NACRWV 2019: DETERMINATION OF ACRYLAMIDE IN COFFEE BY LC-MS/MS

Significance of the Topic

The formation of acrylamide during coffee roasting presents a significant food safety concern due to its potential carcinogenicity. Its high polarity leads to efficient extraction into brewed coffee, making accurate quantitation vital for consumer health protection and regulatory compliance.

Objectives and Study Overview

This study aims to develop and validate a robust LC-MS/MS method with a modified QuEChERS extraction to quantify acrylamide in coffee matrices. The method addresses challenges of polar analyte retention, complex food matrices, and broad concentration ranges across different food types.

Materials and Methods

Samples of homogenized coffee were extracted by a modified QuEChERS procedure with isotopically labelled acrylamide-d3 as internal standard. Dispersive SPE cleanup was applied, followed by evaporation and reconstitution in 0.1% formic acid in water. The approach concentrates the analyte and optimizes injection conditions.

Instrumentation

Liquid chromatography was performed on a Waters ACQUITY UPLC I-Class system with HSS C18 SB column (1.8 µm, 2.1 × 50 mm) at 30 °C and sample temperature of 10 °C. Mobile phases were water/0.1% formic acid (A) and methanol (B) at 0.2 mL/min with a gradient. Mass spectrometry used a Waters Xevo TQ-S micro with ESI+ and MRM transitions: acrylamide m/z 72.05→55.10, 72.05→44.10, 72.05→27.15; acrylamide-d3 m/z 75.00→58.10.

Main Results and Discussion

Calibration showed excellent linearity (r2 = 0.999, 1/x weighting) with all back-calculated standards within 20% of nominal. Analysis of a FAPAS coffee reference (assigned 249 µg/kg) returned 244 µg/kg (RSD 4.6%, bias −2.0%). Chromatograms confirmed strong retention and clear separation at low flow. Method validation met EU 2017/2158 criteria for linearity, accuracy, precision, and repeatability across processed food matrices.

Benefits and Practical Applications

• High sensitivity and selectivity for acrylamide quantitation in coffee.
• Streamlined sample preparation compatible with diverse food samples.
• Regulatory compliance enables routine quality control and risk assessment.

Future Trends and Potential Applications

Emerging developments may include automation of QuEChERS workflows, miniaturized and high-throughput extraction techniques, and integration of high-resolution MS for broader screening. Expansion to additional beverage and multi-residue analyses will further enhance surveillance capabilities.

Conclusion

The presented LC-MS/MS protocol combined with modified QuEChERS extraction offers a reliable, validated approach for determining acrylamide levels in coffee. It provides robust performance in line with regulatory requirements and applicable to various processed foods.

References

1. Kocadağlı T, Göncüoğlu N, Hamzalıoğlu A, Gökmen V. In-depth study of acrylamide formation in coffee during roasting: role of sucrose decomposition and lipid oxidation. Food Function. 2012;3(9):970.
2. Guenther H, Anklam E, Wenzl T, Stadler R. Acrylamide in coffee: progress in analysis, formation and level reduction. Food Additives and Contaminants. 2007;24(sup1):60-70.
3. European Commission. EU Regulation 2017/2158 on mitigation measures and benchmark levels for acrylamide in food. 2017.