高效液相色谱-蒸发光散射检测法测定三乙醇胺乳膏的含量

目的:建立高效液相色谱-蒸发光散射检测法(high performance liquid chromatography-evaporative light-scatting detector,HPLC-ELSD)测定三乙醇胺乳膏含量的方法。方法:采用Lichrospher CN色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-水(含0.1%甲酸)(70∶30),流速1.0 mL·min-1;蒸发光散射检测器参数:漂移管温度为50℃,雾化室温度为70℃,载气流速为1.2 L·min-1。结果:三乙醇胺的色谱峰与辅料峰能够较好的分离,三乙醇胺峰理论塔板数均>2000;软膏80%,100%和120%3个浓度水平加样回收率分别为99.83%(RSD=0.8%,n=3),100.07%(RSD=1.19%,n=3)和98.97%(RSD=1.81%,n=3);三乙醇胺的线性方程为:y=1.404 7x+2.311 6(r=0.999 5),浓度范围25～300 mg·L-1,线性关系良好;三乙醇胺的检测限为2 mg·L-1。结论:本法简便、快速、结果准确、可靠、重现性好,可用于三乙醇胺乳剂含量测定,能够对药品质量进行控制。

Determination of triethanolamine in cream by HPLC-ELSD

Objective: To establish a method to determine the content of triethanolamine in cream by HPLC-ELSD.Methods: The separation was carried out on a Lichrospher CN column(250 mm×4.6 mm,5 μm) with ELSD detector.The mobile phase was acetonitrile-water(70∶30) containing 0.1% methanoic acid,and the flow rate was 1.0 mL·min-1.The conditions of evaporative light-scatting detector(ELSD) were as follows: the evaporator temperature was 50 ℃,the nebulizer temperature was 70 ℃,and the flow rate of gas was 1.2 L·min-1.Results: Good resolution was achieved between the peak of triethanolamine and the related impurities.The recoveries of samples added with 80%,100% and 120% were 99.83%(RSD=0.8%,n=3),100.07%(RSD=1.19%,n=3) and 98.97%(RSD=1.81%,n=3),respectively.A good linearity was obtained in the range of 25~300 mg·L-1 with a correlation coefficient of 0.999 5(y=1.404 7x+2.311 6),and the detection limit was 2 mg·L-1.Conclusion: This HPLC-ELSD method for determining content of triethanolamine ointment is simple,rapid and reproducible with high recovery.It is feasible to assay and determinate the content uniformity of triethanolamine ointment.