江西特色中药茶芎的质量评价方法研究  

Study on the quality evaluation method of the characteristic traditional Chinese medicine Ligusticum sinense Oliv.cv.Chaxiong Mss.from Jiangxi Province

作　　者：王堂勋 张观生 杨建波[3] 陈杨 黄玉芳 杨广迪 夏明艳 王灿坚 张国松[1,2] WANG Tang-xun;ZHANG Guan-sheng;YANG Jian-bo;CHEN Yang;HUANG Yu-fang;YANG Guang-di;XIA Ming-yan;WANG Can-jian;ZHANG Guo-song(Jiangxi University of Chinese Medicine,Nanchang 330006,China;National Engineering Research Center of Chinese Medicine Solid Preparation Manufacturing Technology,Nanchang 330006,China;National Institutes for Food and Drug Control,Beijing 100050,China;Guangxi University of Chinese Medicine,Nanning 530200,China)

机构地区：[1]江西中医药大学,南昌330006 [2]中药固体制剂制造技术国家工程研究中心,南昌330006 [3]中国食品药品检定研究院,北京100050 [4]广西中医药大学,南宁530200

出　　处：《药物分析杂志》2024年第10期1665-1678,共14页Chinese Journal of Pharmaceutical Analysis

基　　金：江西中医药大学创新药物研究与开发创新团队(CXTD22001);国家自然科学基金项目(82260771,82360324);江西省“双千计划”创新领军人才长期(青年)项目(jxsq2023101090);江西省中医药标准化项目(2023A20);江西省“科技+中医药”联合计划项目。

摘　　要：目的:建立茶芎的薄层色谱鉴别方法、HPLC指纹图谱以及绿原酸、咖啡酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、阿魏酸松柏酯、洋川芎内酯A、正丁基苯酞、新蛇床内酯、Z-藁本内酯、丁烯基苯酞、欧当归内酯A、亚油酸13个化学成分含量测定方法,为茶芎药材的质量控制提供依据。方法:采用薄层色谱法,以正己烷-乙酸乙酯-冰醋酸(10∶5∶0.5)为展开剂,对茶芎中洋川芎内酯I、东莨菪内酯、阿魏酸、欧当归内酯A、Z-藁本内酯进行鉴别;采用Acutfex PA-C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.1%磷酸水溶液-乙腈为流动相,进行梯度洗脱,体积流量1 mL·min^(-1),柱温30℃,进样量10μL,检测波长210、285 nm,对54批茶芎药材进行指纹图谱构建;采用SPSS和SIMCA软件进行化学模式识别分析,同时测定13个化学成分的含量。结果:建立了茶芎药材中洋川芎内酯I、东莨菪内酯、阿魏酸、欧当归内酯A、Z-藁本内酯的薄层色谱鉴别方法;建立了茶芎的HPLC指纹图谱,标定了21个共有峰,指认出13个共有峰,除S47号药材外,其他批次药材相似度均>0.9;聚类分析后可以按照采集时间和海拔分为4类;OPLS-DA筛选出峰17(Z-藁本内酯)、峰13(洋川芎内酯A)、峰12(阿魏酸松柏酯)、峰5(阿魏酸)、峰6、峰16(新蛇床内酯)、峰2(绿原酸)7个差异性成分;建立了茶芎中绿原酸、咖啡酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、阿魏酸松柏酯、洋川芎内酯A、正丁基苯酞、新蛇床内酯、Z-藁本内酯、丁烯基苯酞、欧当归内酯A、亚油酸的含量测定方法,其线性、精密度、稳定性、重复性、加样回收率均良好,上述各成分在药材中含量范围分别为0.03~3.80、0.004~0.055、0.17~0.82、0.08~0.57、0.01~0.19、0.04~2.51、1.37~11.64、0.15~0.58、0.18~4.22、2.69~9.53、0.15~0.59、0.07~0.62、0.31~6.04 mg·g^(-1)。结论:建立的茶芎薄层色谱鉴别、HPLC指纹图谱及13个成分的含量测定�Objective:To establish a method of thin-layer chromatographic identification,HPLC fingerprints and a method of the content determination of 13 chemical constituents(chlorogenic acid,caffeic acid,ferulic acid,senkyunolide I,senkyunolide H,coniferyl ferulate,senkyunolide A,butylphthalide,sedanolide,Z-ligustralactone,butenylylphthalide,levistilide A,and linoleic acid)in Ligusticum sinense Oliv.cv.Chaxiong Mss.and to provide a basis for the quality control of Ligusticum sinense Oliv.cv.Chaxiong Mss.Methods:Thin-layer chromatography was used for the qualitative identification of senkyunolide I,scopoletin,ferulic acid,levistilide A and Z-ligustilide in Ligusticum sinense Oliv.cv.Chaxiong Mss.using n-hexane,ethyl acetate and acetic acid(10∶5∶0.5)as the mobile phase.The separation was carried out on an Acutfex PA-C_(18)column(250 mm×4.6 mm,5μm),with gradient elution of 0.1%aqueous phosphoric acid solution and acetonitrile at a flow rate of 1 mL·min^(-1).The column temperature was 30℃,the injection volume was 10μL,and the detection wavelengths were 210 nm and 285 nm.The fingerprints of 54 batches of Ligusticum sinense Oliv.cv.Chaxiong Mss.were constructed.SPSS and SIMCA software were used for the chemical pattern recognition analysis,and 13 chemical components were determined at the same time.Results:A thin-layer chromatographic method was established for the identification of senkyunolide I,scopoletin,ferulic acid,levistilide A and Z-ligustilide in Ligusticum sinense Oliv.cv.Chaxiong Mss.The HPLC fingerprints of Ligusticum sinense Oliv.cv.Chaxiong Mss.were established,21 common peaks were found,13 common peaks were identified,and the similarities of all batches of the herbs were above 0.9,except sample S47.The herbs could be roughly divided into four groups according to the collection time and altitude by clustering analysis.OPLS-DA screened out seven differential constituents:peak 17(Z-ligustilide),peak 13(senkyunolide A),peak 12(coniferyl ferulate),peak 5(ferulic acid),peak 6,peak 16(sedanolide),and peak 2(ch

关 键 词：茶芎 薄层色谱 高效液相色谱 指纹图谱 聚类分析 主成分分析 含量测定 

分 类 号：R917[医药卫生—药物分析学]