Wang Jiajing, Chen Yi, Lin Mei, Fan Guorong, Zhao Weiquan, Wu Yutian, Yan Chao, Wang Jianmin
Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai, PR China.
J Sep Sci. 2007 Feb;30(3):381-90. doi: 10.1002/jssc.200600332.
A pressurized CEC (pCEC) method with postcolumn detection cell had been developed for quantifying the lignans from Fructus schisandrae extracts. The effects of different experimental conditions, such as the ACN content of the mobile phase, the concentration and pH of the buffer, the applied voltage, and the supplementary pressure were studied. Five lignans (schisandrin, gomisin A, schisantherin C, deoxyschizandrin, schisandrin B) were baseline separated using a mobile phase of ACN-phosphate buffer (pH 5.4; 5 mM) (40:60 v/v) under -4 kV applied voltage. The method showed the satisfactory retention time and peak area repeatability. The calibration curves were linear in the range 50.0-1000.0 microg/mL for schisandrin, 20.0-500.0 microg/mL for gomisin A, 10.0-200.0 microg/mL for schisantherin C, 20.0-500.0 microg/mL for deoxyschizandrin, and 20.0-500.0 microg/mL for schisandrin B. The correlation coefficients were between 0.9978 and 0.9989. With this pCEC system, fingerprints of F. schisandrae were preliminarily established to distinguish two members S. chinensis (Turcz.) Baill. and S. sphenanthera Rehd. Et Wils. of F. schisandrae by characteristic peaks, and evaluate the quality of various sources of raw materials by determining the contents of the five lignans.
已开发出一种带有柱后检测池的加压毛细管电色谱(pCEC)方法,用于定量分析五味子提取物中的木脂素。研究了不同实验条件的影响,如流动相中的乙腈含量、缓冲液的浓度和pH值、施加电压以及补充压力。在-4 kV的施加电压下,使用乙腈 - 磷酸盐缓冲液(pH 5.4;5 mM)(40:60 v/v)的流动相,可对五种木脂素(五味子醇甲、戈米辛A、华中五味子酯C、脱氧五味子素、五味子醇乙)进行基线分离。该方法显示出令人满意的保留时间和峰面积重复性。五味子醇甲的校准曲线在50.0 - 1000.0 μg/mL范围内呈线性,戈米辛A在20.0 - 500.0 μg/mL范围内,华中五味子酯C在10.0 -
200.0 μg/mL范围内,脱氧五味子素在20.0 - 500.0 μg/mL范围内,五味子醇乙在20.0 - 500.0 μg/mL范围内。相关系数在0.9978至0.9989之间。利用该pCEC系统,初步建立了五味子的指纹图谱,通过特征峰区分五味子科的两个成员中华五味子(Schisandra chinensis (Turcz.) Baill.)和华中五味子(Schisandra sphenanthera Rehd. Et Wils.),并通过测定五种木脂素的含量来评估各种来源原料的质量。