基于UPLC-ESI-Q-TOF-MS技术定性分析苏孜阿甫化学成分

Identification of chemical constituents in Suziapu by UPLC-ESI-Q-TOF-MS

目的:采用超高效液相色谱离子源-电喷雾-四极杆-飞行时间质谱联用技术(UPLC-ESI-Q-TOF-MS)快速定性分析维药苏孜阿甫方中化学成分。方法:色谱柱为Agilent Poroshell 120 EC-C18(3mm×150mm,2.7μm),流动相为0.01%甲酸-5mmol·L^(-1)甲酸铵水溶液(A),0.1%甲酸-乙腈(B),梯度洗脱,体积流量0.4mL·min^(-1),进样量1μL;采用电喷雾离子源(ESI),正、负离子模式扫描,扫描范围为m/z 50~1200。Sensitivity模式下,依赖MSE方式采集数据。基于UNIFI在线软件、MassLynx V4.2软件及数据库进行化学成分解析、鉴定,并根据精确质荷比、特征离子碎片、离子强度、保留时间等信息,结合对照品及文献信息二次人工复核化合物鉴定结果,总结裂解规律。结果:初步指认出苏孜阿甫方中33个化学成分,包括倍半萜、黄酮、萘醌、有机酸、香豆素及萜类成分,并对主要化合物裂解途径进行了初步分析。结论:首次基于UPLC-ESI-Q-TOF-MS技术对苏孜阿甫方中化学成分进行了快速定性分析,该成分分析为阐明苏孜阿甫药效物质基础,建立产品质量控制方法奠定了基础。

OBJECTIVE To establish a method for rapid detection and identification of the various compounds in Suziafu based on UPLC-ESI-Q-TOF-MS.METHODS The chromatographic separation was performed on an Agilent Poroshell 120 EC-C18(3 mm×150 mm,2.7μm)for gradient elution with the mobile phase of 0.01%formic acid-5 mmol·L^(-1) ammonium formate solution(A)and 0.1%formate acetonitrile solution(B)for gradient elution,the flow rate was 0.4 mL·min^(-1),the injection volume was 1μL.The mass spectrographic analysis was conducted with electron spray ionization(ESI),sample MS data was acquired by time-dependent MSE in both positive and negative ion mode,the collection range was m/z 50~1200.The compounds information was firstly compared with the database by UNIFI software,then manual verification of the structure identification was completed by referring to the accurate mass,fragment ions,the intensity of fragments,retention time,isotope information based on the Pubchem Database,Chemspider Database and the previous reports.RESULTS A total of thirty-three chemical components have been identified in Suziafu,including sesquiterpenoids,flavonoids,naphthoquinones,organic acids and other components.CONCLUSION The rapid method based on UPLC-ESI-Q-TOF-MS and UNIFI was achieved for identification of chemical components in Suziafu for the first time.It also provides ideas for further study on the material basis and the product quality control.