摘要
目的:运用UHPLC-Q-Exactive-Orbitrap HRMS技术分析鉴定肾衰乙方的化学成分,以及大鼠灌胃后主要入血、组织原型成分分布.方法:采用Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以0.1％甲酸水溶液(A)-甲醇(B)为流动相体系,梯度洗脱分离.质谱采用正负离子一级全扫描/数据依赖二级扫描模式(Full MS/dd-MS2)采集数据,经Xcali-bur4.2软件获取色谱保留时间以及准分子离子碎片信息,通过对照品比对、文献参考以及自建数据库等成分检测信息,实现对肾衰乙方化学成分及入血、组织原型成分的鉴定.结果:共鉴定出166种化学成分,包括黄酮类56种、皂苷类25种、蒽醌类24种、有机(酚)酸类23种、苯酞类14种、生物碱和环肽类各7种、木脂素类和香豆素类各3种以及其他类4种.大鼠口服肾衰乙方后分别从血清、心、肝、脾、肺、肾、脑、睾丸中检测到54、53、61、47、71、48、53、42种原型成分.结论:该研究利用高分辨质谱技术完成了肾衰乙方化学成分及主要入血、组织移行成分的快速鉴定,可为肾衰乙方效应物质的解析及作用机制研究提供参考.
Abstract
OBJECTIVE To employ UHPLC-Q-Exactive-Orbitrap HRMS to identify the chemical components of Shensh-uai Yifang and explore the distribution of major components in blood and tissues after oral dosing in rats.METHODS An Acquity UPLC BEH C18 chromatographic column(100 mm×2.1 mm,1.7 μm)was utilized as solid phase while mobile phase composed of 0.1％formic acid(A)and methanol(B)with gradient elution.Mass spectra were collected with a Full scan of posi-tive and negative ions/data-dependent on secondary scan function(Full MS/dd-MS2)for data collection.Chromatographic reten-tion time and quasi-molecular ion fragment information were acquired by Xcalibur 4.2 software while identification of components was compared with reference standards,literature reference and self-established database.RESULTS A total of 166 chemical components were identified from Shenshuai Yifang,including 56 kinds of flavonoids,25 kinds of saponins,24 kinds of anthraqui-nones,23 kinds of organic and phenolic acids,14 kinds of phthalides,7 kinds of cyclic peptides and alkaloids,3 kinds of lignans and coumarins and 4 kinds of others.After oral dosing of Shenshuai Yifang to rats,54,53,61,47,71,48,53,42 prototypic components were detected in sera,heart,liver,spleen,lung,kidney,brain and testicles respectively.CONCLUSION In this study,the chemical components and major blood/tissue distribution components of Shenshuai Yifang,have been rapidly identified by high-resolution mass spectrometry.It may provide references for analyzing effective substances and elucidating the action mechanism of Shenshuai Yifang.
基金项目
浦东新区卫生健康委员会卫生计生科研项目(PW2022D-12)
浦东新区中医专病品牌倍增计划(PDZY-2021-0302)
何立群名中医工作室建设(PDZY-2022-0703)
NETL
NSTL
万方数据