Rapid Analysis and Identification of Chemical Constituents from Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS / 中国实验方剂学杂志

ABSTRACT

Objective::To rapidly characterize and identify the components of Siwei Tumuxiang San by using high performance liquid chromatography tandem quadrupole-electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q-Exactive-MS/MS). Method::Agilent ZORBAX SB-Aq column (4.6 mm×150 mm, 5 μm) was adopted and 5 mmol·L-1 ammonium acetate+ 0.1% formic acid aqueous solution-acetonitrile were used as mobile phase. According to the separation and structure identification results of chemical components based on the methods of ChemSpider and ChemicalBook database retrieval, a local database of molecular formula, molecular weight, structural formula and MS/MS spectrum information of chemical components in Siwei Tumuxiang San was established. An HPLC-Q-Exactive-MS/MS analysis method was established. The complex compounds of Siwei Tumuxiang San were identified rapidly by using Xcalibar 3.0 software, comparison of reference materials and studies on MS/MS fragment pathways. Result::A total of 110 compounds were identified from the Siwei Tumuxiang San by HPLC-Q-Exactive-MS/MS technology, including 3 sesquiterpene compounds from Inulae Radix, 16 alkaloid compunds and 38 isoprene flavonoid compounds from Sophorae Radix flavescentis, 12 triterpenoid saponin compounds, 1 catechin compounds and 4 flavonoid glycoside compounds from Rubus sachalinensis. The fragment pathways of the main types of compounds were summarized. Among them, mass spectrometry information of 31 compounds was reported for the first time. Conclusion::This study can be used to identify the target compounds and non-target compounds in Siwei Tumuxiang San systematically, accurately and quickly, which will lay a foundation for the in vivo analysis and pharmacokinetic study of the formulation.