[关键词]
[摘要]
目的 建立不同产地川牛膝Cyathula officinalis UPLC指纹图谱,并与不同部位川牛膝及混淆品进行对比分析。方法 采用Waters acquity UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8 µm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,体积流量为0.3 mL/min,波长为210 nm,柱温为30 ℃,进样量为4 μL。结合相似度评价、聚类分析(cluster analysis,CA)、主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判别式分析(orthogonal partial least squares method-discriminant analysis,OPLS-DA)比较不同产地、不同部位川牛膝及其混淆品的差异。结果 UPLC指纹图谱共标定了川牛膝19个特征峰,并指认了2-羟基-3-[(4-羟基-3-甲氧基苯甲酰)氧基]琥珀酸、杯苋甾酮、滨蒿内酯、2-(苯甲酰基)-3-[(4-羟基-3-甲氧基苯甲酰)氧基]琥珀酸4个特征峰。通过相似度分析发现,川牛膝的不同产地、不同部位及混淆品样品均存在一定的差异,CA、PCA、OPLS-DA可将62批样品根据主产地、部位、基原进行区分,通过OPLS-DA项下的投影中的变量重要性投影(variable importance in projection,VIP)各筛选出9个差异性标志物。结论 建立的指纹图谱方法能准确有效区分川牛膝的不同产地、不同部位及其混淆品,为川牛膝的质量评价及鉴别提供参考。
[Key word]
[Abstract]
Objective To establish UPLC fingerprint for different regions of Cyathula officinalis and analyze them with C. officinalis in different parts and adulterants. Methods The UPLC analysis was performed on a Waters ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 µm) by using a mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution in a gradient elution at a flow rate of 0.3 mL/min, with a detection wavelength of 210 nm, and a column temperature of 30 ℃ and the injection volume of 4 µL. Similarity evaluation, cluster analysis (CA), principal component analysis (PCA), and orthogonal partial least squares method-discriminant analysis (OPLS-DA) were utilized to compare the differences among different regions and parts of C. officinalis and its adulterants. Results The UPLC fingerprints identified 19 characteristic peaks for C. officinalis, including four specific compounds: 2-hydroxy-3-[(4-hydroxy-3-methoxybenzyl)oxy] succinic acid, cyasterone, scoparone, and 2-(benzoyl)-3-[(4-hydroxy-3-methoxybenzyl) oxy] succinic acid. Similarity analysis revealed distinct differences among samples from various origins, parts, and adulterants of C. officinalis. CA, PCA, and OPLS-DA could differentiate 62 batches of samples according to their primary regions, parts, and botanical origins, and OPLS-DA identified nine differential markers through the variable importance in projection (VIP). Conclusion The established fingerprint method can accurately and effectively differentiate between various sources and parts of C. officinalis, as well as its adulterants, which provides reference for quality evaluation and identification of . officinalis.
[中图分类号]
R286.2
[基金项目]
四川省药品检验研究院院立科研项目(2024-KYYL-002);国家药品监督管理局中国药品监管科学行动计划第三批重点项目(RS2024Z006-075,RS2024Z006-076)