Analysis of furan and alkylfuransin food commodities using headspace SPME arrow and GC-MS

Importance of the Topic

Heating of foods such as coffee and baby formula leads to the formation of furan and alkylfuran compounds, some of which are classified as possible carcinogens. Accurate and sensitive detection of these volatiles is critical for food safety monitoring and regulatory compliance. Headspace SPME Arrow combined with GC-MS offers improved sensitivity and robustness over traditional SPME fibers, addressing both analytical performance and practical handling concerns.

Objectives and Study Overview

This study aimed to establish a reliable workflow for quantifying furan and five alkylfurans (2-methylfuran, 3-methylfuran, 2-ethylfuran, 2,5-dimethylfuran and 2-pentylfuran) in baby formula and coffee. Four isotopically labeled internal standards were used to correct for matrix effects and ensure accurate quantitation across a wide concentration range.

Methodology and Instrumentation

Samples were prepared by spiking with internal standards and adding NaCl solution to promote volatility. Extraction was performed at 50 °C with agitation at 250 rpm for 10 min using a Wide Range Carbon SPME Arrow coating. Desorption occurred at 280 °C for 1 min in a split mode (1:10 for formula, 1:100 for coffee). Separation was achieved on an Rxi-624Sil MS column (30 m × 0.25 mm, 1.40 µm) with constant He flow (1.4 mL/min). Quantitation employed single-ion monitoring on an Agilent 7890B GC with 5977B MSD, optimizing transfer line, source and quadrupole temperatures for maximum sensitivity.

Main Results and Discussion

Comparison of headspace, traditional SPME and SPME Arrow showed 2–3× higher peak areas for most analytes using the Arrow device. Coating screening identified Wide Range Carbon as the best phase for furans. Extraction equilibrium was reached at 10 min for highly volatile furans, balancing throughput and sensitivity. Calibration curves were linear (r²>0.995) from low (1.25–150 ng) to high (25–8000 ng) concentration ranges. Recovery in baby formula at 5 and 50 µg/kg ranged from 87–113% with RSD <14%. In coffee at 1000 and 4000 µg/kg, recoveries were 83–125% with RSD <11%, though elevated accuracy at high levels suggests potential matrix bias requiring further investigation.

Benefits and Practical Applications

• Enhanced sensitivity and signal-to-noise for volatile analytes.
• Improved fiber robustness reduces downtime and maintenance.
• Rapid sample throughput with a 10-min extraction cycle.
• Accurate quantitation across diverse food matrices.

Future Trends and Applications

Further work could expand to other food matrices and low-moisture products, explore automated SPME Arrow workflows, and integrate high-resolution MS for improved selectivity. Miniaturized or on-line headspace sampling may enable real-time process monitoring in food manufacturing.

Conclusions

A headspace SPME Arrow GC-MS method was successfully developed for sensitive and reproducible analysis of furan and alkylfurans in baby formula and coffee. Method validation demonstrated excellent linearity, precision and recovery, positioning the approach as a practical tool for routine food safety testing.

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