蒌芍痉挛平颗粒的血清药物化学研究

Analysis of the pharmacodynamic constituents in Loushaojingluanping Granules by serum pharmacochemistry

目的对蒌芍痉挛平颗粒进行血清药物化学成分研究,研究其入血成分。方法通过建立超高效液相串联飞行时间质谱法(UPLC-Q-TOF-MS)快速鉴定蒌芍痉挛平颗粒经大鼠灌胃给药后吸收入血的化学成分。超高效液相串联飞行时间质谱法采用Waters CORTECS C_(18)色谱柱(2.1 mm×100 mm,1.6μm),以乙腈-0.1%甲酸水为流动相进行梯度洗脱,对大鼠灌胃蒌芍痉挛平颗粒后的含药血清进行负离子模式一级分子离子和二级子离子扫描,鉴定血中移行成分。结果通过比较色谱峰保留时间、对照品或文献质谱一级、二级信息、质谱裂解方式,共鉴定了蒌芍痉挛平颗粒35个吸收入血成分,主要包括单萜苷类、黄酮类、酚酸类、皂苷类等。结论建立的超高效液相串联飞行时间质谱法鉴定蒌芍痉挛平颗粒血清药物化学成分的分析方法简便、快速、准确,为揭示院内制剂蒌芍痉挛平颗粒对体内药效物质基础与制剂开发奠定基础。

Objective To study the serum pharmacochemistry of Loushaojingluanping Granules(LSJRPG)and its components into blood.Methods An utra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS)method was developed for the analysis of the absorbed components in serum after intragastric administration(i.g.)of LSJRPG to rats.The separation was achieved on a Waters CORTECS C_(18) column by gradient elution with acetonitrile-aqueous solution(containing 0.1%formic acid)as mobile phase.The serum sample after i.g.LSJRPG to rats,the ion acquisition was performed by full scan MS and MS/MS in negative ion mode by HPLC-Q-TOF-MS.Results 35 prototype compounds including monoterpene glycosides,flavonoids,phenolic acids,saponins and others were identified in serum by comparing the retention time,mass spectrometry MS1,MS2 and fragmentation characteristics with reference standards or literatures.Conclusion The UPLC-Q-TOF-MS method was simple,rapid and accurate for the qualitative of serum chemical constituents in LSJRPG to reveal the hospital preparation LSJRPG on the body pharmacodynamic material basis and lay a foundation for the development and utilization of preparation.