AbstractThe voltammetric behavior of β‐carboline alkaloids at carbon nanotubes‐modified glassy carbon electrodes, as well as their quantification by amperometric monitoring of the oxidation responses, are reported. Cyclic voltammograms of harmane, harmine, harmaline and harmalol at the CNT‐GCE showed enhanced voltammetric responses with respect to those obtained at a bare GCE. The effect of pH on the oxidation ip and Ep values obtained by differential pulse voltammetry was discussed, as well as their mechanistic aspects. Hydrodynamic voltammogram of these compounds led us to select a potential value of +900 mV for their amperometric detection. Under these conditions, no fouling of the modified electrode surface is evidenced. The HPLC separation and determination of β‐carboline alkaloids were carried out using a mobile phase consisting of 20% (v/v) methanol‐20% (v/v) acetonitrile‐0.05 mol L−1 HPO solution of pH 9.0. Detection limits ranging between 28 nM (harmalol) and 88 nM (harmaline) were achieved. The usefulness of the chromatographic method with amperometric detection at the CNT‐GCE was demonstrated by analyzing soy seeds samples spiked with harmaline, harmane and harmine at a 0.25 μg/g level.
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