摘要
目的:总结知母中皂苷类成分的质谱裂解途径,探讨不同结构亚型的皂苷类成分的裂解规律。方法:采用超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF-MS/MS),Waters ACQUITY UPLC HSS T3色谱柱,以0.01%甲酸水-乙腈作为流动相进行梯度洗脱,采用电喷雾离子源,在负离子模式进行扫描,解析知母总皂苷成分的质谱信息,总结该类成分的质谱裂解规律。根据保留时间、精确分子量及二级质谱碎片离子等相关信息,结合质谱裂解规律,对知母皂苷类成分进行快速识别。结果:在知母中共鉴识出15个皂苷成分及3个皂苷元成分,在多级质谱中,15个皂苷化合物在负离子模式下均可产生[M-H]^(-)、[M-H-C_(6)H_(12)O_(5)]^(-);发现皂苷化合物的母核具有相似的裂解途径,在负离子模式下主要特征碎片离子为m/z 302.26、274.23、256.22。结论:本研究确立了知母中皂苷类化合物的主要裂解规律,为该类化合物的快速检测提供了方法。
Objective:To summarize the fragmentation pathway of saponins in Anemarrhenae Rhizoma by mass spectrometry and explore the fragmentation patterns of saponins in different subtypes.Methods:By UPLC-Q-TOF-MS/MS,the determination was performed on Waters ACQUITY UPLC HSS T3 column with 0.01%formic acid solution-acetonitrile as mobile phase(gradient elution).The mass spectrometric condition included ESI,negative ion mode.This method was used to analyze the mass spectrum information of the total saponins of Anemarrhenae Rhizoma and summarize the fragmentation patterns of these components.According to retention time,accurate molecular weight,and secondary mass spectrometry fragment ion information,combined with the fragmentation pattern of mass spectrometry.Total saponins of Anemarrhenae Rhizoma were quickly identified.Results:A total of 15 saponins and 3 sapogerins were identified in Anemarrhenae Rhizoma.Characteristic fragment ions such as[M-H]-and[M-H-C_(6)H_(12)O_(5)]_(-)were generated from 15 saponins under negative mode in multistage mass spectrometry.It was determined that the parent nucleus of saponins had a similar cleavage pathway,and the main characteristic fragment ions in negative ion mode were m/z 302.26,274.23,256.22.Conclusion:This study established the main fragmentation patterns of saponins in Anemarrhenae Rhizoma,and provided a method for the rapid detection of these compounds.
作者
王晓婷
于颖琦
高慧
WANG Xiao-ting;YU Ying-qi;GAO Hui(School of Pharmacy,Liaoning University of Traditional Chinese Medicine,Dalian 116600,China)
出处
《中华中医药杂志》
CAS
CSCD
北大核心
2022年第5期2593-2597,共5页
China Journal of Traditional Chinese Medicine and Pharmacy
基金
国家自然科学基金项目(No.81102810)
辽宁省自然科学基金项目(No.20180550141)。