艾椒散质量标准研究

Study on quality standard of Aijiao powder

目的:为艾椒散质量标准的建立提供参考。方法:采用薄层色谱法(TLC)对艾椒散中蜂房、艾叶、芦荟进行定性鉴别;采用高效液相色谱法(HPLC)测定艾椒散中大黄素、大黄酚的含量,色谱柱为Waters Xbridge C18(4.6×250 mm,5μm),流动相为甲醇-0.1%磷酸溶液(75∶25),柱温为25℃,流速为1.0 mL/min,检测波长为254 nm,进样量为10μL。结果:TLC结果显示各供试品色谱与对照药材色谱相应位置上有相同颜色的对应斑点,斑点清晰,分离度好,且阴性对照无干扰。大黄素、大黄酚质量浓度分别在0.256~5.12 mg/mL(r=0.99967)、0.374~14.96 mg/mL(r=0.99912)范围内线性关系良好;平均加样回收率分别为97.7%(RSD=2.3%)、99.7%(RSD=2.5%);测得艾椒散中大黄素、大黄酚的平均含量分别为1.3075、1.8225 mg/g。结论:本研究所建立的鉴别方法简单、精确,专属性强、重现性好,可以用于控制艾椒散的质量。

Objective:To provide reference for the establishment of quality standard of Aijiao powder.Methods:The beehive,wormwood leaf and aloe in Aijiao powder were qualitatively identified by TLC and the contents of emodin and chrysophanol in Aijiao powder were determined by HPLC.HPLC was corried on Waters Xbridge C18 columns(4.6×250 mm,5μm),column temperature was 25℃,the mobile phase was methanol-0.1%phosphoric acid solution(75∶25)at a flow rate of 1.0 mL/min.The detection wavelength was 254 nm and the injection volume was 10μL.Results:TLC spotting were clear without negative interference.The linear ranges of emodin and chrysophanol were 0.256~5.12 mg/mL(r=0.99967)and 0.374~14.96 mg/mL(r=0.99912)respectively,and average recovery rates were 97.7%(RSD=2.3%)and 99.7%(RSD=2.5%)respectively.The average contents of emodin and chrysophanol in Aijiao powder were 1.3075 mg/g and 1.8225 mg/g respectively.Conclusion:The methods of identification and content determination developed by this study were simple,accurate,have strong specificity and good reproducibility,and applicable for the quality control of Aijiao powder.