Single-drop microextraction combined with gas chromatography-electron capture detection for the determination of...

A single-drop microextraction method followed by gas chromatography-electron capture detection was developed to determine acrylamide in food samples. Acrylamide was extracted by water and derivatized by hydrobromic acid in the presence of ammonium peroxydisulfate. The derivatization was carried out at 45 °C in 15 min using 46 µL of hydrobromic acid and 98 mg of ammonium peroxydisulfate. A 3.0-mL volume of the derivatized analyte was extracted using a 1.0-µL n-octanol droplet hanging from the needle tip of a GC microsyringe. After extraction, the extract was injected into the gas chromatograph. The influence of experimental parameters effective on derivatization reaction yield and extraction performance was studied. The limit of detection and quantification, relative standard deviation and linearity of the method were 0.60 µg/L, 2.0 µg/L, <6.0%, and 2.0-100.0 µg/L, respectively. The method was utilized to determine acrylamide in three food samples (i.e., bread, potato chips and cookie).