A rapid microwave-assisted derivatization process for the determination of phenolic acids in brewer's spent grains

A simple and fast method for the TMS derivatization of phenolic acids in a closed vial using microwave irradiation followed by GC/MS analysis is proposed. A full factorial design was used to investigate the effects of two independent variables, namely, time and power of microwave irradiation, on the yield of silylation reaction. The optimal conditions were tested against the classical heating derivatization procedure. No significant differences were found between the classical heating and microwave-assisted derivatization. Chromatographic separation of the nine phenolic acids examined was achieved in 16 min. The mass spectral fragmentation patterns of the derivatives obtained by the proposed method were identical to those from the classical heating. Four different batches of brewer's spent grain were extracted and analyzed for the total phenolic acid content. Significant differences between the batches of spent grains were found for all analytes. The total phenolic acid content varied between 2688 and 4884 mu g/g. (c) 2006 Elsevier Ltd. All rights reserved.