氯化胆碱中N,N-二甲基乙醇胺的测定方法  

An Assay Method of N,N-dimethyl Ethanolamine in Choline Chloride

作　　者：周洁 高衎 李春刚 唐祁匀 Zhou Jie;Gao Kan;Li Chun-gang;Tang Qi-yun(Shanghai Shyndec Pharmceutical(Haimen)Co.,Ltd.,Nantong 226100,China)

机构地区：[1]上海现代制药海门有限公司

出　　处：《化工管理》2020年第4期45-46,57,共3页Chemical Engineering Management

摘　　要：目的:建立一种测定氯化胆碱中N,N-二甲基乙醇胺的测定方法。方法:以6%氰丙基苯基-94%二甲基硅氧烷为固定液的毛细管柱为色谱柱;FID检测器,检测器温度为250℃;进样口温度230℃,分流比1:1;载体为氮气,流速5mL·min-1;柱温程序初始温度40℃,保持5分钟后,以20℃每分钟的升温速率上升到230℃,并维持2.5分钟。顶空条件:加热箱温度为100℃;定量环温度为105℃;传输线温度为120℃;GC循环时间为25min;样品平衡时间为20min;进样体积为1.0mL。结果:方法专属、灵敏;在50~150μg·mL-1范围内,N,N-二甲基乙醇胺线性关系良好,线性方程为y=1.6914x-62.3380,线性回归系数r=0.9991;同一均质供试品平行测定6份,结果间的RSD<1.5%,方法重复性良好;加样回收率结果均介于98%~102%,方法准确度良好。结论:该方法适用于氯化胆碱中N,N-二甲基乙醇胺的测定。Objective To establish an assay method of N,N-dimethyl ethanolamine in Choline chloride.Methods The capillary column with 6%cyanopropyl phenyl-94%dimethylsiloxane as stationary solution is used.FID detector temperature:250℃;Inlet temperature:230℃;Split ratio 1:1;Carrier gas:N2;Flow rate:5ml·min-1;Column temperature program:initial temperature 40℃hold for 5 minutes,heat up to 230℃at a rate of 20℃·min-1,and hold for 2.5 minutes.Top air condition:heating box temperature is 100℃;Quantitative ring temperature is 105℃;Transmission line temperature is 120℃;GC cycle time is 25min.The sample balance time is 20min.The injection volume is 1.0ml.Results The specificity is good and the linearity is acceptable.Perform the linear regression equation in the range of 50~150μg·ml-1,Linear equation:y=1.6914x-62.3380,correlation coefficient r=0.9991.The RSD of the same homogenous sample is less than 1.5%,so the method has good precision.All the results of recovery are in the range of 98%~102%,so the method is accurate.Conclusion This method is suitable for testing N,N-dimethyl ethanolamine in Choline chloride.

关 键 词：N N-二甲基乙醇胺 气相色谱法 氯化胆碱 

分 类 号：R927[医药卫生—药学] O657[理学—分析化学]