UPLC-Triple-TOF-MS/MS快速鉴定豨桐制剂的化学成分

Rapid Identification of Chemical Components in Xitong Preparations by UPLC-Triple-TOF-MS/MS

关键词:  豨桐制剂  超高压液相色谱串联四极杆飞行时间质谱法  苯丙素  萜类  黄酮类  脂氧化物

Key words:  Xitong prepration  UPLC-Triple-TOF-MS/MS  phenylpropanoids  terpenes  flavonoids  oxylipins

摘要:

目的 建立超高压液相色谱串联四极杆飞行时间质谱法快速分析抗类风湿性关节炎中药复方豨桐制剂中的化学成分。方法 采用ACQUITY UPLC HSS T3(2.1 mm×150 mm，1.8 μm)色谱柱，以0.1%甲酸水溶液(A)-0.1%甲酸乙腈(B)作为流动相梯度洗脱，流速为0.3 mL·min^-1，分别在正离子、负离子模式下进行检测，采用Peakview 软件结合药材化合物数据库进行分析；根据获得的精确相对分子量，结合与对照品比对、二级质谱特征碎片以及文献报道确定化学成分。结果 推测鉴定了78个化学成分，包括苯丙素类20个，萜类33个，黄酮类19个，脂氧化物6个，其中2个可能为新化合物。结论 该方法可以全面快速地鉴定豨桐制剂中的化学成分，为豨桐丸、豨桐胶囊的质量控制和药效物质基础研究提供参考。

Abstract:

OBJECTIVE To establish a rapid analytical method to identify the chemical components in Xitong preparations for the treatment of rheumatoid arthritis by ultra-high performance liquid chromatography coupled triple time-of-flight mass spectrometry(UPLC-Triple-TOF-MS/MS). METHODS The analysis was performed on an ACQUITY UPLC HSS T3 (2.1 mm×150 mm, 1.8 μm) column with the mobile phase consisting of water containing 0.1% formic acid(A) and acetonitrile containing 0.1% formic acid(B) in gradient mode at a flow rate of 0.3 mL·min^-1. Data acquisition was carried out under positive and negative ion modes. The processed data was analyzed by Peakview software and compound database. The chemical components were determined by comparison with standard products, combining with the characteristic fragments in secondary MS, and those in the related literatures. RESULTS Seventy-eight compounds were identified including 20 phenylpropanoids, 33 terpenes, 19 flavonoids, 6 oxylipins, two of which might be new compounds. CONCLUSION The method can be used for rapid identification of chemical compositions in Xitong preparations, which provides basis for quality control and elucidation of phamarcodynamic material basis of Xitong pills and capsules .