摘要
目的:采用超高效液相色谱-电喷雾离子源-四极杆-飞行时间质谱技术(UPLC-ESI-Q-TOF/MSE)快速分离、分析颠茄草化学成分。方法:采用Agilent Poroshell 120 EC-C18色谱柱(3 mm×150 mm,2.7μm),以乙腈为流动相A,醋酸铵缓冲溶液为流动相B,梯度洗脱,流速0.5 mL·min-1,柱温30℃,进样量2μL;采用电喷雾离子源(ESI),正离子模式下采集数据,通过建立的Agilent PCDL颠茄属化合物数据库初步检索鉴定化合物,并人工复核相对分子质量、特征离子、中性丢失、色谱保留时间等信息,同时利用Agilent MSC结构解析软件,结合对照品信息和数据库信息确证结构,总结裂解规律。结果:初步鉴定出颠茄草中化学成分19个,并归纳了莨菪碱类化合物的裂解规律。结论:采用UPLC-ESI-Q-TOF/MS法快速分析颠茄草化学成分,为进一步阐明颠茄草药效物质基础和质控指标的选择提供依据。
Objective:To rapidly identify the chemical constituents of Belladonnae Herb using ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry(UPLC-Q-TOF/MSE).Methods:The analysis was performed on an Agilent Poroshell 120 EC-C18 column(3 mm×150 mm,2.7μm)at 30℃.Acetonitrile(A)and ammonium acetate buffer solution(B)were used as the mobile phase in gradient elution mode.The flow rate was 0.5 mL·min-1.Data were collected under ESI positive mode,and the constituents were identified primaril by the software of Agilent mass hunter qualitative analysis and Agilent PCDL database.Then their structure and fragmentation patterns were verified based on accurate mass,characteristic ions,neutral losses,retention time,reference substance,Agilent MSC software and database.Results:A total of 19 chemical components were identified,and the fragmentation patterns of tropane alkaloids were summarized.Conclusion:The chemical constituents of Belladonnae Herba are rapid identified by UPLC-Q-TOF/MSE,which provides basis for further clarifying the material of its efficacy and the selection of quality control indicators.
作者
王宇卿
庄果
王晓瑜
卞华
WANG Yu-qing;ZHUANG Guo;WANG Xiao-yu;BIAN Hua(Scientific Research Center,Nanyang Medical College,Nanyang 473061,China;Henan Key Laboratory of Zhang Zhong-jing Formulae and Herbs for Immunoregulation,Nanyang 473004,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第6期1063-1068,共6页
Chinese Journal of Pharmaceutical Analysis
基金
河南省高校科技创新人才支持计划(19HASTIT007)
河南省博士后科研项目(2014110)
河南省张仲景方药与免疫调节重点实验室开放课题(kfkt201702)
河南省基础与前沿技术研究项目(152300410181)
河南省高等学校青年骨干教师培养计划(2016GGJS-279)
