OBJECTIVE: The objective of this study is to establish a micellar electrokinetic chromatography (MEKC) method for simultaneous separation and determination of seven biphenyl cyclooctene lignans (Gomisin D, E, G, H, J, N, and O) in Schisandra chinensis and its preparations.
METHODS: The method was optimized by studying the effects of the main parameters on the separation. The method has been validated and successfully applied to the determination of seven Gomisins in S. chinensis and its preparations.
RESULTS: In the separation system, the running buffer was composed of 20 mM Na2HPO4, 8.0 mM sodium dodecyl sulfate (SDS), 11% (v/v) methanol, and 6.0% (v/v) ethanol. A diode array detector was used with a detection wavelength of 230 nm, a separation voltage of 17 kV, and an operating temperature of 25°C. Under this condition, the seven analytes were separated at baseline within 20 min, and a good linear relationship was obtained with correlation coefficient ranging from 0.9919 to 0.9992. The limit of detection (LOD, S/N = 3) and the limit of quantification (LOQ, S/N = 10) ranged from 0.8 to 0.9 μg/mL and from 2.6 to 3.0 μg/mL, respectively. The recovery rate was between 99.1% and 102.5%.
CONCLUSIONS: The experimental results indicated that this method is suitable for the separation and determination of seven Schisandra biphenyl cyclooctene lignan compounds in real samples. At the same time, it provides an effective reference for the quality control of S. chinensis and its preparations.
目的:本研究的目的是建立胶束电动色谱(MEKC)方法,用于同时分离和测定7种联苯环辛烯木脂素(GomisinD,E,G,H,J,N,和O)在五味子及其制剂中。
方法:通过研究主要参数对分离的影响,对方法进行了优化。该方法已经过验证,并成功地应用于五味子及其制剂中7种Gomisin的测定。
结果:在分离系统中,运行缓冲液由20mMNa2HPO4、8.0mM十二烷基硫酸钠(SDS)、11%(v/v)甲醇,和6.0%(v/v)乙醇。使用二极管阵列检测器,检测波长为230nm,分离电压为17kV,工作温度为25℃。在这种情况下,七种分析物在基线20分钟内分离,线性关系良好,相关系数在0.9919~0.9992之间。检测限(LOD,S/N=3)和定量限(LOQ,S/N=10)范围为0.8至0.9μg/mL和2.6至3.0μg/mL,分别。回收率在99.1%~102.5%之间。
结论:实验结果表明,该方法适用于实际样品中7种五味子联苯环辛烯木脂素类化合物的分离和测定。同时,为五味子及其制剂的质量控制提供了有效参考。