高效液相色谱法测定大黄末中大黄蒽醌的含量

Determination of Rhubarb anthraquinone in Rhubarb powder by HPLC

建立了大黄末中大黄蒽醌含量测定的高效液相色谱方法。采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm),甲醇-0.1%磷酸溶液(85∶15)为流动相,流速1.0 m L/min,荧光检测器检测,激发波长为442 nm,发射波长为514 nm。大黄酸、大黄素、大黄酚的浓度分别在0.2108-10.540 0μg/m L(r=0.999 9)、0.200 0-10.000 0μg/m L(r=0.999 6)、0.209 2-10.460 0μg/m L(r=0.999 5)范围内线性关系良好;平均回收率(n=3)分别为103.5%(RSD为3.0%)、102.3%(RSD为2.6%)、98.76%(RSD为2.9%)。结果提示,本方法准确灵敏,可用于大黄末的质量控制。

The HPLC method was established for the determination of Rhubarb anthraquinone in Rhubarb powder. A chromatographic column of Agilent Eclipse XDB-C18 （250 mm×4.6 mm,5μm） was used with the mobile phase of methanol - 0.1% phosphoric acid solution （85：15） at the flow rate of 1.0 mL/min. The compound was determined at λex 442 nm and λex 514 nm by fluorescence detector. The calibration curves were linear in ranges of 0.210 8-10.540 0 μg/mL （r= 0.999 9） for rhein, 0.200 0-10.000 0 μg/mL（r=0.999 6） for emodin, 0.209 2-10.460 0 μg/mL （r=0.999 5） for chrysophanol. The average recoveries （n=3） of rhein, emodin and chrysophanol were 103.5% （RSD= 3.0%）, 102.3% （RSD=2.6%） and 98.76% （RSD= 2.9%）, respectively. The method is accurate and sensitive for the quality control of Rhubarb powder.