MEKC-DAD同时测定大黄及其炮制品中5种蒽醌的含量___

目的: 建立胶束电动毛细管色谱二极管阵列检测法(MEKC-DAD)同时测定大黄及其炮制品中大黄素、芦荟大黄素、大黄酸、大黄酚及大黄素甲醚含量。 方法: 选择胶束电动毛细管电泳分离模式,用未涂渍标准熔融石英毛细管(75 μm×64.5 cm,有效长度56 cm)为分离通道,以25 mmol·L^–1硼砂-25mmol·L^–1 SDS-10%乙腈(pH 10.90)为背景电解质溶液,运行电压为12 kV,运行温度为24 ℃,检测波长为254 nm,压力进样为5 kPa,5 s。 结果: 大黄素、芦荟大黄素、大黄酸、大黄酚及大黄素甲醚浓度分别在2.4~47.0,2.4~48.4,2.1~41.4,1.9~37.0,3.8~75.0 μg·mL^–1范围内呈良好线性关系(r≥0.9994);加样回收率(n=5)分别为99.5%(RSD=3.7%),101.4%(RSD=2.4%),98.5%(RSD=3.8%),101.3%(RSD=3.9%),101.4%(RSD=3.1%)。 结论: 该方法简单、准确,重现性好,可用于大黄饮片内在质量的评价和控制。

Objective: To establish a method for simultaneous determination of emodin,aloe-emodin,rhein,chrysophanol and physcion in Radix et Rhizoma Rhei and its processed products by micellar electrokinetic chromatography with diode array detection(MEKC-DAD). Methods: Based on the mode of micellar electrokinetic chromatography,a uncoated fused silica capillary(64.5 cm×75 μm,an effective length of 56 cm)was adopted.25 mmol·L^-1 borax-25 mmol·L^-1 SDS-10% acetonitrile was selected for the running buffer(pH 10.90).The separation voltage was 12 kV and the capillary temperature was 24 ℃.The detection wavelength was set at 254 nm.The sample was injected at 5 kPa,5 s. Results: The regression equation for emodin,aloe-emodin,rhein,chrysophanol and physcion showed good linearity(r≥0.9994)in the ranges of 2.4-47.0,2.4-48.4,2.1-41.4,1.9-37.0,3.8-75.0 μg·mL^-1 respectively.The average recoveries(n=5)were 99.5%(RSD=3.7%),101.4%(RSD=2.4%),98.5%(RSD=3.8%),101.3%(RSD=3.9%),101.4%(RSD=3.1%),respectively. Conclusion: The method is simple,accurate and reproducible,and can be used for quality control of Radix et Rhizoma Rhei.

[1]. SONG Li-ren(宋立人),HONG Xun(洪恂),DING Xu-liang(丁绪亮),et al.A Dictionary of Modern Chinese Materia Medica(现代中药学大辞典).Beijing(北京):People’s Medical Publishing House(人民卫生出版社),2001.116
[2]. ZHANG Dan(张丹),JIANG Xin-hui(蒋心惠).Determination of aloe-emodin,rhein,emodin and chrysophanol in Radix Rhei by reversed phase high performance liquid chromatography(反相高效液相色谱法测定大黄药材中游离及结合型蒽醌类衍生物的含量).Chin J Anal Chem(分析化学),2003,31(4):459
[3]. LI Wei(李伟),CHAI Jin-ling(柴金玲),ALIMJAN Abaydulla(阿里木江·艾拜都拉),et al.Separation and determination of anthraquinone compounds in Chinese Herb Rhubarb extracts by capillary zone electrophoresis(区带毛细管电泳分离测定大黄提取液中游离蒽醌化合物).J Anal Sci(分析科学学报),2006,22(1):68
[4]. Gong YX,Li SP,Wang YT,et al.Simultaneous determination of anthraquinones in Rhubarb by pressurized liquid extraction and capillary zone electrophoresis.Electrophoresis,2005,26(9):1778
[5]. Li Y,Liu H,Ji X,et al.Optimized separation of pharmacologically active anthraquinones in Rhubarb by capillary electrochromatography.Electrophoresis,2000,21(15):3109
[6]. Lü H,Wang J,Wang X,et al.Rapid separation and determination of structurally related anthraquinones in Rhubarb by pressurized capillary electrochromatography.J Pharm Biomed Anal,2007,43(1):352
[7]. ZONG Yu-ying(宗玉英),YU Man-tang(余满堂),ZHU Zhi-qiang(朱志强),et al.Micellar electrokinetic capillary chromatography separation and determination Chinese traditional medicine-several Rheum species(胶束电动毛细管色谱法分离和测定几种大黄含量).Acta Pharm Sin(药学学报),1995,30(8):594