Abstract

This paper shows the applicability of capillary electrophoresis (CE) coupled to mass spectrometry (MS) for the analysis of acrylamide (AA) in foodstuffs. In order to obtain an ionisable compound amenable to be analysed by CE, acrylamide was derivatised with 2-mercaptobenzoic acid. Spectra in positive and negative modes were studied in order to select the best ionisation mode and multistep tandem mass spectrometry was used to obtain structural information. Maximum signal was observed when negative mode was used and MS/MS and MS 3 were selected for quantitation and confirmation, respectively. For the separation, a fused-silica capillary of 80 cm and 50 μm I.D. and 35 mM ammonium formate/ammonia solution at pH 10 as running electrolyte were used. The applicability of field amplified sample injection (FASI) in reversed polarity was evaluated in order to decrease detection limits. The developed FASI–CE–MS/MS method provided a detection limit of 8 ng g −1 and good linearity ( r = 0.999) and precision (day-to-day lower than 15%). The method has been applied to the analysis of different representative food products and the results were compared with those obtained by LC–MS/MS.

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