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Optimization of a liquid chromatography method based on simultaneous electrospray ionization mass spectrometric and ultraviolet photodiode array detection for analysis of flavonoid glycosides.
Rapid Commun Mass Spectrom. 2002; 16(24):2341-8.RC

Abstract

Different reversed-phase liquid chromatography (LC) columns of conventional dimensions were coupled to an ultraviolet photodiode array detector (UV-DAD) and a magnetic sector-type spectrometer, equipped with an electrospray ionization (ESI) source, by a laboratory-made flow splitter. A mixture of three flavonoid-O-glycosides was employed to examine the effects of the solvent composition, the flow rate, the stationary phase, the pH and the organic acid added, on the chromatographic separation, the UV-DAD detection, the ESI process and the entire LC system with ESI-MS and UV-DAD detection. In the positive ion mode, methanol containing 1% acetic acid was by far the most sensitive in ESI-MS analysis, whereas an acetonitrile/water mobile phase containing 0.5% formic acid was proved to give the best sensitivity in LC/ESI-MS/UV-DAD analysis. In the negative ion mode, the highest sensitivity was obtained with a mobile phase containing 0.1% formic acid, while addition of bases decreased the sensititvity. The optimal flow rate was higher in negative ESI (20-50 micro L/min) than in positive ESI (5 micro L/min), and the percentage of organic phase had an influence on the sensitivity of ESI-MS detection. With regard to the selection of a suitable C(18) reversed-phase LC column, a column which is well end-capped is to be preferred, because residual silanol groups appear to impair the separation of flavonoid glycosides. The optimized LC/ESI-MS/UV-DAD method was applied to a commercial Crataegus extract, which is used in phytomedicine to treat cardiovascular problems and is known to be rich in flavonoids. It is demonstrated how UV spectra and first-order ESI mass spectra allow a fast characterization of flavonoids, even if reference compounds are not available or at hand.

Authors+Show Affiliations

University of Antwerp (UIA), Department of Pharmaceutical Sciences, Universiteitsplein 1, 2610 Antwerp, Belgium.No affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

12478580

Citation

Cuyckens, Filip, and Magda Claeys. "Optimization of a Liquid Chromatography Method Based On Simultaneous Electrospray Ionization Mass Spectrometric and Ultraviolet Photodiode Array Detection for Analysis of Flavonoid Glycosides." Rapid Communications in Mass Spectrometry : RCM, vol. 16, no. 24, 2002, pp. 2341-8.
Cuyckens F, Claeys M. Optimization of a liquid chromatography method based on simultaneous electrospray ionization mass spectrometric and ultraviolet photodiode array detection for analysis of flavonoid glycosides. Rapid Commun Mass Spectrom. 2002;16(24):2341-8.
Cuyckens, F., & Claeys, M. (2002). Optimization of a liquid chromatography method based on simultaneous electrospray ionization mass spectrometric and ultraviolet photodiode array detection for analysis of flavonoid glycosides. Rapid Communications in Mass Spectrometry : RCM, 16(24), 2341-8.
Cuyckens F, Claeys M. Optimization of a Liquid Chromatography Method Based On Simultaneous Electrospray Ionization Mass Spectrometric and Ultraviolet Photodiode Array Detection for Analysis of Flavonoid Glycosides. Rapid Commun Mass Spectrom. 2002;16(24):2341-8. PubMed PMID: 12478580.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Optimization of a liquid chromatography method based on simultaneous electrospray ionization mass spectrometric and ultraviolet photodiode array detection for analysis of flavonoid glycosides. AU - Cuyckens,Filip, AU - Claeys,Magda, PY - 2002/12/13/pubmed PY - 2003/2/13/medline PY - 2002/12/13/entrez SP - 2341 EP - 8 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 16 IS - 24 N2 - Different reversed-phase liquid chromatography (LC) columns of conventional dimensions were coupled to an ultraviolet photodiode array detector (UV-DAD) and a magnetic sector-type spectrometer, equipped with an electrospray ionization (ESI) source, by a laboratory-made flow splitter. A mixture of three flavonoid-O-glycosides was employed to examine the effects of the solvent composition, the flow rate, the stationary phase, the pH and the organic acid added, on the chromatographic separation, the UV-DAD detection, the ESI process and the entire LC system with ESI-MS and UV-DAD detection. In the positive ion mode, methanol containing 1% acetic acid was by far the most sensitive in ESI-MS analysis, whereas an acetonitrile/water mobile phase containing 0.5% formic acid was proved to give the best sensitivity in LC/ESI-MS/UV-DAD analysis. In the negative ion mode, the highest sensitivity was obtained with a mobile phase containing 0.1% formic acid, while addition of bases decreased the sensititvity. The optimal flow rate was higher in negative ESI (20-50 micro L/min) than in positive ESI (5 micro L/min), and the percentage of organic phase had an influence on the sensitivity of ESI-MS detection. With regard to the selection of a suitable C(18) reversed-phase LC column, a column which is well end-capped is to be preferred, because residual silanol groups appear to impair the separation of flavonoid glycosides. The optimized LC/ESI-MS/UV-DAD method was applied to a commercial Crataegus extract, which is used in phytomedicine to treat cardiovascular problems and is known to be rich in flavonoids. It is demonstrated how UV spectra and first-order ESI mass spectra allow a fast characterization of flavonoids, even if reference compounds are not available or at hand. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/12478580/Optimization_of_a_liquid_chromatography_method_based_on_simultaneous_electrospray_ionization_mass_spectrometric_and_ultraviolet_photodiode_array_detection_for_analysis_of_flavonoid_glycosides_ L2 - https://doi.org/10.1002/rcm.861 DB - PRIME DP - Unbound Medicine ER -