HPLC法测定银屑舒凝胶中间体中蒽醌成分的含量

Determination of anthraquinone Intermediates in YinXieShu Gel by HPLC

目的:建立银屑舒凝胶中间体大黄素、大黄酚、大黄素甲醚的含量测定方法。方法:采用HPLC法测定中间体中三个成分的含量,选用Phenomenex Luna C18色谱柱(4.6×250 mm,5μm),流动相为甲醇(A)-0.1%磷酸水溶液(B)=81∶19,流速:1.0 mL/min,检测波长254 nm,柱温25℃。结果:大黄素、大黄酚、大黄素甲醚分别在5.11~102.2μg/mL(r=0.999 9)、6.22~124.5μg/mL(r=0.999 8)、5.92~118.4μg/mL(r=0.999 1)范围内线性关系良好,银屑舒凝胶中间体中3个成分的加样回收率分别为103.79%、100.67%、104.87%;3批中间体中大黄素、大黄酚、大黄素甲醚的含量分别为3.5~3.7、3.4~3.6、1.0~1.1mg/g。结论:本试验所建立的方法有较强的选择性和专属性,准确可靠,可作为银屑舒凝胶中间体蒽醌的含量测定方法,也为银屑舒制剂的方法探讨提供依据和基础。

Objective:To establish an HPLC method for the determination of emodin,chrysophanol,and emodin in the intermediates of YinXieShu gel. Methods:The content of 3 components in the intermediate were determined by HPLC,and the HPLC method was performed on a Phenomenex Luna C18 column(4.6×250 mm,5 μm)with the mobile phase consisting of methanol(A)-0.1% phosphoric acid(B)(81∶19)at the flow rate of 1.0 mL/min,The detection wavelength was set at 254 nm,and the column temperature was 25 ℃. Results:The emodin,chrysophanol,and ararobinol revealed a good linear relationship in the range of 5.11 to 102.2 μg/mL(r=0.999 9),6.22 to 124.5 μg/mL(r=0.999 8),and 5.92 to 118.4 μg/mL(r=0.9991),respectively.The recoveries of the 3 components in the Yinxueshu gel intermediate were obtained. They were103.79%,100.67%,and 104.87%,respectively. The contents of emodin,chrysophanol,and emodin in the three batches of intermediates were 3.5 ~3.7,3.4 ~3.6,and 1.0 ~1.1 mg/g,respectively. Conclusion:the method has strong selectivity and specificity,and it is accurate and reliable.It can be used for determination of anthraquinone in YinXieShu gel intermediate. It also provides basis for the exploration of YinXieShu preparation methods.