超高效液相色谱-四级杆飞行时间串联质谱快速分析复方守宫散化学成分及血中移行成分

目的 采用超高效液相色谱-四级杆飞行时间质谱(ultra-performance liquid chromatogra-phy/quadrupole time-of-flight-tandem mass spectrometry,UPLC-Q-TOF/MS)对复方守宫散中化学成分及其血中移行成分进行定性分析,为该制剂的体内有效物质研究提供参考.方法 采用沃特世超高效液相色谱仪(ACQUITY UPLC)和沃特世高分辨质谱仪(Waters Synapt G2-Si QTOF)获得复方守宫散原药样品溶液、混合对照品溶液、空白血浆和含药血浆的液相色谱-质谱信息,再通过比对UNIFI(沃特世科学信息平台)质谱数据库中化合物信息以及部分对照品的提取离子流色谱图、质谱碎片裂解信息,鉴定出目标化合物.结果 共识别出复方守宫散中77个化学成分(主要有皂苷类25个、黄酮类13个、醌类12个),采用对照品对其中6个成分进行了验证;通过比对空白血浆和含药血浆,发现复方守宫散中绿原酸、槲皮素、虎杖苷、人参皂苷Re等27个成分为入血成分.结论 具有高分辨率、高灵敏度的UPLC-QTOF/MS能够快速分析复方守宫散化学成分及其血中移行成分.

Rapid Determination of Chemical Components of Compound Shougong Powder and Its Transitional Components in Blood by Ultra-performance Liquid Chromatography/Quadrupole Time-of-flight Tandem Mass Spectrometry

Objective To qualitatively analyze the chemical components of Compound Shougong Powder and its transitional components in blood by ultra-performance liquid chromatography/quadrupole time-of-flight tandem mass spectrometry (UPLC-QTOF/MS), and to provide a reference for research on pharmacodynamic substances of the preparation in vivo. Methods The Waters HPLC instrument (ACQUITY UPLC) and the Waters high-resolution mass spectrometer (Waters Synapt G2-Si QTOF) were used to obtain the liquid chromatography-mass spectrometry information of Compound Shougong Powder sample solution, mixed reference solution, blank plasma, and medicated plasma. The compound information in self-built database and UNIFI (Waters scientific information platform) mass spectrometry database was compared, as well as the extracted ion flow chromatogram and mass spectrometry fragment cleavage information of some reference substances, and then the target compounds were identified. Results A total of 77 chemical components of Compound Shougong Powder were identified, mainly including 25 saponins, 13 flavonoids, and 12 quinones, among which 6 components were verified by reference substance. Comparison of blank plasma and medicated plasma showed that 27 components in Compound Shougong Powder were the transitional components in blood, such as chlorogenic acid, quercetin, polydatin, and ginsenoside Re. Conclusion UPLC-QTOF/MS with high resolution and sensitivity can rapidly analyze the chemical components of Compound Shougong Powder and its transitional components in blood.