摘要
建立了GC-FID法测定恩他卡朋(1)中间体中杂质二环己基碳二亚胺(DCC,4)和二环己基脲(DCU,7)的含量。采用HP-5柱(0.32 mm×30 m×0.25μm),程序升温,FID检测器温度为320℃;进样口温度为300℃,进样量为1μl,分流比为10∶1。结果表明,4和7在相应浓度范围内线性关系良好,平均回收率分别为98.75%和100.05%。以外标法计算6批样品中4和7的含量均低于0.1%。建立的方法简单、准确、重复性好,可用于1中间体中4和7的测定。
A GC-FID method was established to determine the content of dicyclohexylcarbodiimide(DCC,4)and dicyclohexylurea(DCU,7)in the intermediate of entacapone(1).HP-5 Column(0.32 mm×30 m×0.25μm)was used with programmed temperature rise,the FID detector temperature was 320℃,the injection port temperature was 300℃,the injection volume was 1μl and the split ratio was 10∶1.The results showed that it was linear for 4 and 7 in the corresponding ranges,and the average recoveries were 98.75%and 100.05%,respectively.The contents of 4 and 7 in the six batches of samples calculated by the external standard method were all lower than 0.1%.The established method is simple,accurate and reproducible,which can be used for the determination of 4 and 7 in 1 intermediates.
作者
刘进艳
庄子晗
夏春雨
李建其
周爱南
LIU Jinyan;ZHUANG Zihan;XIA Chunyu;LI Jianqi;ZHOU Ainan(College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,Shanghai 201203;Shanghai Institute of Pharmaceutical Industry,China State Institute of Pharmaceutical Industry,Shanghai 201203;Jilin Aodong Taonan Pharmaceutical Co.,Ltd.,Taonan 137100)
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2021年第7期960-963,共4页
Chinese Journal of Pharmaceuticals
