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Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF).
J Nat Prod 2007; 70(9):1424-8JN

Abstract

Silychristins A (1) and B (2), silydianin (3), silybins A (4) and B (5), and isosilybins A (6) and B (7) are major bioactive flavonolignans in silymarin, a herbal remedy derived from the milk thistle Silybum marianum. In this study, the seven major active flavonolignans including the diastereomers 1/ 2, 4/ 5, and 6/ 7 were completely separated using semi-micro-high performance liquid chromatography (HPLC) with a Nucleosil 100-3 C 18 HD column and a MeOH/water/formic acid mobile phase system. The collision-induced dissociation (CID) MS/MS and MS (3) spectra of these flavonolignans were studied systematically using hybrid ion-trap and time-of-flight (IT-TOF) mass spectrometry. Efficient differentiation between the seven flavonolignans (1- 7) was possible based on comparison of the resultant CID-MS/MS or MS (3) spectra. Each characteristic MS/MS or MS (3) fragmentation pattern was elucidated with high-resolution mass spectra by IT-TOF. The results with the present methodology show that liquid chromatography-mass spectrometry IT-TOF (LC-MS/IT-TOF) can be useful for general screening of active natural products from plant extracts and for the specific quality control of silymarin.

Authors+Show Affiliations

Natural Products Research Laboratories, School of Pharmacy, University of North Carolina, Chapel Hill, North Carolina 27599-7360, USA.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, N.I.H., Extramural

Language

eng

PubMed ID

17764149

Citation

Shibano, Makio, et al. "Separation and Characterization of Active Flavonolignans of Silybum Marianum By Liquid Chromatography Connected With Hybrid Ion-trap and Time-of-flight Mass Spectrometry (LC-MS/IT-TOF)." Journal of Natural Products, vol. 70, no. 9, 2007, pp. 1424-8.
Shibano M, Lin AS, Itokawa H, et al. Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF). J Nat Prod. 2007;70(9):1424-8.
Shibano, M., Lin, A. S., Itokawa, H., & Lee, K. H. (2007). Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF). Journal of Natural Products, 70(9), pp. 1424-8.
Shibano M, et al. Separation and Characterization of Active Flavonolignans of Silybum Marianum By Liquid Chromatography Connected With Hybrid Ion-trap and Time-of-flight Mass Spectrometry (LC-MS/IT-TOF). J Nat Prod. 2007;70(9):1424-8. PubMed PMID: 17764149.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF). AU - Shibano,Makio, AU - Lin,An-Shen, AU - Itokawa,Hideji, AU - Lee,Kuo-Hsiung, Y1 - 2007/09/01/ PY - 2007/9/4/pubmed PY - 2007/12/6/medline PY - 2007/9/4/entrez SP - 1424 EP - 8 JF - Journal of natural products JO - J. Nat. Prod. VL - 70 IS - 9 N2 - Silychristins A (1) and B (2), silydianin (3), silybins A (4) and B (5), and isosilybins A (6) and B (7) are major bioactive flavonolignans in silymarin, a herbal remedy derived from the milk thistle Silybum marianum. In this study, the seven major active flavonolignans including the diastereomers 1/ 2, 4/ 5, and 6/ 7 were completely separated using semi-micro-high performance liquid chromatography (HPLC) with a Nucleosil 100-3 C 18 HD column and a MeOH/water/formic acid mobile phase system. The collision-induced dissociation (CID) MS/MS and MS (3) spectra of these flavonolignans were studied systematically using hybrid ion-trap and time-of-flight (IT-TOF) mass spectrometry. Efficient differentiation between the seven flavonolignans (1- 7) was possible based on comparison of the resultant CID-MS/MS or MS (3) spectra. Each characteristic MS/MS or MS (3) fragmentation pattern was elucidated with high-resolution mass spectra by IT-TOF. The results with the present methodology show that liquid chromatography-mass spectrometry IT-TOF (LC-MS/IT-TOF) can be useful for general screening of active natural products from plant extracts and for the specific quality control of silymarin. SN - 0163-3864 UR - https://www.unboundmedicine.com/medline/citation/17764149/Separation_and_characterization_of_active_flavonolignans_of_Silybum_marianum_by_liquid_chromatography_connected_with_hybrid_ion_trap_and_time_of_flight_mass_spectrometry__LC_MS/IT_TOF__ L2 - https://dx.doi.org/10.1021/np070136b DB - PRIME DP - Unbound Medicine ER -