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. 2021 Oct 16:12:100143.
doi: 10.1016/j.fochx.2021.100143. eCollection 2021 Dec 30.

Chemical characterization of flavonoids and alkaloids in safflower (Carthamus tinctorius L.) by comprehensive two-dimensional hydrophilic interaction chromatography coupled with hybrid linear ion trap Orbitrap mass spectrometry

Songsong Wang  1 , Jiliang Cao  2 , Jiagang Deng  3 , Xiaotao Hou  3 , Erwei Hao  3 , Lei Zhang  4 , Hua Yu  1 , Peng Li  1
Affiliations

Chemical characterization of flavonoids and alkaloids in safflower (Carthamus tinctorius L.) by comprehensive two-dimensional hydrophilic interaction chromatography coupled with hybrid linear ion trap Orbitrap mass spectrometry

Songsong Wang et al. Food Chem X. .

Abstract

Safflower (Carthamus tinctorius L.) is a famous food additive and herbal medicine in China. In the present research, an online comprehensive two-dimensional hydrophilic interaction chromatography coupled to a diode array detector and a hybrid linear ion trap-Orbitrap mass spectrometry (HILIC × HILIC-DAD-ESI/HRMS/MS n ) platform was developed to analyze the flavonoids and alkaloids in safflower. By combining with an XBridge Amide column (150 mm × 4.6 mm, 3.5 μm) and an Ultimate amide column (50 mm × 4.6 mm, 5 μm), the system orthogonality reached 88% and a total of 231 peaks were detected. Altogether 93 compounds, including 75 flavonoids and their glycosides and 10 alkaloids were unambiguously or tentatively identified in both negative and positive ion modes, using accurate mass and MS fragment data. Among them, 5 compounds were discovered and reported from safflower for the first time. The established HILIC × HILIC platform should be a powerful tool for the separation and characterization of complicated matrices in natural herbs.

Keywords: Alkaloids; Carthamus tinctorius L; Flavonoids; LTQ-Orbitrap mass spectrometry; Online HILIC×HILIC.

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Conflict of interest statement

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Figures

None
Graphical abstract
Fig. 1
Fig. 1
The chemical structures of the 14 reference compounds.
Fig. 2
Fig. 2
2D-TIC contour plots of different 2D-LC systems for separation of 14 reference compounds standards. (A) Combination of HILIC with Hypersil gold PFP column, (B) Combination of HILIC with Accucore Polar Premium column, (C) Combination of HILIC with Accucore Polar Premium column configured with online dilution module.
Fig. 3
Fig. 3
(A) The separation of safflower sample on 2D-TIC contour plots by using the optimal online HILIC × HILIC-ESI/HRMS/MSn system, (B) The separation comparison of 1D-HILIC and HILIC × HILIC in safflower.
Fig. 4
Fig. 4
The MS/MS spectra and proposed fragmentation pathway for compound 2 (A), and the MS/MS spectra and proposed fragmentation pathway for compound 25 (B) and 61 (D), and compound 65 under positive ion mode (C) and negative ion mode (E).
Fig. 5
Fig. 5
The MS/MS/MS spectra and proposed fragmentation pattern for compound 63 under positive ion mode (A, B) and negative ion mode (C).
Fig. 6
Fig. 6
The MSn spectra and proposed fragmentation pattern for compound 74 under positive ion mode (A, B) and negative ion mode (C).
See this image and copyright information in PMC

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