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

Significance of the Topic

Furan and alkylfurans form in foods during thermal processing via degradation of carbohydrates, ascorbic acid and lipids. Recognized as potentially carcinogenic, their accurate quantitation in products such as baby formula and coffee is critical for consumer safety and regulatory compliance.

Objectives and Study Overview

The study aims to develop and validate a headspace solid-phase microextraction arrow (HS-SPME Arrow) coupled with gas chromatography-mass spectrometry (GC-MS) method for simultaneous analysis of furan and its alkyl derivatives. A comparison of HS-SPME Arrow, traditional SPME fibers and static headspace was performed to select the optimal sample-preparation approach. Calibration strategies were tailored to low-concentration (1.25–150 ng/vial) and high-concentration (25–8 000 ng/vial) ranges matching baby formula and coffee matrices.

Methodology and Instrumentation

• Instrumental Setup
  • Gas chromatograph: Agilent 7890B GC
  • Mass spectrometer: Agilent 5977B MSD
  • Column: Rxi-624Sil MS, 30 m × 0.25 mm ID, 1.40 µm
  • Ionization: Electron impact (70 eV), SIM acquisition
• Sample Preparation
  • Matrix: 0.5 g baby formula or coffee + saline solution (30 % NaCl)
  • SPME device: Carbon wide-range (CWR) arrow
  • Incubation: 50 °C, 250 rpm, 10 min
  • Extraction: 50 °C, 250 rpm; 10 min for formula, 1 min for coffee
  • Desorption: 280 °C, 1 min in split mode (1:10 for formula, 1:100 for coffee)
• Calibration
  • Internal standards: Deuterated analogues for each analyte
  • Curve ranges: 1.25–150 ng/vial (low), 25–8 000 ng/vial (high)
  • Quantitation: Analyte/ISTD area ratios vs. spiked concentrations

Main Results and Discussion

• Sample-Preparation Comparison
  • HS-SPME Arrow delivered highest response for all analytes, outperforming traditional fibers and static HS
• Extraction Parameters
  • Optimal temperature: 50 °C balanced sensitivity across volatile furans
  • Extraction time: 10 min to reach equilibrium for most analytes
• Analytical Performance
  • Linearity: Correlation coefficients > 0.99 in both calibration ranges
  • Precision: RSDs typically < 10 %
  • Accuracy: 87–113 % in baby formula, 93–125 % in coffee, with slight positive bias at highest levels

Practical Benefits and Applications

The optimized HS-SPME Arrow GC-MS protocol offers robust, sensitive detection of furan compounds in complex food matrices. Its improved fiber durability and high signal-to-noise ratio support routine monitoring in quality control laboratories, regulatory analysis and research on thermal contaminants.

Future Trends and Applications

Anticipated developments include automation of headspace-sampling workflows, integration with high-resolution MS for suspect screening, expansion to additional food and environmental matrices, and on-site monitoring solutions to ensure rapid safety assessments.

Conclusion

A validated HS-SPME Arrow GC-MS method was established for reliable quantitation of furan and alkylfurans in baby formula and coffee. Optimized sampling conditions and calibration strategies achieved satisfactory linearity, precision and accuracy, demonstrating suitability for routine contaminant analysis.

Reference

• Pawliszyn J. Handbook of Solid Phase Microextraction. Chemical Industry Press, Beijing, 2009.
• Frank N., Dubois M., Huertas Pérez J.F. Detection of Furan and Five Alkylfurans, Including 2-Pentylfuran, in Various Food Matrices. J. Chromatogr. A 2020, 1622, 461119.