目的:建立灯盏细辛中多酚类成分的定性、定量分析方法。方法:色谱分离采用AlltimaTMC18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%甲酸水体系,梯度洗脱,流速为1.0 mL.min-1,检测波长为330 nm;质谱定性采用离子阱多级质谱(Trap-MSn)结合飞行时间质谱(TOF-MS),负离子模式扫描;应用HPLC法建立不同产地、不同药用部位灯盏细辛药材中绿原酸、灯盏乙素、3,5-O-双咖啡酰基奎宁酸、1,5-O-双咖啡酰基奎宁酸、4,5-O-双咖啡酰基奎宁酸5个多酚类化合物的含量测定方法,应用紫外-可见分光光度法建立灯盏细辛总多酚含量测定方法。结果:通过应用2种质谱信息组合分析策略鉴定了灯盏细辛中14个主要色谱峰的结构;含量测定结果表明,不同产地及不同药用部位灯盏细辛药材中有效成分含量存在明显的差异。结论:本实验所建立的分析方法,简单易行,为灯盏细辛药材质量控制提供可行的方法。
Objective: To establish qualitative and quantitative analysis methods for quality evaluation of Erigeron breviscapus.Methods: The separation was performed on an Alltima C18 reverse-phase column(250 mm × 4.6 mm,5 μm);the mobile phase consisted of water containing 0.1% formic acid and acetonitrile with gradient elution at the flow rate of 1.0 mL.min-1,and the detection wavelength was 320 nm.A combination of ion trap tandem mass spectrometer(Trap-MSn) and time-of-flight mass spectrometer(TOF-MS) was applied to qualitative analysis under negative ion mode.The contents of 5 marker compounds,chlorogenic acid(3-O-CQA),scutellarin,3,5 O-dicaffeoylquinic acid(3,5-O-diCQA),1,5-O-dicaffeoylquinic acid(1,5-O-diCQA) and 4,5-O dicaffeoylquinic acid(4,5-O-diCQA),as well as total polyphenol of 11 samples of different origin and different parts of Erigeron breviscapus were determined by HPLC and UV,respectively.Results: Totally 14 peaks were identified based on the retention time,on-line UV spectra and MS spectra.The quantitative analysis results showed that there were obvious differences among different origins and different parts of Erigeron breviscapus.Conclusion: The established methods are simple and reliable,which are helpful for quality control of Erigeron breviscapus.