基于UPLC-ESI-QTOF-MS/MS技术检测扶正固本颗粒化学成分  

Identification of Chemical Substances in Fuzheng Guben Granules Based on UPLC-ESI-QTOF-MS/MS Technique

作　　者：仝立国[1] 牛艳艳[1] 贾力莉[1] 王若瑜 宋美卿[1] 夏召弟 冯玛莉[1] 汪欣文[1] 吉海杰[1,2] TONG Liguo;NIU Yanyan;JIA Lili;WANG Ruoyu;SONG Meiqing;XIA Zhaodi;FENG Mali;WANG Xinwen;JI Haijie(Shanxi Academy of Traditional Chinese Medicine,Taiyuan Shanxi 030012,China;Postdoctoral Research Station,China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]山西省中医药研究院,山西太原030012 [2]中国中医科学院博士后流动站,北京100700

出　　处：《中国药物警戒》2021年第9期831-836,共6页Chinese Journal of Pharmacovigilance

基　　金：国家自然科学基金资助项目(81973672);山西省科技攻关项目山西省中药现代化关键技术研究振东专项(2016ZD0302);中国博士后科学基金面上项目(2016M590186);山西省中医药管理局科研课题(2019ZYYC005,2020ZYYZ010);山西中医药大学科技创新能力培育计划项目(2019PY-020)。

摘　　要：目的基于超高效液相色谱-电喷雾离子源-四极杆飞行时间质谱联用技术(UPLC-ESI-QTOF-MS/MS)检测扶正固本颗粒中的化学成分并进行确认。方法采用ACQUITY UPLC HSS T3 C_(18)色谱柱(2.1 mm×100 mm,1.8μm),以0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B)为流动相梯度洗脱,流速0.2 mL/min,柱温40℃,同时联合XEVO G2-XS ESI离子源进行正、负离子模式测定,通过比对保留时间、分子精确质量数及二级质谱碎片等参数,结合UNIFI软件分析各成分碎片裂解方式并参考化学成分数据库及文献数据对检测到的化学成分进行确认鉴定。结果初步鉴定出56个化合物,其中包括黄酮类化合物29个,蒽醌类化合物9个,二苯乙烯苷类化合物2个,萜类化合物6个,皂苷类化合物3个及7个其他成分。结论该方法可快速、准确的鉴定出扶正固本颗粒中的多种化学成分,为寻找其药效物质基础及进一步建立全面质量控制方法提供了依据。Objective To analyze the chemical constituents in Fuzheng Guben granules using ultra performance liquid chromatography electrospray ion source quadrupole time of flight mass spectrometry(UPLC-ESI-QTOFMS/MS).Methods The chromatographic column of Acquity UPLC HSS T3 C18(2.1×100 mm,1.8μm)was used.The mobile phase was 0.1%formic acid methanol solution(A)-0.1%formic acid aqueous solution(B)in gradient elution,the flow rate 0.2 ml/min,and the column temperature was 40℃.The positive and negative ion modes of each component were determined respectively by Xevo G2-XS ESI ion source.According to such parameters as the retention time,molecular accurate mass number and secondary mass spectrum fragments,Unifi software was used to analyze the fragmentation mode of each component,while the reference chemical component database and literature data were used to analyze the detected chemical components.Results Fiftysix compounds were identified,including 29 flavonoids,9 anthraquinones,2 stilbene glycosides,6 terpenes,3 saponins and 7 other components.Conclusion This method can identify various chemical components of Fuzheng Guben granules quickly and accurately,which provides data for finding effective substances and establishing methods for total quality control.

关 键 词：扶正固本颗粒 超高效液相色谱仪 电喷雾离子源 四极杆飞行时间质谱 

分 类 号：R927.2[医药卫生—药学]