《中华人民共和国药典》中灯盏细辛含量测定方法的优化  

Optimization of determination method for Erigerontis Herba in Chinese Pharmacopoeia

作　　者：李资磊 唐琼 董媛 张赟华 杜江 张雯洁 LI Zi-lei;TANG Qiong;DONG Yuan;ZHANG Yun-hua;DU Jiang;ZHANG Wen-jie(Yunnan Biovalley Pharmaceutical Co.,Ltd.,Kunming 650503,China;Yunnan Institute for Food and Drug Control,Kunming 650106,China)

机构地区：[1]云南生物谷药业股份有限公司,昆明650503 [2]云南省食品药品监督检验研究院,昆明650106

出　　处：《药物分析杂志》2020年第7期1309-1318,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：国家中药标准化项目“灯盏生脉胶囊标准化建设”(ZYBZH-C-YN-57)。

摘　　要：目的:优化《中华人民共和国药典》(简称《中国药典》)中灯盏细辛含量测定项下野黄芩苷的供试品溶液制备方法及色谱条件。方法:对供试品溶液制备方法进行比较;采用DAD检测器对野黄芩苷色谱峰进行峰纯度检查,分离色谱峰中的杂质化合物鉴定其结构,选择能将野黄芩苷与杂质峰分离的色谱条件。结果:采用50%甲醇超声处理制备供试品溶液方法提取更完全且操作简便。《中国药典》灯盏细辛的含量测定项下"野黄芩苷"峰实际是野黄芩苷与飞蓬酯乙的混合峰;以甲醇-四氢呋喃-0.2%磷酸溶液(14∶14∶72)为流动相可使野黄芩苷与飞蓬酯乙完全分离;经方法学验证其线性范围为21.2~424.0μg·mL^-1(r=0.9999);加样回收率平均值(n=12)为98.7%,RSD为2.1%。结论:优化后的方法较《中国药典》方法测定结果准确,且简便,重复性好,为灯盏细辛质量标准修订提供依据。Objective:To optimize the extracting methods and chromatographic conditions for content determination of scutellarin in Erigerontis Herba.Methods:Preparation methods of test solution were compared.A diode array detector was used to detect the peak purity of the chromatographic peak of scutellarin.The impurity compound contained was separated and the structure was elucidated.The chromatographic conditions that could separate the scutellarin from the impurity impurities were chosen.Results:Using 50%methanol ultrasonic treatment to prepare the test solution was more complete and easier to operate.The peak of scutellarin obtained from Chinese Pharmacopeia method was the mixture of scutellarin and erigeron B in deed.Methanoltetrahydrofuran-0.2%phosphoric acid solution(14∶14∶72)could be used as the mobile phase to completely separate scutellarin and erigeron B.Methodological verification showed that the linear range was 21.2-424.0μg·mL^-1(r=0.9999),and the average recovery(n=12)was 98.7%with RSD of 2.1%.Conclusion:The optimized method is more accurate than the method of Chinese Pharmacopoeia,and it is simple and repeatable.This study provides a scientific basis for the revision of the quality standards of Erigerontis Herba.

关 键 词：灯盏细辛 野黄芩苷 飞蓬酯乙 质量标准修订 供试品溶液制备优化 色谱条件优化 

分 类 号：R917[医药卫生—药物分析学]