Determination of Polyamines in Baby Food by Gas Chromatography-Mass Spectrometry: Optimization of Extraction and Microwave-Assisted Derivatization Using Response Surface Methodology

The present work evaluates the feasibility of microwave-assisted acylation combined with previous ion-pair extraction for the determination of the polyamines spermidine and spermine in baby food by GC-MS. In this way, extraction and derivatization reaction times were simultaneously optimized using a central composite rotational design. From response surface analysis, we verified maximum analytical response for spermidine and spermine employing 1 M hydrochloric acid solution as extraction solvent under shaking during 35 min, followed by acylation derivatization using a household microwave at 600 W for only 5 min. Limits of detection and quantification of 5 and 10 mu g kg(-1) were achieved, and recoveries from 72 to 112% and RSD values ae<currency>16% were obtained under repeatability and within-reproducibility conditions for both polyamines, at levels of 250 and 500 mu g kg(-1). The validated GC-MS method was applied for 20 baby food samples commercially available in Brazil, thus resulting in the first report on spermidine and spermine in baby food.