摘要
目的 建立鉴定两面针根部化学成分的超高效液相色谱-四极杆-飞行时间串联质谱法。方法 色谱柱为Zorbax Eclipse Plus C_(18)柱(100 mm×3.0 mm,1.8μm),流动相为乙腈-0.1%甲酸水溶液(梯度洗脱),流速为0.3 mL/min,柱温为30℃,进样量为4μL。检索PubMed、SciFinder、ChemSpider、中国知网、中国科学院化学专业数据库,检索时限为自建库至2024年1月,收集两面针根部化学成分数据,采用Qualitative Analysis B 8.0定性分析软件,建立化学成分数据库。采用电喷雾离子化正、负离子模式对两面针根部进行质谱检测,得化合物精准相对分子质量及二级碎片离子信息,通过核对对照品的文献数据、二级质谱数据及自建数据库信息,快速鉴定目标化合物。结果 共鉴定出化合物73个,包括生物碱类64个(含苯并菲啶类23个,喹啉类12个,原小檗碱类11个,阿朴芬类6个,苄基异喹啉类4个,呋喃喹啉类和普罗托品类各3个,原鸦片碱类2个),氨基酸衍生物3个,黄酮类2个,倍半萜1个,其他类3个,其中4个化合物为首次在两面针根部中发现。结论 所建方法可快速鉴定两面针根部化学成分,该研究为后续药理活性和质量控制等研究提供了参考。
Objective To establish an ultra-performance liquid chromatography electrospray quadrupole time-of-flight mass spectrometry(UPLC-TOF-MS/MS)method for the identification of the chemical constituents of Zanthoxyli Radix Methods The chromatographic column was Zorbax Eclipse Plus C_(18) column(100 mm×3.0 mm,1.8μm),the mobile phase was acetonitrile-0.1%formic acid aqueous solution(gradient elution),the flow rate was 0.3 mL/min,the column temperature was 30℃and the injection volume was 4µL.The databases of PubMed,SciFinder,ChemSpider,CNKI and Chemistry Database of Chinese Academy of Sciences were searched from the establishment of the database to January 2024 and the chemical constituents data of the Zanthoxyli Radix were collected.Qualitative Analysis B 8.0 qualitative analysis software was used to establish a chemical constituents database.Electrospray ionization positive and negative ion modes were used for mass spectrometry detection of Zanthoxyli Radix to obtain accurate relative molecular mass and secondary fragment ion information of chemical constituents.The target chemical compounds were quickly identified by checking the literature information of the reference substance,secondary mass spectrometry data and self-built database information.Results A total of seventy-three compounds were identified,including sixty-four alkaloids(including twenty-three benzophenanthridines,twelve quinolines,eleven protoberberine types,six aporphines,four benzylisoquinolines,three furanquinolines and protopines,respectively and two protopines),three amino acid derivatives,two flavonoids,one sesquiterpene and three others.Four of them were found in the Zanthoxyli Radix for the first time.Conclusion The established method can quickly identify the chemical constituents of the Zanthoxyli Radix.This study provides a reference for subsequent studies on pharmacological activity and quality control.
作者
饶碧莹
肖幸华
周自勤
张珞瑜
王玉新
刘文龙
RAO Biying;XIAO Xinghua;ZHOU Ziqin;ZHANG Luoyu;WANG Yuxin;LIU Wenlong(College of Pharmacy,Hunan University of Chinese Medicine,Changsha,Hunan,China 410208;Xiangya Changde Hospital,Changde,Hunan,China 415000;Xiangya Hospital of Central South University,Changsha,Hunan,China 410008;Changde Pharmaceutical Group Co.,Ltd.,Changde,Hunan,China 415000;College of Pharmacy,Dali University,Dali,Yunnan,China 671013)
出处
《中国药业》
2025年第18期42-49,共8页
China Pharmaceuticals
基金
湖南省自然科学基金(科药联合基金)[2021JJ80020]。
