微乳液相色谱法对吴茱萸中辛弗林、吴茱萸碱与吴茱萸次碱含量的测定

摘要

构建了一种新的微乳体系,用于微乳液相色潜同时分析吴茱萸药材中的辛弗林、吴茱萸碱和吴茱萸次碱.用甲醇超声提取方法制备样品,通过对表面活性剂种类及浓度、酸度、添加剂等影响因素进行考察,得到最佳微乳体系的组成为:3.0%SDS-6.0%正丁醇-0.6%正辛烷-1.0%甲酸-1.2%乙腈-88.2%水.选择Diamonsil C18(250 mm×4.6 mm,5 μm)色谱柱;流速0.7 mL·min-1;检测波长260nm.结果显示,在优化条件下,辛弗林、吴茱萸碱和吴茱萸次碱的线性范围分别为5.21～26.05、7.04～35.2、1.31～6.55 mg/L,相关系数r≥0.999 7,平均回收率为96%～101%,相对标准偏差(n=6)为1.0%～1.5%,检出限为0.048～0.095 mg/L.方法准确,简单易行,可用于吴茱萸药材中3种有效成分的含量分析.%An analytical method based on microemulsion liquid chromatography ( MELC ) was devel-oped for the simultaneous determination of synephrine, evodiamine and rutecarpine in Fructus Evodiae. The samples were prepared by methanol sonication. The main factors influencing the separation selectivity, including the types and concentrations of surfactant, pH values of mobile phase and the types of organic solvent additive, were investigated. The best composition of the microemulsion system was 3.0％ SDS - 6. 0％ n-butanol - 0. 6％ n-octane - 1.0％ formic acid - 1.2％ acetonitrile 88.2％ water. Three target compounds were separated with Diamonsil C18 column ( 250 mm × 4. 6 mm, 5 tμm) at a flow rate of 0. 7 ml/min. The detection wavelength was set at 260 nm. Under the optimal conditions, the calibration curves of synephrine, evodiamine and rutecarpine were linear in the range of 5.21 - 26. 05, 7.04 - 35.2, 1.31 - 6. 55 mg/L, respectively, with their correlation coefficients more than 0. 999 7. The average recoveries of three components were between 96％ and 101％ with RSD( n = 6 ) of 1.0％ - 1.5％. The limits of detection ranged from 0. 048 to 0. 095 mg/L. This method was simple, accurate and reliable, and could be applied in the determination of three components in Fructus Evodiae.