An ion mobility-enabled and high-efficiency hybrid scan approach in combination with ultra-high performance liquid chromatography enabling the comprehensive characterization of the multicomponents from Carthamus tinctorius

• Published in: Journal of Chromatography A Vol. 1667; p. 462904
• Main Authors: Qian, Yue-xin, Zhao, Dong-xue, Wang, Hong-da, Sun, He, Xiong, Ying, Xu, Xiao-yan, Hu, Wan-di, Liu, Mei-yu, Chen, Bo-xue, Hu, Ying, Li, Xue, Jiang, Mei-ting, Yang, Wen-zhi, Gao, Xiu-mei
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 29.03.2022
• Subjects: Carthamus tinctorius; Chromatography, High Pressure Liquid - methods; Collision cross section; Hdmse-hddda; Ion-mobility/quadrupole time-of-flight mass spectrometry; Ions; Multicomponent characterization; Reproducibility of Results; Tandem Mass Spectrometry - methods; Carthamus tinctorius; Multicomponent characterization; Collision cross section; Ion-mobility/quadrupole time-of-flight mass spectrometry; Hdmse-hddda
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2022.462904

•A hybrid scan approach of HDMSE-HDDDA was developed.•Streamlined workflows to process the HDMSE and HDDDA data were created.•It could merge the merits of data-independent and data-dependent acquisitions.•141 components were characterized from carthamus tinctorius.•CCS was useful for more reliable characterization of herbal components. Liquid chromatography/mass spectrometry (LC/MS) is extensively applied for the untargeted/targeted analyses of the herbal components, utilizing data-dependent acquisition (DDA) or data-independent acquisition (DIA) to record the fragmentation information useful for the structural elucidation. A new trend recently has emerged by integrating DDA and DIA to render the hybrid scan, which, unfortunately, has rarely been reported. Herein, by using the Vion™ ion-mobility quadrupole time-of-flight mass spectrometer, a hybrid scan strategy (HDMSE-HDDDA) was presented and validated by the untargeted characterization of the multicomponents from Carthamus tinctorius (safflower), in combination with reversed-phase ultra-high performance liquid chromatography (RP-UHPLC). Good chromatographic separation was achieved on an HSS T3 column within 26 min, while HDMSE-MS/MS was used to acquire the collision-induced dissociation MS2 data in the negative mode. Automatic workflows (e.g., data correction, precursors/product ions matching, and peak annotation) were well established on UNIFI™ (incorporating an in-house library recording 261 known compounds) to process the obtained MS2 data. Compared with single DDA or DIA, the hybrid approach of HDMSE-HDDDA better balanced between the coverage and reliability, led to high-definition MS spectra, offered useful collision cross section (CCS) information, and showed satisfactory identification performance comparable to MSE. A total of 141 components (involving 41 quinochalcones, 66 flavanols/flavones, 11 flavanones, 6 organic acids, 1 polyacetylene, and 16 others) were characterized from safflower. Moreover, CCS prediction could assist isomers characterization, to some extent. Conclusively, this hybrid scan approach enables a dimension-enhanced MS data acquisition strategy providing the complementary structural information, which more suits the chemical characterization of complex samples.