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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.
- Authors
Marzouk, Abdelrahman M.; Shendy, Amr H.; Ahmed Aboelhassan, AlaaEldean Fathy; Gomaa, Ahmed M.; El-Shahat, M. F.
- 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 6 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.
- Subjects
EUROPEAN Union; ACRYLAMIDE; BABY foods; LIQUID chromatography-mass spectrometry; SOLID phase extraction; GRADIENT elution (Chromatography)
- Publication
Journal of AOAC International, 2023, Vol 106, Issue 4, p899
- ISSN
1060-3271
- Publication type
Article
- DOI
10.1093/jaoacint/qsad053