Determination of acrylamide in coffee by ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry

Abstract

A method using ultra high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (UHPLC-APCI-MS/MS) was developed for the determination of acrylamide in coffee. The coffee samples spiked with 13C3-acrylamide as the internal standard were extracted with methanol, and cleaned using HLB solid phase extraction (SPE) cartridges. The liquid chromatography separation was performed on a Brownlee validated AQ C18 column with isocratic elution. Methanol and 0.1% (volume percentage) formic acid aqueous solution were used as the mobile phase. Identification of acrylamide was achieved by APCI-MS/MS with multiple reaction monitoring (MRM) in the positive mode. The quantification analysis was performed by the internal standard method. The calibration curve showed good linearity with a correlation coefficient of 0.999 in the range of 0.5-100.0 μg/L. The limit of detection (LOD) was 5.0 μg/kg. The limit of quantification (LOQ) was 10.0 μg/kg. Recovery of acrylamide from coffee sample was evaluated at concentrations of 100.0, 200.0 and 1000.0 μg/kg. The average recoveries of acrylamide were between 94.6%-115.0% with relative standard derivations (RSDs) in the range of 2.8%-3.6% (n=6). This simple, accurate and sensitive method was proven to be suitable for the determination of acrylamide in coffee.