路路通的UHPLC双检测指纹图谱及多指标成分测定方法研究  

UHPLC with dual detection fingerprinting and determinationof multi-indicator components of Fructus Liquidambaris

作　　者：王昌宇 张鑫华 柴瑞平 张璐 陶新玉 章弘扬 胡坪 WANG Chang-yu;ZHANG Xin-hua;CHAI Rui-ping;ZHANG Lu;TAO Xin-yu;ZHANG Hong-yang;HU Ping(School of Chemistry and Molecular Engineering,Shanghai Key Laboratory of Functional Materials Chemistry,East China University of Science and Technology,Shanghai 200237,China;Thermo Fisher Scientific(China)Co.,Ltd.,Beijing 100080,China)

机构地区：[1]华东理工大学化学与分子工程学院/上海市功能性材料化学重点实验室,上海200237 [2]赛默飞世尔科技(中国)有限公司,北京100080

出　　处：《中国新药杂志》2025年第2期191-198,共8页Chinese Journal of New Drugs

摘　　要：目的:建立路路通药材的UHPLC双检测指纹图谱,并建立路路通药材中3种酚酸类化合物和3种三萜类化合物的含量测定方法,以全面反映该药材化学成分的整体分布。方法:指纹图谱分析采用超高效液相色谱-紫外检测器串联电雾式检测器(UHPLC-UV-CAD),色谱柱为Thermo Acclaim RSLC C18柱(100 mm×2.1 mm, 2.2μm),流动相为乙腈-0.1%甲酸水溶液,以梯度程序1洗脱,检测波长为254 nm。原儿茶酸、鞣花酸和丹皮酚的含量测定采用超高效液相色谱-二极管阵列检测器,紫外检测波长分别为254,259和274 nm,以梯度程序2分离。路路通酸、齐墩果酮酸和熊果酮酸的含量测定采用高效液相色谱-电雾式检测器,以Sunrise C30柱(250 mm×4.6 mm, 5.0μm)为色谱柱,梯度程序3分离。结果:指纹图谱中共确定了16个共有峰,该方法精密度、重复性及稳定性良好,18批路路通药材的指纹图谱相似度均≥0.935,化学成分相似性高。6种指标成分的标准曲线线性关系良好(R^(2)≥0.999 6),平均加标回收率在93.7%~103.8%之间,回收率的RSD≤3.07%。18批路路通药材中原儿茶酸、鞣花酸、丹皮酚、路路通酸、齐墩果酮酸和熊果酮酸的含量均值分别为0.004 1%,0.006 4%,0.015 4%,0.299%,0.310%和0.219%。结论:本文所建立的方法准确、灵敏、重复性好,能够更全面地反映路路通中的化学成分,其中的三萜类成分对路路通药材的内在质量有重要贡献。Objective:To establish an UHPLC dual detection fingerprint for Fructus Liquidambaris and develop a method for determining the content of three phenolic acid compounds and three triterpenoid compounds in Fructus Liquidambaris to comprehensively reflect the overall distribution of its chemical components.Methods:The fingerprint analysis was conducted using UHPLC coupled with a UV detector and a charged aerosol detector(UHPLC-UV-CAD).Thermo Acclaim RSLC C 18(100 mm×2.1 mm,2.2μm)column was used,with acetonitrile-0.1%formic acid aqueous solution as the mobile phase in gradient elution procedure 1,and the detection wavelength was 254 nm.The content determination of protocatechuic acid,gallic acid,and paeonol was performed using UHPLC-PDA at wavelengths of 254 nm,259 nm,and 274 nm in gradient elution procedure 2.The content determination of betulonic acid,oleanolic acid,and ursolic acid was carried out using HPLC-CAD,utilizing a Sunrise C 30 column(250 mm×4.6 mm,5.0μm)with gradient elution procedure 3.Results:A total of 16 common peaks were identified in the fingerprint,demonstrating good precision,repeatability,and stability of the method.The similarity of the fingerprints of 18 batches of Fructus Liquidambaris was all≥0.935,indicating a high similarity in chemical composition.The standard curves of the six indicator components showed good linearity(R^(2)≥0.9996),with average spiked recoveries ranging from 93.7%to 103.8%,and the RSD of recovery rates were≤3.07%.The mean contents of protocatechuic acid,gallic acid,paeonol,betulonic acid,oleanolic acid,and ursolic acid in 18 batches of Fructus Liquidambaris were 0.0041%,0.0064%,0.0154%,0.299%,0.310%,and 0.219%,respectively.Conclusion:The method established in this study is accurate,sensitive,and reproducible,capable of reflecting the chemical components in Fructus Liquidambaris more comprehensively.Among these,the triterpenoid components significantly contribute to the intrinsic quality of Fructus Liquidambaris.

关 键 词：路路通 电雾式检测器 UHPLC 双检测指纹图谱 多指标成分定量 

分 类 号：R917[医药卫生—药物分析学]