气相色谱法测定N,N-二异丙基乙胺中的有关物质  

Determination of Related Substances in N,N-Diisopropylethylamine by Gas Chromatography

作　　者：廉贞霞 李霞 姜鹰雁 杨帅 刘延新 杨海霞 LIAN Zhen-xia;LI Xia;JIANG Ying-yan;YANG Shuai;LIU Yan-xin;YANG Hai-xia(Shandong Provincial Key Laboratory of Biopharmaceuticals,Shandong Academy of Pharmaceutical Sciences,Jinan 250101,China;Shandong Provincial Key Laboratory of Mucosal and Transdermal Drug Delivery Technology,Shandong Freda Pharmaceutical Group Co.,Ltd.,Jinan 250101,China)

机构地区：[1]山东省药学科学院山东省生物药物重点实验室,山东济南250101 [2]山东福瑞达医药集团有限公司山东省黏膜与皮肤给药技术重点实验室,山东济南250101

出　　处：《食品与药品》2023年第6期520-523,共4页Food and Drug

基　　金：医药绿色智能制造与新药评价关键技术研究(编号:2021ZDSYS07)。

摘　　要：目的 建立气相色谱法测定N, N-二异丙基乙胺(DIPEA)中有关物质的方法。方法 采用气相色谱法,色谱柱为DB-624毛细管柱(30 m×0.53 mm,3.0μm),载气为氮气,流速为2.2 ml/min,进样口温度为210℃,FID检测器,检测器温度为250℃,程序升温:起始温度为50℃,维持5 min,再以每分钟20℃的速率升温至200℃,维持3 min。结果 已知杂质二异丙胺与其他各杂质的分离度良好,线性关系良好,线性相关系数大于0.999,平均回收率在90%~110%范围内,检出限为0.44μg/ml,定量限为0.74μg/ml。结论 该方法灵敏度高,准确度好,适用于DIPEA中有关物质的测定。Objective To establish a method for the determination of related substances in N,N-diisopropylethylamine(DIPEA)by gas chromatography(GC).Methods A DB-624 capillary column(30 m×0.53 mm,3.0μm)was adopted for GC determination,using nitrogen at a flow rate of 2.2 ml/min as carrier gas.The inlet temperature was 210℃,and the FID detector temperature was 250℃.The temperature of the column was programmed as follows:the initial temperature was 50℃,after maintenance for 5 min,the temperature of the column was raised to 200℃at the rate of 20℃per minute,then was maintained for 3 min.Results The resolution of diisopropylamine and other impurities was good.The linear correlation coefficient was greater than 0.999,the average recoveries were in the range of 90%-110%,the detection limit was 0.44µg/ml and the quantitative limit was 0.74µg/ml.Conclusion The method has high sensitivity and good accuracy,and is suitable for the determination of related substances in DIPEA.

关 键 词：N N-二异丙基乙胺 二异丙胺 有关物质 气相色谱法 

分 类 号：R917[医药卫生—药物分析学]