[Simultaneous determination of nine artificial sweeteners in food by solid-phase extraction coupled with high...

A simple and rapid method based on solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry for the simultaneous determination of nine artificial sweeteners (acesulfame-K, saccharin sodium, cyclamate, sucralose, aspartame, alitame, neotame, dulcin, neohesperidin dihydrochalcone) in various foods was developed. The sweeteners in food samples were extracted with triethylamine buffer solution (pH 4.5) and cleaned using an SPE column equipped with hydrophilic and lipophilic packing material. The analytes were separated on a Phenomenex Knietex^® F5 column (100 mm×2.1 mm, 2.6 μm) using 0.1% (v/v) formic acid-5 mmol/L ammonium formate/methanol as a mobile phase for gradient elution, and then determined by tandem mass spectrometry in positive and negative ESI modes under multiple reaction monitoring (MRM). The internal standard method was used to further suppress the matrix effect. The method proved to be very effective in the removal of matrix interferences. Calibration curves were linear within a studied range of concentrations (r²>0.999) for the nine artificial sweeteners. The limits of detection (LODs) and limits of quantification (LOQs) were within 2-30 μg/kg and 6-100 μg/kg, respectively. The recoveries for the nine investigated sweeteners were within 86.3%-106.3% at three spiked levels, with relative standard deviations (RSDs) between 1.2% and 5.9%. The developed method is rapid, efficient, accurate, and reliable; it can also be applied for the rapid determination of other artificial sweeteners in a complex food matrix.