Determination of biogenic amines in food samples using derivatization followed by liquid chromatography/mass spectrometry |
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Authors: | Susanne Bomke Bettina Seiwert Lukas Dudek Stefan Effkemann Uwe Karst |
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Institution: | 1.Institut für Anorganische und Analytische Chemie,Westf?lische Wilhelms-Universit?t Münster,Münster,Germany;2.LAVES-Institut für Fische und Fischereierzeugnisse,Nieders?chsisches Landesamt für Verbraucherschutz und Lebensmittelsicherheit,Cuxhaven,Germany |
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Abstract: | A liquid chromatography (LC)/mass spectrometry method was developed for the determination of selected biogenic amines in various
fish and other food samples. It is based on a precolumn derivatization of the amines with succinimidylferrocenyl propionate
under formation of the respective amides and their reversed-phase liquid-chromatographic separation with subsequent electrospray
ionization mass-spectrometric detection. Deuterated putescine, cadaverine, and histamine are added prior to the derivatization
as internal standards that are coeluted, thus allowing excellent reproducibility of the analysis to be achieved. Depending
on the analyte, the limits of detection were between 1.2 and 19.0 mg/kg, covering between 2 and 3 decades of linearity. The
limit of detection and the linear range for histamine are suitable for the surveillance of the only defined European threshold
for biogenic amines in fish samples. Compared with the established ortho-phthalaldehyde (OPA)/LC/fluorescence method, the
newly developed method allows an unambiguous identification of the biogenic amines by their mass spectra in addition to only
retention times, a fivefold acceleration of the separation, and independency from the sample matrix owing to the isotope-labeled
internal standards. Various fish, calamari, and salami samples were successfully analyzed with the new method and validated
with an independent OPA/LC/fluorescence method. |
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Keywords: | Biogenic amines Derivatization Ferrocene Liquid chromatography Mass spectrometry Stable isotopes |
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