Vortex-assisted dispersive low-density liquid–liquid microextraction of xanthydrol derivatized acrylamide in processed chips and water samples for gas chromatographic analysis

Abstract

Acrylamide, a probable human carcinogen present in heat-processed foods and environmental contaminants, requires sample extraction and preconcentration before chromatographic analysis. The method developed in this study employed derivatization with xanthydrol and dispersive liquid–liquid microextraction utilizing low-density anisole. Durian or potato chips were combined with deionized water, defatted with hexane, and subjected to precipitation of soluble carbohydrates and proteins using clarification reagents. Water samples were filtered through a membrane filter. Acrylamide was derivatized by introducing an acidic methanolic solution of xanthydrol at 50 °C. The derivatized acrylamide was extracted with 70 µL of anisole and vortexed, with the methanol from the xanthydrol solution serving as the disperser solvent. The anisole layer was analyzed using gas chromatography with both flame ionization and mass spectrometric detection. Linear calibration plots exhibited coefficients of determination >0.9997. The precision was measured at <10% RSD, and recoveries ranged from 84% to 107%. The quantitation limit varied from 2 to 10 µg kg−1 for processed chips and from 0.05 to 0.10 µg L−1 for water samples. Acrylamide was detected in all processed chip samples, with some concentrations exceeding the benchmark value of 750 μg kg−1. However, no acrylamide was identified in any of the water samples.