Dimension-Enhanced Ultra-High Performance Liquid Chromatography/Ion Mobility-Quadrupole Time-of-Flight Mass Spectrometry Combined with Intelligent Peak Annotation for the Rapid Characterization of the Multiple Components from Seeds of Descurainia sophia

Abstract

The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components. The seeds of Descurainia sophia (SDS) are utilized in China as a cough and asthma relieving agent. Herein, a dimension-enhanced integral approach, by combining ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry (UHPLC/IM-QTOF-MS) and intelligent peak annotation, was developed to rapidly characterize the multicomponents from SDS. Good chromatographic separation was achieved within 38 min on a UPLC CSH C18 (2.1 × 100 mm, 1.7 μm) column which was eluted by 0.1% formic acid in water (water phase) and acetonitrile (organic phase). Collision-induced dissociation-MS² data were acquired by the data-independent high-definition MS^E (HDMS^E) in both the negative and positive electrospray ionization modes. A major components knockout strategy was applied to improve the characterization of those minor ingredients by enhancing the injection volume. Moreover, a self-built chemistry library was established, which could be matched by the UNIFI software enabling automatic peak annotation of the obtained HDMS^E data. As a result of applying the intelligent peak annotation workflows and further confirmation process, a total of 53 compounds were identified or tentatively characterized from the SDS, including 29 flavonoids, one uridine derivative, four glucosides, one lignin, one phenolic compound, and 17 others. Notably, four-dimensional information related to the structure (e.g., retention time, collision cross section, MS¹ and MS² data) was obtained for each component by the developed integral approach, and the results would greatly benefit the quality control of SDS.

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