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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(75μm×64.5cm,有效长度56cm)为分离通道,以25mmol.L-1硼砂-25mmol.L-1SDS-10%乙腈(pH10.90)为背景电解质溶液,运行电压为12kV,运行温度为24℃,检测波长为254nm,压力进样为5kPa,5s。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2.4～47.0,2.4～48.4,2.1～41.4,1.9～37.0,3.8～75.0μg.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 MEKC-DAD assay for simultaneous determination of emodin, aloe-emodin, rhein, chrysophanol and physcion in rhubarb and its processed products. Methods: Micellar electrokinetic capillary electrophoresis separation mode was used. With the uncoated standard fused silica capillary tube (75μm × 64.5cm, effective length 56cm) as the separation channel and 25mmol.L-1 borax-25mmol.L-1SDS-10% (pH10.90) as the background electrolyte solution. The operating voltage was 12kV, the operating temperature was 24 ℃, the detection wavelength was 254nm, and the pressure injection was 5kPa for 5s. Results: The concentrations of emodin, aloe-emodin, rhein, chrysophanol and physcion were all good in the range of 2.4 ~ 47.0,2.4 ~ 48.4,2.1 ~ 41.4,1.9 ~ 37.0,3.8 ~ 75.0μg.mL-1 (RSD = 3.8%), 101.4% (RSD = 3.8%), 101.3% (RSD = 3.8%), and the average recoveries (n = 5) were 99.5% = 3.9%), 101.4% (RSD = 3.1%). Conclusion: The method is simple, accurate and reproducible. It can be used to evaluate and control the internal quality of Rhubarb Pieces.