期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 393, 期 1, 页码 247-256出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-008-2420-2
关键词
Biogenic amines; Derivatization; Ferrocene; Liquid chromatography; Mass spectrometry; Stable isotopes
资金
- Deutsche Forschungsgemeinschaft (Bonn, Germany)
- Fonds der Chemischen Industrie (Frankfurt, Germany)
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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