Development and Validation of a modified QuEChERS coupled to Liquid Chromatography-Tandem Mass Spectrometry for the Rapid and Accurate Determination of Acrylamide in Cereal-Based Baby Foods.

Abstract

With the widespread consumption of cereal-based baby food by children, acrylamide contamination is a prevalent risk that may have carcinogenic consequences. This study aims to develop and validate a modified QuEChERS protocol without solvent exchange, followed by rapid separation and accurate determination of acrylamide in cereal-based baby foods using RP-LC-MS/MS. Samples were extracted using a modified AOAC QuEChERS version and cleaned up with basic alumina. Separation was performed on the Phenomenex® Kinetex C18 column (100 Å × 3.5µm × 4.6 mm × 150 mm) using a gradient elution program with a mobile phase of 10-mM ammonium formate/methanol. Determinations were conducted by ESI-MS/MS in positive ion mode. Basic alumina yielded clean extracts, resulting in acceptable recovery percentages and a tolerable ME < 5%. This has allowed extraction without a solvent exchange step. Efficient separation was achieved at a tR of 3.39 ± 0.05 employing an RP-C18 column with core-shell properties in a relatively short analysis run time of only 5 min. Trueness, precision, LOD, LOQ, linearity range, and R2 results were 92.5-104.6%, RSD≤12.2%, 5 µg/kg, 20 µg/kg, 4.0-1000.0 µg/kg, and > 0.9999, respectively. The test method applicability was demonstrated by proficiency testing and 50 real samples of cereal-based baby foods. Most of the tested samples were in violation of acrylamide's established EU benchmark (40 µg/kg). Acetate-buffered QuEChERS in conjunction with optimized amounts of basic alumina was confirmed as a superior driving approach for optimal method performances. Successful selection of the RP-C18 column is the proper means toward selective separation for acrylamide at a relatively short analysis run time. The modified AOAC QuEChERS with a d-SPE of basic alumina assisted in reducing the ME to tolerable levels while maintaining acceptable method performance. The RP-C18 column of core-shell properties enabled a rapid and accurate acrylamide determination.