journal of Chengdu University of Traditional Chinese Medicine
基金
四川省科技支撑计划项目(2016SZ0027)
关键词
气相色谱法
有机溶剂残留
顶空进样
红古豆醇酯
Gas chromatography
Residual organic solvent
Headspace injection
Cuscohygrinolisα-acetylbenzoacetate
