UPLC-Q-TOF-MS/MS快速鉴别北豆根中的生物碱类成分

Rapid Identification of Alkaloids in Menispermi Rhizoma by UPLC-Q-TOF-MS/MS

目的:利用UPLC-Q-TOF-MS/MS技术对北豆根中的生物碱化学成分进行分析和鉴定。方法:采用Welch C18色谱柱(2.1 mm×100 mm,1.7μm),以0.1%氨水溶液(A)-乙腈(B)为流动相进行梯度洗脱,流速0.3 mL·min^(-1),柱温40℃,进样体积2μL。质谱采用电喷雾(ESI)离子源,在正离子模式下采集数据,质量数扫描范围m/z 50~1 250,使用质谱分析软件中的目标化合物筛查法,通过保留时间、精确相对分子质量和二级质谱裂解碎片鉴定监测到的化学成分。结果:在优化的LCMS条件下,结合Scifinder数据库、对照品和相关文献鉴定了37个生物碱类化合物,包括双苄基异喹啉类、阿朴啡及氧化异阿朴啡类、单苄基异喹啉类等。结论:基于HPLC-ESI-Q-TOF技术,通过高效液相色谱分离,质谱测定相对分子质量、裂解数据、文献分析检索,能快捷、准确、较全面地鉴定北豆根中的生物碱类化学成分,为北豆根化学成分的进一步提取分离和药效物质基础的研究提供科学依据。

Objective：To analyze and identify the alkaloids chemical constituents from the Menispermi Rhizoma by UPLC-Q-TOF-MS/MS.Method：Welch C18 reverse phase column（2.1 mm×100 mm,1.7μm） was adopted,with 0.1% ammonia solution（A）-acetonitrile（B） as the mobile phase for gradient elution.The flow rate was 0.3 mL·min-1;column temperature was 40 ℃;and the injection volume was 2 μL.ESI ion source was used as mass spectra,and the data were collected in the positive mode.The mass scanning range was between m/z50-1 250.By using the target compound screening method in the mass spectrometry analysis software,the chemical components were identified according to retention time,accurate relative molecular mass and second mass spectrum fragmentation.Result：Under the optimized LC-MS condition,37 alkaloids compounds were identified based on the database of Scifinder,control substances and related references,including bis-benzyl isoquinoline compounds,apomorphine and isooxyphene oxide compounds,and monobenzylisoquinolines,et al.Conclusion：Based on UPLC-Q-TOF-MS/MS technology,relative molecular mass and fragmentation data determined by high performance liquid chromatography,as well as literature analysis,could rapidly and accurately identify the chemical components of Menispermi Rhizoma.This study could provide powerful evidences for further studying the pharmacodynamics material basis of Menispermi Rhizoma.