An enhanced targeted identification strategy for the selective identification of flavonoid O-glycosides from Carthamus tinctorius by integrating offline two-dimensional liquid chromatography/linear ion-trap-Orbitrap mass spectrometry, high-resolution diagnostic product ions/neutral loss filtering and liquid chromatography-solid phase extraction-nuclear magnetic resonance

doi:10.1016/j.chroma.2017.02.041

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	An enhanced targeted identification strategy for the selective identification of flavonoid O-glycosides from Carthamus tinctorius by integrating offline two-dimensional liquid chromatography/linear ion-trap-Orbitrap mass spectrometry, high-resolution diagnostic product ions/neutral loss filtering and liquid chromatography-solid phase extraction-nuclear magnetic resonance
	Yao, Chang-liang 1,2; Yang, Wen-zhi 1; Si, Wei 1; Shen, Yao 1; Zhang, Nai-xia3 ; Chen, Hua-li 3; Pan, Hui-qin 1,2; Yang, Min 1; Wu, Wan-ying1 ; Guo, De-an1
刊名	JOURNAL OF CHROMATOGRAPHY A
	2017-03-31
卷号	1491 页码:87-97
关键词	Enhanced targeted identification strategy Offline two-dimensional liquid chromatography Diagnostic product ions filtering Liquid chromatography-solid phase extraction-nuclear magnetic resonance Carthamus tinctorius Flavonoid O-glycoside
ISSN号	0021-9673
DOI	10.1016/j.chroma.2017.02.041
文献子类	Article
英文摘要	Targeted identification of potentially bioactive molecules from herbal medicines is often stymied by the insufficient chromatographic separation, ubiquitous matrix interference, and pervasive isomerism. An enhanced targeted identification strategy is presented and validated by the selective identification of flavonoid O-glycosides (FOGs) from Carthamus tinctorius. It consists of four steps: (i) enhanced separation and detection by offline two-dimensional liquid chromatography/LTQ-Orbitrap MS (offline 2D-LC/LTQ-Orbitrap MS) using collision-induced dissociation (CID) and high-energy C-trap dissociation (HCD); (ii) improved identification of the major aglycones by acid hydrolysis and LC-SPE-NMR; (iii) simplified spectral elucidation by high-resolution diagnostic product ions/neutral loss filtering; and (iv) more convincing structural identification by matching an in-house library. An offline 2D-LC system configuring an Acchrom XAmide column and a BEH Shield RP-18 UPLC column enabled much better separation of the easily co-eluting components. Combined use of CID and HCD could produce complementary fragmentation information. The intensity ratios of the aglycone ion species ([Y-0-H]-/Y-0-and [Y-0-2H] (-)/Y-0(-)) in the HCD-MS2 spectra were found diagnostic for discriminating the aglycone subtypes and characterizing the glycosylation patterns. Five aglycone structures (kaempferol, 6-hydroxykaempferol, 6-methoxykaempferol, carthamidin, and isocarthamidin) were identified based on the H-1-NMR data recorded by LC-SPE-NMR. Of the 107 characterized flavonoids, 80 FOGs were first reported from C. tinctorius. Unknown aglycones, pentose, and novel acyl substituents were discovered. A new compound thereof was isolated and fully identified, which could partially validate the MS-oriented identification. This integral strategy can improve the potency, efficiency, and accuracy in the detection of new compounds from medicinal herbs and other natural sources. (C) 2017 Elsevier B.V. All rights reserved.
资助项目	National Natural Science Foundation of China[81503240]
WOS关键词	TRADITIONAL CHINESE MEDICINE ; COLLISION-INDUCED DISSOCIATION ; QUINOCHALCONE C-GLYCOSIDES ; PANAX-GINSENG ; COMPREHENSIVE CHARACTERIZATION ; COLUMN CHROMATOGRAPHY ; EFFICIENT DISCOVERY ; NATURAL COMPOUNDS ; CONSTITUENTS ; GINSENOSIDES
WOS研究方向	Biochemistry & Molecular Biology ; Chemistry
语种	英语
出版者	ELSEVIER SCIENCE BV
WOS记录号	WOS:000397375700010
内容类型	期刊论文
源URL	[http://119.78.100.183/handle/2S10ELR8/272733]
专题	上海中药现代化研究中心
通讯作者	Wu, Wan-ying; Guo, De-an
作者单位	1.Chinese Acad Sci, Shanghai Inst Mat Med, Shanghai Res Ctr Modernizat Tradit Chinese Med, Natl Engn Lab TCM Standardizat Technol, 501 Haike Rd, Shanghai 201203, Peoples R China; 2.Univ Chinese Acad Sci, 19A Yuquan Rd, Beijing 100049, Peoples R China; 3.Chinese Acad Sci, Shanghai Inst Mat Med Chinese, Dept Analyt Chem, Shanghai 201203, Peoples R China
推荐引用方式 GB/T 7714	Yao, Chang-liang,Yang, Wen-zhi,Si, Wei,et al. An enhanced targeted identification strategy for the selective identification of flavonoid O-glycosides from Carthamus tinctorius by integrating offline two-dimensional liquid chromatography/linear ion-trap-Orbitrap mass spectrometry, high-resolution diagnostic product ions/neutral loss filtering and liquid chromatography-solid phase extraction-nuclear magnetic resonance[J]. JOURNAL OF CHROMATOGRAPHY A,2017,1491:87-97.
APA	Yao, Chang-liang.,Yang, Wen-zhi.,Si, Wei.,Shen, Yao.,Zhang, Nai-xia.,...&Guo, De-an.(2017).An enhanced targeted identification strategy for the selective identification of flavonoid O-glycosides from Carthamus tinctorius by integrating offline two-dimensional liquid chromatography/linear ion-trap-Orbitrap mass spectrometry, high-resolution diagnostic product ions/neutral loss filtering and liquid chromatography-solid phase extraction-nuclear magnetic resonance.JOURNAL OF CHROMATOGRAPHY A,1491,87-97.
MLA	Yao, Chang-liang,et al."An enhanced targeted identification strategy for the selective identification of flavonoid O-glycosides from Carthamus tinctorius by integrating offline two-dimensional liquid chromatography/linear ion-trap-Orbitrap mass spectrometry, high-resolution diagnostic product ions/neutral loss filtering and liquid chromatography-solid phase extraction-nuclear magnetic resonance".JOURNAL OF CHROMATOGRAPHY A 1491(2017):87-97.