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.
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)
出处
《食品与药品》
CAS
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)。
关键词
N
N-二异丙基乙胺
二异丙胺
有关物质
气相色谱法
N,N-diisopropylethylamine(DIPEA)
diisopropylamine
related substance
gas chromatography(GC)
作者简介
廉贞霞,硕士,工程师,从事药物分析工作,E-mail:mslzx1688@126.com;通讯作者:杨海霞,硕士,工程技术应用研究员,从事药物分析工作,Tel:0531-81213065,E-mail:hxyangxu@163.com。
