基于UHPLC-Q-Exactive Orbitrap MS、指纹图谱及多成分含量测定的铁线透骨草质量评价与提取工艺优化OA
Quality Evaluation and Extraction Process Optimization of Clematis intricata Based on UHPLC-Q-Exactive Orbitrap MS,Fingerprinting,and Multi-component Content Determination
目的:分析铁线透骨草化学成分,建立其指纹图谱及绿原酸等 4 个成分的含量测定方法,并结合化学计量学对不同产地的铁线透骨草进行质量评价.方法:基于超高效液相色谱轨道阱质谱法(UHPLC-Q-Exactive Orbitrap MS)对铁线透骨草进行化学成分分析;基于高效液相色谱法(HPLC)建立化学成分指纹图谱并进行相似度评价;结合聚类分析(CA)、主成分分析(PCA)、正交偏最小二乘法-判别分析(OPLS-DA)评价铁线透骨草的质量;以提取溶剂、料液比、超声时间为影响因素,对绿原酸、咖啡酸、芦丁及丹皮酚的含量进行测定,采用L9(34)正交试验法优化提取工艺.结果:从铁线透骨草中鉴别出包括黄酮、苯丙素等类 50 个化合物,通过对照品比对,指认出其中的 5 个成分;通过HPLC指纹图谱标定了 16 批样品中的 15 个共有峰,绿原酸和芦丁为张家口-保定产区特征性成分,峰 5、峰 2、峰 1 和峰 15 关联承德产区样本.确定的绿原酸、咖啡酸、芦丁、丹皮酚的最佳提取工艺为50%乙醇 100 mL,超声提取 15 min,4 个成分在各自质量浓度范围内线性关系良好,平均加样回收率为 92%～104%,RSD<4%,含量检测方法符合《中华人民共和国药典》2025 年版要求.结论:建立的铁线透骨草HPLC指纹图谱及多成分含量测定方法合理可靠,结合化学计量学可有效评价河北铁线透骨草质量,可为其质量控制提供参考.
Objective:To analyze the chemical constituents of Clematis intricata,establish its fingerprint profile and a quantitative determination method for four components(chlorogenic acid,caffeic acid,rutin,and paeonol),and evaluate the quality of C.intricata from different geographical origins by combining chemometric analysis.Methods:The chemical constituents of C.intricata were analyzed using ultra-high-performance liquid chromatography-Q-Exactive Orbitrap mass spectrometry(UHPLC-Q-Exactive Orbitrap MS).A chemical fingerprint was established based on high-performance liquid chromatography(HPLC),and similarity evaluation was performed.Cluster analysis(CA),principal component analysis(PCA),and orthogonal partial least squares-discriminant analysis(OPLS-DA)were applied to evaluate the quality of C.intricata.Using extraction solvent,solid-to-liquid ratio,and ultrasonication time as influencing factors,the contents of chlorogenic acid,caffeic acid,rutin,and paeonol were determined,and the extraction process was optimized using an L9(34)orthogonal experimental design.Results:A total of 50 compounds,including flavonoids and phenylpropanoids,were identified in C.intricata,among which five components were identified by comparison with reference standards.Fifteen common peaks were identified in 16 batches of samples using the HPLC fingerprint.Chlorogenic acid and rutin were characteristic components of samples from the Zhangjiakou-Baoding production area,while Peak 5,Peak 2,Peak 1,and Peak 15 were associated with samples from the Chengde region.The optimal extraction conditions for chlorogenic acid,caffeic acid,rutin,and paeonol were 50%ethanol(100 mL)with ultrasonication for 15 min.The four components exhibited good linearity within their respective concentration ranges.The average recovery ranged from 92%to 104%,with RSD values less than 4%.The content determination method complied with the requirements of the Pharmacopoeia of the People's Republic of China(2025 Edition).Conclusion:The established HPLC fingerprint and multi-component quantitative determination method for C.intricata are rational and reliable.When combined with chemometric analysis,they can effectively evaluate the quality of C.intricata from Hebei Province and provide a reference for its quality control.
徐梦婷;赵春雨;周舒;黄文奕;郭彦杰;杜守颖;白洁
北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400北京中医药大学 中药学院,北京 102400
医药卫生
铁线透骨草化学成分分析高效液相色谱法指纹图谱正交试验设计含量测定质量评价
Clematis intricata Bungechemical composition analysisHPLC fingerprintorthogonal experimental designcontent determinationquality assessment
《中国现代中药》 2026 (1)
74-85,中插14,13
国家中医药管理局高水平中医药重点学科建设项目(zyyzdxk-2023272)
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