栀子大黄汤化学成分的HPLC-PDA-ESI-MS/MS分析

Chemical constituents of Zhizidahuang decoction detected by HPLC-PDA-ESI-MS/MS

目的:对栀子大黄汤中的化学成分进行归属研究,以揭示其可能的药效物质基础。方法:采用高效液相色谱/光电二极管阵列检测/串联质谱(HPLC-PDA-MS/MS)技术,分析研究栀子大黄汤中主要化学成分的结构。色谱条件:C18柱,0.1%乙酸-甲醇二元梯度;PDA扫描范围:210～480nm;ESI离子源,负离子模式,Data dependent scan方式采集数据。结果:建立栀子大黄汤水煎液的HPLC-PDA-ESI-MS/MS色谱分离分析体系。根据各色谱峰对应物质的质谱裂解碎片、紫外吸收光谱特征、提取离子流结果,初步归属鉴定出20个化学成分,分属黄酮类、蒽醌类、环烯醚萜类等。结论:高效液相色谱结合光谱检测技术、质谱检测技术,可以在基本不依赖对照品的情况下,实现对中药复杂体系中主要成分的定性分析。

Aim： To investigate the chemical components in Zhizidahuang decoction（ZZDHD） to reveal the possible material therapeutic basis. Methods： High performance liquid chromatography coupled with photodiode array detector and tandem mass spectrometry（HPLC-PDA-MS/MS） was applied to simultaneously characterize the chemical components and their structures in ZZDHD. The analysis was preformed on a Lichrospher C18 column using a binary eluent of 0. 1% acetic acid（A） and methanol（B） mixed under the gradient mode; UV spectra were scaned from 210 nm to 480 nm; negative ESI experiments in data-dependent scan mode were performed. Results： HPLC-PDA-MS/MS chromatogram of ZZDHD was achieved. Based on UV spectral data, information of molecular weight and mass fragmentation behaviors connected with extracted ion current（EIC） chromatogram, twenty kinds of components were detected and identified, including flavonoids, anthraquinones, iridoids and other constituents. Conclusion： The method presented in this study, which combined HPLC with UV and MS, allowes the characterization of compounds in the complex herbal system even without the reference standards.