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Title: Development and Validation of a Modified QuEChERS protocol Coupled to Liquid Chromatography-Tandem Mass Spectrometry for the Rapid and Accurate Determination of Acrylamide in Cereal-Based Baby Foods.
Author: Marzouk AM, Shendy AH, Aboelhassan AFA, Gomaa AM, El-Shahat MF.
Journal: J AOAC Int; 2023 Jul 17; 106(4):899-908. PubMed ID: 37137234.
Abstract:
BACKGROUND: With the widespread consumption by children of cereal-based baby food, acrylamide contamination is a prevalent risk that may have carcinogenic consequences. OBJECTIVE: This study aims to develop and validate a modified QuEChERS protocol (quick, easy, cheap, effective, rugged, and safe) without solvent exchange, followed by rapid separation and accurate determination of acrylamide in cereal-based baby foods using reversed-phase (RP)-LC-MS/MS. METHODS: Samples were extracted using a modified QuEChERS protocol of the AOAC version and cleaned up with basic alumina. Separation was performed on a Phenomenex® Kinetex C18 column (100 Å × 3.5 µm × 4.6 mm × 150 mm) using a gradient elution program with a mobile phase of 10 mM ammonium formate-methanol. Determinations were conducted using electrospray ionization (ESI)-MS/MS in positive-ion mode. RESULTS: Basic alumina yielded clean extracts, resulting in acceptable recovery percentages and a tolerable matrix effect (ME) <5%. This allowed extraction without a solvent exchange step. Efficient separation was achieved at a retention time (tR) of 3.39 ± 0.05 min 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 (PT) and 50 real samples of cereal-based baby foods. Most of the tested samples were in violation of acrylamide's established European Union benchmark (40 µg/kg). CONCLUSION: Acetate-buffered QuEChERS protocol in conjunction with optimized amounts of basic alumina was confirmed as an efficient extraction protocol for acrylamide from cereal-based baby foods resulting in optimal method performance. Successful selection of the RP-C18 column is key for selective separation for acrylamide in a relatively short analysis run time. HIGHLIGHTS: The modified AOAC QuEChERS protocol with a dispersive solid phase extraction (d-SPE) of basic alumina assisted in reducing the ME to tolerable levels while maintaining acceptable method performance. The use of an RP-C18 column with core-shell properties enabled a rapid and accurate acrylamide determination.

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