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Determination of Acrylamide in Processed Foods using ACQUITY UPLC I-Class and Xevo TQ-S micro

Applications | 2019 | WatersInstrumentation
LC/MS, LC/MS/MS, LC/QQQ
Industries
Food & Agriculture
Manufacturer
Waters

Summary

Significance of Acrylamide Determination


Acrylamide arises in many processed foods via high-temperature Maillard reactions and is a probable carcinogen. Its ubiquitous presence in staples like potato products, coffee and baked goods poses a public health concern and mandates reliable analytical monitoring to ensure consumer safety and regulatory compliance.

Objectives and Study Overview


This study aimed to develop and validate a rapid, cost-effective UPLC-MS/MS approach using Waters ACQUITY UPLC I-Class and Xevo TQ-S micro to quantify trace levels of acrylamide in diverse food matrices, including potato chips, bread, coffee, and infant foods. Internal validation followed EU Regulation 2017/2158 performance criteria.

Methodology and Instrumentation


  • Sample preparation: Modified QuEChERS extraction with isotopically labelled acrylamide-d3 internal standard; dispersive SPE cleanup (PSA, MgSO4); evaporation and reconstitution in 0.1% formic acid.
  • Chromatography: ACQUITY UPLC I-Class with HSS C18 SB column (2.1 × 100 mm, 1.8 µm) at 30 °C; gradient elution between 0.1% formic acid in water and LC-MS grade methanol; flow rate 0.2 mL/min; 5 µL injection; sample at 10 °C.
  • Mass spectrometry: Xevo TQ-S micro with ESI+; MRM acquisition; capillary voltage 0.5 kV; cone voltage 20 V; desolvation at 600 °C; source at 150 °C; desolvation gas 1000 L/hr; cone gas 50 L/hr.

Key Results and Discussion


  • The method achieved excellent chromatographic retention and peak shape for acrylamide at low nanogram levels, with linearity (0.5–2500 ng/mL) exhibiting r2 > 0.999.
  • Limits of detection and quantification met or exceeded EU benchmark requirements for target food categories.
  • Recovery of spiked samples ranged 86–107% with repeatability (RSDr) below 6%, surpassing both EU and SANTE guidelines.
  • Analysis of FAPAS reference materials confirmed accuracy and precision, with measured values aligning with assigned concentrations and ion ratios/retention time tolerances.
  • Effective cleanup minimized matrix interferences even in complex samples like potato chips and coffee.

Contributions and Practical Applications


This validated protocol provides laboratories with a fast, sensitive and robust tool for routine acrylamide monitoring in compliance with EU regulations. The integration of QuEChERS cleanup and Xevo TQ-S micro enhances throughput and reduces solvent consumption, facilitating implementation in quality assurance and regulatory environments.

Future Trends and Potential Uses


Emerging directions include adaptation of the method to ultra-trace screening in novel food matrices, coupling with high-resolution MS for non-targeted contaminant profiling, and automation of sample preparation to improve laboratory efficiency and traceability.

Conclusion


The combination of ACQUITY UPLC I-Class and Xevo TQ-S micro delivers a reliable, high-throughput solution for acrylamide quantification across diverse processed foods. The method meets stringent regulatory criteria, offering a valuable asset for food safety monitoring and risk assessment.

Reference


  1. EFSA CONTAM Panel. Scientific Opinion on acrylamide in food. EFSA Journal 2015, 13(6), 4104.
  2. EFSA Panel on Contaminants in the Food Chain. Public Consultation Outcome on acrylamide draft opinion. EFSA Supporting Publication 2015; EN-817.
  3. Carere A. Genotoxicity and Carcinogenicity of Acrylamide: a Critical Review. Ann Ist Super Sanita 2006;42(2):144–155.
  4. Food Standards Agency. Food Survey Information Sheet; Acrylamide and Furan FSIS 2017.
  5. EU Commission Regulation 2017/2158. Mitigation measures and benchmark levels for acrylamide in food.
  6. European Union SANTE 11813/2017. Guidance Document on Analytical Quality Control and Method Validation for Pesticide Residues.

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