基于UHPLC-Q-Exactive Orbitrap-MS技术分析桂附地黄丸的化学成分及入血成分  

Chemical constituents of Guifu Dihuang pills and absorbed components in the plasma based on UHPLC-Q-Exactive Orbitrap-MS technology

作　　者：刘爽 戴宇滢 赵爽同 陈晴 魏苗苗 周昌燕 高金薇 LIU Shuang;DAI Yu-ying;ZHAO Shuang-tong;CHEN Qing;WEI Miao-miao;ZHOU Chang-yan;GAO Jin-wei(School of Pharmacy,Shenyang Medical College,Shenyang 110034;College of Dentistry,Shenyang Medical College,Shenyang 110034)

机构地区：[1]沈阳医学院药学院,沈阳110034 [2]沈阳医学院口腔学院,沈阳110034

出　　处：《中南药学》2023年第8期2069-2075,共7页Central South Pharmacy

基　　金：沈阳医学院大学生科研课题(No.20219042);沈阳医学院博士科研启动基金(No.20205045)。

摘　　要：目的采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱联用技术(UHPLC-QExactive Orbitrap-MS)对该复方的体外化学成分谱及入血成分进行研究。方法利用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸水溶液(A)-0.1%甲酸乙腈(B)为流动相进行梯度洗脱(0~1 min,1%B;1~10 min,1%~99%B;10~11.5 min,99%B;11.5~11.6 min,99%~1%B;11.6~13.5 min,1%B),流速为0.4 mL·min^(-1),在电喷雾离子源(ESI)下,以正、负离子模式采集数据。运用Xcalibur software软件,根据化合物保留时间、准分子离子峰和二级质谱信息,结合对照品及文献报道,对该复方的化学成分及入血成分进行解析。结果在桂附地黄丸体外样品中共鉴定出85个化学成分,包括生物碱类11个、环烯醚萜苷类14个、苯乙醇苷类9个、单萜苷类11个、三萜类14个、酚酸类9个、有机酸/醛6个、糖苷类5个、其他类6个,并对化学成分进行药材来源归属;共表征了大鼠血浆中的化合物22个,包括14个原形药物和8个代谢物。结论所建立的方法能高效、灵敏地分析桂附地黄丸中的体外化学成分和入血成分,初步阐明了该复方的体外化学成分轮廓及血中移行成分,为其体内的药效物质基础和作用机制研究奠定基础。Objective To determine the chemical constituents spectrum of Guifu Dihuang pills and absorbed components in the plasma by UHPLC-Q-Exactive Orbitrap-MS technology.Methods Gradient elution was performed on an ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm)with 0.1%formic acid in water(A)to 0.1%formic acid in acetonitrile(B)as the mobile phase(0~1 min,1%B;1~10 min,1%~99%B;10~11.5 min,99%B;11.5~11.6 min,99%~1%B;11.6~13.5 min,1%B)and the flow rate at 0.4 mL·min-1.The data were collected in the positive and negative ion mode under the electrospray ion source.The chemical constituents and absorbed components in the plasma were analyzed by Xcalibur software according to the retention time,excimer ion peak and secondary mass spectrum,in combination with the reference substance and literature reports.Results Totally 85 chemical components were identified in Guifu Dihuang pills,including 11 alkaloids,14 iridoid glycosides,9 phenylethanolic glycosides,11 monoterpene glycosides,14 triterpenes,9 phenolic acids,6 organic acids/aldehydes,5 glycosides and 6 other types.Totally 22 chemical constituents were identified in the rat plasma after the intragastric administration,including 14 prototype constituents and 8 metabolites.Conclusion The established method can efficiently analyze the chemical constituents and absorbed components in the plasma in Guifu Dihuang pills and elucidate the contour of the chemical components in vitro in the compound prescription and constituents absorbed into the blood,which lays a foundation for the study of the material basis and mechanism of its in vivo efficacy.

关 键 词：桂附地黄丸 UHPLC-Q-Exactive Orbitrap-MS 化学成分 入血成分 

分 类 号：R284.1[医药卫生—中药学]