Development of High‐Performance Liquid Chromatography–Electrospray Mass Spectrometry with Size‐Exclusion Chromatography for Determination of Acrylamide in Fried Foods

Abstract

A method by liquid chromatography–electrospray mass spectrometry (LC/MS) with a size‐exclusion chromatography column for the analysis of acrylamide in fried foods, is reported. In the mass spectral analysis using an electrospray MS, the signal at m/z 72, which was assigned to the [M + H]⁺ ion, was observed as the main peak. The main m/z signal showed a maximum at the fragmentor voltage of 100 V. The retention time for the elution of acrylamide from the size‐exclusion chromatography column ranged from 15 to 20 min, and the eluate was analyzed by LC/MS with a reversed‐phase column. A linear response was found for the acrylamide standard tested within the concentration range of 5.0–1000 ng/mL, with correlation coefficients (r) greater than 0.99. Sample preparation was performed by means of solvent extraction, which gave acrylamide recoveries higher than 90% with relative standard deviations less than 10%, with ¹³C‐labeled acrylamide standard.

Keywords:

• Acrylamide
• Liquid chromatography mass spectrometry
• Size‐exclusion chromatography
• Fried food