摘要
运用超高效液相色谱-四极杆-静电场轨道阱质谱(UPLC-Q-Exactive-Orbitrap-MS)技术及超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)对小柴胡颗粒化学成分及大鼠口服后的入血成分进行鉴定。采用CORTECS UPLC C^(+)_(18)色谱柱(2.1 mm×100 mm,1.6μm),乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,在电喷雾离子源正、负离子模式下采集数据后与对照品比较保留时间、精确相对分子质量、二级离子碎片以及参照相关文献进行化学成分鉴别;通过皮下注射干酵母建立大鼠发热模型后,灌胃给予正常组及模型组大鼠小柴胡颗粒,给药后于不同时间点眼眶静脉取血,分离血浆,在多反应监测模式(MRM)下进行扫描鉴定入血成分。从小柴胡颗粒中共初步鉴定出112种化学成分,包括63种黄酮类、31种皂苷类、6种有机酸类、4种苯丙素类、3种氨基酸类以及5种其他类化合物;从血浆中鉴定得到18个入血原型成分。该研究鉴定了小柴胡颗粒化学成分及入血成分,为进一步的药效物质基础及质量控制研究奠定了基础。
The chemical components of Xiaochaihu Granules and absorbed components in rats after oral administration were identified by using ultra performance liquid chromatography-quadrupole orbitrap mass spectrometry(UPLC-Q-Exactive-Orbitrap-MS)and UPLC-triple quadrupole mass spectrometry(UPLC-MS/MS).Separation was performed on a CORTECS UPLC C^(+)_(18)(2.1 mm×100 mm,1.6μm)column with gradient elution using acetonitrile-0.1%formic acid aqueous solution as the mobile phase.Data on the chemical components were collected in positive and negative ion modes and identified based on the retention time,precise molecular weight,fragment ion information in comparison with the reference substance,and literature report.The rat fever model was established by subcutaneous injection of dry yeast.Subsequently,the normal and model rats received oral administration of Xiaochaihu Granules.Blood samples were taken from the orbital vein at different time points after administration,and the plasma was isolated for scanning and identification of absorbed components using the multi reaction monitoring mode(MRM).A total of 112 chemical components were identified in Xiaochaihu Granules,including 63 flavonoids,31 saponins,6 organic acids,4 phenylpropanoids,3 amino acids and 5 other compounds.Additionally,18 prototypical components were identified in rat plasma.This study lays the foundation for further study of the therapeutic material and quality control of Xiaochaihu Granules.
作者
刘晓丽
欧沛思
林爱华
刘奕明
LIU Xiao-li;OU Pei-si;LIN Ai-hua;LIU Yi-ming(the Second Clinical Medical College,Guangzhou University of Chinese Medicine,Guangzhou 510006,China;Zhuhai Hospital,the Second Afiliated Hospital of Guangzhou University of Chinese Medicine,Zhuhai 519000,China;Guangdong Provincial Key Laboratory of Clinical Research on Traditional Chinese Medicine Syndrome,Guangzhou 510120,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2024年第15期4078-4090,共13页
China Journal of Chinese Materia Medica
基金
广州市科技计划项目(202206010112)
广东省科技计划项目(2023B1212060063)。
作者简介
刘晓丽,硕士研究生,E-mail:liuxiaoli2023@163.com;通信作者:刘奕明,研究员,博士生导师,主要从事中药临床药理与药代动力学研究,E-mail:lyming2000@163.com。
