Isolation and characterization of methoxylated flavones in the flowers of Primula veris by liquid chromatography and mass spectrometry |
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Authors: | Huck C W Huber C G Ongania K H Bonn G K |
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Institution: | a Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens-University, Innrain 52a, 6020 Innsbruck, Austria b Institute of Organic Chemistry, Leopold-Franzens-University, Innrain 52a, 6020 Innsbruck, Austria |
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Abstract: | Characterization of six flavones, which were named substances G1, G2, G3, G4, G5 and G6 according to their RF values in normal-phase thin-layer chromatography, is reported. The pure flavones were purified after maceration with methanol by normal-phase solid-phase extraction, normal-phase medium-pressure liquid chromatography, normal-phase preparative thin-layer chromatography and preparative reversed-phase high-performance liquid chromatography (RP-HPLC). The collected fractions of several isolation steps were analyzed by normal-phase (NP) and RP-HPLC. Detection and identification of the substances G was accomplished by UV detection at 213–216 nm, diode array UV detection, or fluorescence detection (λex=330 nm; λem=440 nm). The molecular mass, the elementary composition, and the structure of the six components was determined by electron-impact high-resolution mass spectrometry (EI-HRMS). Substance G4 was identified as 3′,4′,5′-trimethoxyflavone. The substances G1–G6 were shown to be mono-, di- tri- and pentamethoxyflavones. HPLC–electrospray ionization tandem mass spectrometry (ESI-MS–MS) of the flavones was carried out employing a 150×2 mm I.D. column packed with a 3 μm/100 Å octadecylsilica stationary phase and a mobile phase comprising 1.0% acetic acid in water–acetonitrile (50:50). Comparative RP-HPLC–ESI-MS of the raw methanol extract and the isolated substances G1–G6 proved that the isolated compounds were pure and were not artifacts. Finally, RP-HPLC–ESI-MS–MS was used to identify substances G1–G6 in phytopharmaceutical drugs. |
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Keywords: | Flavones |
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