摘要
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。
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 ram, 5μm） 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 e- vaporator 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 recover- ies 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^-11l. 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 triethano- lamine ointment.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2012年第16期1942-1945,共4页
Chinese Journal of New Drugs
