Robust Quantification of Acrylamide in Food using Gas Chromatography-Single Quadrupole Mass Spectrometry

Importance of the Topic

Acrylamide is a probable human carcinogen formed during high-temperature cooking of starch-rich foods. Its routine monitoring in food products such as potato crisps, breads and coffee is critical for consumer safety and regulatory compliance. A robust, cost-effective analytical method supports industry efforts to control acrylamide levels and protect public health.

Objectives and Study Overview

This study evaluates a streamlined gas chromatography–mass spectrometry (GC-MS) workflow for low-level acrylamide quantification in food and coffee matrices. Key goals include simplifying sample preparation, enhancing sensitivity and selectivity, and eliminating the need for expensive isotope-labeled standards.

Methodology and Instrumentation

The protocol employs acetonitrile extraction followed by silylation with MSTFA. Derivatized samples are analyzed on a Thermo Scientific™ ISQ™ 7000 GC-MS system coupled to a TRACE™ 1310 gas chromatograph and TriPlus™ RSH autosampler. Data acquisition and quantification use Chromeleon™ CDS software.

Main Results and Discussion

• Chromatographic performance: Gaussian peak shapes (tailing factor 0.91–1.01) and narrow peak widths (~4 s) improved detection limits.
• Linearity: External calibration from 1 to 1000 ppb (equivalent to 5–5000 µg/kg) yielded R²≥0.9993, residual %RSD ≤4.8.
• Standard addition: Crisps and coffee samples spiked at 1000 and 2000 µg/kg produced R²≥0.9987, residual %RSD ≤4.0, compensating for matrix effects without 13C internal standard.
• Sensitivity: Limit of identification (LOI) of 1 ppb (5 µg/kg in sample) achieved in selected ion monitoring (m/z 128).
• Repeatability and robustness: Sixteen injections of spiked coffee (1000 µg/kg) delivered %RSD of 2.9; mid- and late-sequence injections over 99 runs showed %RSD of 1.3 without instrument maintenance.

Benefits and Practical Applications

• Cost-effective alternative to LC-MS/MS and bromination methods.
• High sensitivity and selectivity through silylation and SIM mode.
• Reduced solvent consumption and simplified cleanup.
• Elimination of isotope-labeled internal standard reduces analysis cost.
• User-friendly workflow and reporting via Chromeleon CDS supporting high-throughput laboratories.

Future Trends and Potential Applications

• Extension of silylation-based GC-MS methods to other food contaminants.
• Integration with automated sample handling and miniaturized GC-MS platforms.
• Adoption of real-time data processing and AI-driven quality control.
• Application in regulatory monitoring, QA/QC and industrial process control.

Conclusion

The GC-MS method combining acetonitrile extraction, MSTFA derivatization and SIM detection on the ISQ 7000 platform delivers a robust, sensitive and economical solution for routine acrylamide quantification in food and coffee. Its high repeatability, linearity and selectivity meet regulatory and industry requirements without recourse to costly labeled standards.

Instrumental Setup

• Gas Chromatograph: Thermo Scientific TRACE 1310 with split/splitless injector
• Mass Spectrometer: Thermo Scientific ISQ 7000 with ExtractaBrite source in SIM mode
• Autosampler: Thermo Scientific TriPlus RSH
• Software: Thermo Scientific Chromeleon CDS v7.2

References

1. Friedman M. Chemistry, Biochemistry, and Safety of Acrylamide. J Agric Food Chem. 2003;51:4504.
2. Swedish National Food Administration. WHO to hold expert consultation on acrylamide in food. 2002.
3. Mottram DS, Wedzicha BL, Dodson AT. Acrylamide is formed in the Maillard reaction. Nature. 2002;419:448–449.
4. Stradler RH, et al. Acrylamide from Maillard reaction products. Nature. 2002;419:449–450.
5. Rydberg P, et al. Factors influencing acrylamide in heated foodstuffs. J Agric Food Chem. 2003;51:7012.
6. Smith EA, Oehme FW. Acrylamide and polyacrylamide: production, use, environmental fate and neurotoxicity. Rev Environ Health. 1991;9:215.
7. Food Standards Agency. Acrylamide legislation and guidance. 2017/2158.
8. Riediker S, Stadler RH. Analysis of acrylamide in food by isotope-dilution LC-MS/MS. J Chromatogr. 2003;1020:121–130.
9. Andrawes F, et al. Chemistry of acrylamide bromination for GC-MS analysis. J Chromatogr. 1987;399:269–275.