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  • Title: Fourier transform ion cyclotron resonance mass spectrometry for the characterisation of kavalactones in the kava plant: elemental formulae confirmation by dual spray accurate mass measurement and structural confirmation by infrared multiphoton dissociation and sustained off-resonance irradiation collision induced dissociation.
    Author: Warburton E, Bristow T.
    Journal: Eur J Mass Spectrom (Chichester); 2006; 12(4):223-33. PubMed ID: 17057279.
    Abstract:
    Roots and extracts of the kava plant have been used in herbal medicine to treat sleep disturbances, stress and anxiety, although reported cases of liver toxicity led to many countries restricting its sale. The detection of the presence of kava in many medicinal products requires the use of methods capable of identifying the kavalactones with high certainty. Here, we describe the use of Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) for the characterisation of six kavalactones (kavain, dihydrokavain, methysticin, dihydromethysticin, yangonin and desmethoxyyangonin) utilising accurate mass measurement for the determination of their elemental formulae and product ion MS (both sustained off-resonance irradiation collision-induced dissociation and infrared multiphoton dissociation (SORI-CID and IRMPD) for structural confirmation. High performance liquid chromatography/FT-ICR-MS with a dual spray system for internal calibration of mass spectra was employed for accurate mass measurement and the determination of elemental formulae of the kavalactones in both standards and a root extract to confirm the presence of the kavalactones in the root powder. Mass accuracy of < 1 ppm was achieved. For structural confirmation, the IRMPD and SORI-CID spectra of the kavalactones in standards and a kava root powder extract were compared. Accurate mass measurement of the product ions was also conducted by external calibration and the elemental formula determined to aid with structural confirmation. The presence of the same fragment ions detected in the standards as in the extract further confirmed the presence of the kavalactones in the kava root powder with high certainty.
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