泽菊降脂片中橙黄决明素和大黄酚的定性鉴别和含量测定

Qualitative Identification and Content Determination of Aurantio-obtusin and Chrysophanol in Zeju Jiangzhi Tablets

目的:建立泽菊降脂片中橙黄决明素和大黄酚的定性鉴别与含量测定方法。方法:采用TLC法进行定性鉴别,并采用HPLC法进行含量测定。色谱柱为Wondasil C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液,梯度洗脱,流速为1.0 ml·min^(-1),检测波长为286 nm,柱温为30℃,进样量为10μl。结果:橙黄决明素和大黄酚的TLC色谱斑点清晰,分离度良好,阴性无干扰;HPLC色谱显示橙黄决明素质量浓度在1.03~25.72μg·ml^(-1)(r=0.999 9)、大黄酚质量浓度在0.48~11.92μg·ml^(-1)(r=0.999 9)范围内线性关系良好,平均回收率分别为99.21%、98.85%,RSD分别为0.70%、0.73%(n=9)。结论:本方法操作简便、结果准确、重复性好,可用于泽菊降脂片中橙黄决明素和大黄酚的定性鉴别与含量测定。

Objective： To establish the methods for the qualitative identification and content determination of aurantio-obtusin and ehrysophanol in Zeju Jiangzhi tablets. Methods： A TLC method was adopted for the qualitative identification, and an HPLC method was used for the content determination. The determination was performed on a Wondasil Cls （250 mm× 4.6 mm, 5 μm ） column with the mobile phase of aeetonitrile -0.1% phosphonie acid with gradient elution at the flow rate of 1.0 ml min - l, the detection wave- length was 286 nm, the column temperature was 30 ℃ and the injection volume was 10 μl. Results： The TLC spots of aurantio-obtusin and chrysophanol were clear and well-separated without any negative interference. The HPLC experiment results showed the good line- arity within the range of 1.03-25.72 μg ml -1 （ r = 0.999 9 ） for aurantio-obtusin, and 0.48-11.92 μg ml - 1 （ r = 0. 999 9 ） for chry- sophanol. The average recovery was 99.21%. and 98.85%, and RSD was 0.70% and 0.73% , respectively （n = 9 ）. Conclusion： The method is simple, accurate and repeatable, which can be used for the qualitative identification and content determination of auran- tio-obtusin and ehrysopbanol in Zeju Jiangzbi tablets.