双标多测法同时测定地胆草中11种成分的含量  

Simultaneous content determination of eleven constituents in Elephantopus scabre by TRSDMC

作　　者：果佳慧 高乐 甄亚钦 蔡于罗 胡婧楠 田伟 牛丽颖 GUO Jia-hui;GAO Le;ZHEN Ya-qin;CAI Yu-luo;HU Jing-nan;TIAN Wei;NIU Li-ying(Hebei University of Chinese Medicine,Shijiazhuang 050091,China;Hebei Provincial Technology Innovation Center for Traditional Chinese Medicine Formula Granules,Shijiazhuang 050091,China;Hebei Provincial Engineering Research Center for Quality Evaluation and Standardization of Traditional Chinese Medicines,Shijiazhuang 050091,China)

机构地区：[1]河北中医药大学,河北石家庄050091 [2]河北省中药配方颗粒技术创新中心,河北石家庄050091 [3]中药材品质评价与标准化河北省工程研究中心,河北石家庄050091

出　　处：《中成药》2024年第11期3557-3564,共8页Chinese Traditional Patent Medicine

基　　金：河北省自然科学基金重点项目(H2022423335);河北省重点研发计划项目(20372502D);河北省中医药管理局科研计划项目(2023125)。

摘　　要：目的建立双标多测法同时测定地胆草中新绿原酸、绿原酸、隐绿原酸、木犀草苷-7-O-葡萄糖醛酸苷、异绿原酸B、异绿原酸A、异绿原酸C、去氧地胆草素、异去氧地胆草素、异地胆草种内酯、地胆草种内酯的含量。方法分析采用Waters Symmetry C_(18)、Phenomenex C_(18)、Agilent ZORBAX Eclipse Plus C_(18)色谱柱(4.6 mm×250 mm,5.0μm);流动相乙腈-0.1%磷酸,梯度洗脱;体积流量1.0 mL/min;柱温35℃;检测波长220、326 nm。以绿原酸为内标,计算新绿原酸、隐绿原酸、木犀草苷-7-O-葡萄糖醛酸苷、异绿原酸B、异绿原酸A、异绿原酸C相对校正因子;以异去氧地胆草素为内标,计算去氧地胆草素、地胆草种内酯、异地胆草种内酯相对校正因子,测定其含量。再进行聚类分析、主成分分析、正交偏最小二乘法-判别分析。结果11种成分在各自范围内线性关系良好(r≥0.9990),平均加样回收率95.3%~103.4%,RSD 0.32%~3.45%。双标多测法所得结果与外标法接近。异绿原酸A、异绿原酸C、异绿原酸B、绿原酸、木犀草苷-7-O-葡萄糖醛酸苷、隐绿原酸为质量差异成分。结论该方法稳定可靠,可用于地胆草的质量控制。AIM To establish a two reference substances for determination of multiple components(TRSDMC)method for the simultaneous content determination of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,luteolin-7-O-glucuronide,isochlorogenic acid B,isochlorogenic acid A,isochlorogenic acid C,deoxyelephantopin,isodeoxyelephantopin,isoscabertopin and scabertopin in Elephantopus scabre L..METHODS The analysis was performed on a 35℃thermostatic Waters Symmetry C_(18),Phenomenex C_(18),Agilent ZORBAX Eclipse Plus C_(18) columns(4.6 mm×250 mm,5.0μm),with the mobile phase comprising of acetonitrile and 0.1%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 220,326 nm.Chlorogenic acid was used as an internal standard to calculate the relative correction factors of neochlorogenic acid,cryptochlorogenic acid,luteolin-7-O-glucuronide,isochlorogenic acid B,isochlorogenic acid A and isochlorogenic acid C,while isodeoxyelephantopin was used as an internal standard to calculate the relative correction factors of deoxyelephantopin,scabertopin and isoscabertopin,after which the content determination was made.Subsequently,cluster analysis,principal component analysis and orthogonal partial least squares-discriminant analysis were conducted.RESULTS Eleven constituents showed good linear relationships within their own ranges(r≥0.9990),whose average recoveries were 95.3%-103.4%with the RSDs of 0.32%-3.45%.The result obtained by TRSDMC approximated those obtained by external standard method.Isochlorogenic acid A,isochlorogenic acid C,isochlorogenic acid B,chlorogenic acid,luteolin-7-O-glucuronide and cryptochlorogenic acid were taken as quality differential constituents.CONCLUSION This reliable and stable method can be used for the quality control of E.scabre.

关 键 词：地胆草 化学成分 含量测定 双标多测 聚类分析 主成分分析 正交偏最小二乘法-判别分析 

分 类 号：R284.1[医药卫生—中药学]