DETERMINATION OF ACRYLAMIDE IN COFFEE BY LIQUID CHROMATOGRAPHY – TANDEM MASS SPECTROMETRY

Significance of the topic

Acrylamide is a toxic Maillard reaction by-product classified by IARC as a probable human carcinogen. It forms during coffee roasting and transfers readily into brewed coffee, posing potential health risks. Regulatory bodies have set benchmark levels for acrylamide in coffee products, driving the need for reliable analytical methods.

Objectives and study overview

This work aims to develop and validate a robust liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for quantifying acrylamide in coffee. The approach integrates a modified QuEChERS extraction, dispersive solid-phase cleanup, and sensitive MS detection to meet regulatory requirements and practical laboratory needs.

Methodology and sample preparation

Sample extraction and cleanup

• Take 1 g ground coffee, add isotopically labeled internal standard (acrylamide-d3).
• Perform modified QuEChERS extraction to isolate acrylamide.
• Clean extracts by dispersive SPE, evaporate to dryness and reconstitute in 0.1 % formic acid in water.

Chromatographic conditions

• UPLC I-Class system with HSS C18 SB 1.8 µm column, temperature 30 °C.
• Gradient elution with water/0.1 % formic acid (A) and methanol (B), 0.2 mL/min flow, 5 µL injection.

Mass spectrometry settings

• Xevo TQ-S micro in positive ESI mode.
• MRM transitions for acrylamide and acrylamide-d3, capillary voltage 0.5 kV, desolvation at 600 °C.

Used instrumentation

• Waters ACQUITY UPLC I-Class
• ACQUITY UPLC HSS C18 SB column
• Xevo TQ-S micro mass spectrometer
• MassLynx v4.2 software

Main results and discussion

The method shows excellent linearity over 0.5–2500 ng/mL (r2 = 0.999) and achieves low detection limits suitable for benchmark ranges. Clean-up reduces matrix interference, yielding sharp acrylamide peaks. Analysis of FAPAS reference materials returned measured values within 2 % of assigned concentrations and relative standard deviations below 5 %.

Benefits and practical applications

The validated method enables:

• Accurate quantification of acrylamide in roasted and instant coffee.
• Compliance with EU regulation 2017/2158 and other standards.
• Extension to diverse processed foods by adjusting extraction cleanup.

Future trends and potential applications

Advances may include higher throughput automation, coupling with high-resolution mass spectrometry for non-target screening, and real-time monitoring in production lines. Miniaturized and multiplexed platforms could further streamline routine quality control.

Conclusion

The modified QuEChERS LC-MS/MS method offers sensitive, precise and regulatory-compliant analysis of acrylamide in coffee. Its robustness and adaptability make it a valuable tool for laboratories ensuring food safety and meeting legislative benchmarks.

Reference

1. Kocadağlı T, Göncüoğlu N, Hamzalıoğlu A, Gökmen V. In-depth study of acrylamide formation in coffee: role of sucrose decomposition and lipid oxidation. Food Function. 2012;3(9).
2. Guenther H, Anklam E, Wenzl T, Stadler R. Acrylamide in coffee: progress in analysis, formation and level reduction. Food Addit Contam. 2007;24(sup1).
3. EUR-Lex. Commission Regulation (EU) 2017/2158 laying down mitigation measures and benchmark levels for acrylamide in food. 2019.