广西民族药材小叶金花草质量标准提升研究  

Research on improvement of quality standard of the Guangxi ethnic herb Onychii Herba

作　　者：林雀跃 戴胜云 谢培德 滕爱君 马双成[2] 李丽莉 郑健[2] LIN Que-yue;DAI Sheng-yun;XIE Pei-de;TENG Ai-jun;MA Shuang-cheng;LI Li-li;ZHENG Jian(Guangxi Institute for Food and Drug Control,Nanning 530021,China;National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]广西壮族自治区食品药品检验所,南宁530021 [2]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2022年第8期1319-1327,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：2017年国家“重大新药创制”子课题“壮药材小叶金花草的质量评价研究”(2017ZX09301060-011-002)。

摘　　要：目的:完善广西民族药材小叶金花草质量标准,提高其质量控制水平。方法:对广西境内小叶金花草进行资源调查及实地采样,收集17批次小叶金花草药材及5批混伪品大叶金花草药材,结合显微鉴别(包括根茎横切面和粉末显微)和薄层色谱鉴别对二者进行判别;参照2020年版《中华人民共和国药典》通则,对小叶金花草药材的水分、总灰分、酸不溶灰分和浸出物进行测定;建立小叶金花草中菊苣酸的HPLC测定法,采用CAPCELLPAK MGⅡC色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.3%磷酸水溶液(19∶81),流速为1.0 mL·min,检测波长为330 nm,柱温为25℃。结果:与现行质量标准2018年版《广西壮族自治区壮药质量标准》第三卷相比,新增了根茎横切面显微鉴别,修订了薄层色谱鉴别方法,斑点更清晰,专属性更强;建立了菊苣酸的含量测定方法,菊苣酸质量浓度在2.73~273μg·mL范围内线性关系良好(r=1.000),平均回收率为102.8%(RSD为1.1%,n=6),17批次样品菊苣酸的含量范围为0.12%~2.23%。结论:本文建立了完整的显微鉴别、薄层色谱鉴别、检查及含量测定方法,完善了小叶金花草药材的质量标准,为合理评价小叶金花草质量提供数据支撑和科学依据。Objective:To improve the quality standard of Onychii Herba and improve its quality control level.Methods:A resource survey and field collection of Onychii Herba were carried out in Guangxi.Microscopical characteristics of 17 batches of Onychii Herba and 5 batchs of Sphenomeridis Herba were studied based on transverse section and powder.TLC was adopted to distinguish between Onychii Herba and Sphenomeridis Herba.The water content,total ash,acid-insoluble ash and ethanol soluble extractives were determined according to the method in the appendix of Chinese Pharmacopoeia.The content of cichoric acid was determined by HPLC.TheCAPCELLPAK MGⅡCcolumn(250 mm×4.6 mm,5μm)was used,the mobile phase was acetonitrile-0.3%phosphoric acid(19∶81)at a flow rate of 1.0 mL·min,the column temperature was 25℃,and the detection wavelength was at 330 nm.Results:Compared with Quality Standards for Zhuang Medicine in Guangxi Zhuang Autonomous Region,microscopically characteristics of transverse section was proposed,the improved TLC showed the spots developed clearly.The linear range of cichoric acid was 2.73-273μg·mL(r=1.000)and the average recovery was 102.8%(RSD=1.1%,n=6),the content of cichoric acid in 17 batches of samples ranged from 0.12%to 2.23%.Conclusion:The established method in this paper such as microscopic identification,TLC identification,inspection and content determination,improves the quality standardand provides evidence for further improvement of quality standards of Onychii Herba.

关 键 词：小叶金花草 大叶金花草 菊苣酸 质量标准 显微鉴别 薄层色谱鉴别 含量测定 

分 类 号：R917[医药卫生—药物分析学]