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

Importance of the Topic

Furan and alkylfurans are volatile byproducts generated during thermal processing of carbohydrates, ascorbic acid, and lipids in food. Classified as possible carcinogens, their presence in commodities such as baby formula and coffee raises health and regulatory concerns. Routine monitoring supports food safety and quality control.

Study Objectives and Overview

This work aimed to develop a robust workflow using headspace SPME arrow coupled to GC-MS for quantification of furan and six alkylfurans in baby formula and coffee. The study encompassed method optimization, calibration over low and high concentration ranges, and performance evaluation against traditional techniques.

Methodology and Instrumentation

Sample Preparation

• Matrix: 0.5 g baby formula or coffee
• Salt addition: 10 mL (baby formula) or 5 mL (coffee) of 30 % NaCl solution
• Internal standards: deuterated analogues added at 50 µL (1 µg/mL) for baby formula and 40 µL (25 µg/mL) for coffee
• Incubation and extraction: 50 °C, 250 rpm agitation, 10 min

SPME Arrow Extraction and Desorption

• Fiber coating: Carbon Wide Range (CWR)
• Extraction: 50 °C, 10 min
• Desorption: 280 °C, 1 min

GC-MS Conditions

• Instrument: Agilent 7890B GC with 5977B MSD
• Column: Rxi-624Sil MS, 30 m × 0.25 mm ID, 1.40 µm film
• Injection: split 1:10 for baby formula, 1:100 for coffee
• Carrier gas: He at 1.40 mL/min
• Oven program: 35 °C (3 min) to 75 °C at 8 °C/min, then to 200 °C at 25 °C/min (1 min hold)
• Detection: EI 70 eV, SIM mode with quantifier and qualifier ions

Key Results and Discussion

Calibration and Linearity

• Low range for baby formula (1.25–150 ng in vial) and high range for coffee (25–8000 ng in vial)
• Excellent linearity with correlation coefficients within acceptance criteria

Extraction Optimization

• Temperature study (40, 50, 60 °C) favored 50 °C to preserve volatile analytes
• Time profiles showed furan equilibrium at 10 min; 10 min chosen as compromise for all targets

Technique Comparison

• SPME Arrow outperformed traditional SPME and static headspace in response and signal-to-noise
• Enhanced sensitivity and robustness achieved with CWR coating

Performance Metrics

• Accuracy: 87–113 % across matrices and levels
• Precision: RSD below 12 % in most cases
• Higher bias in coffee at elevated spike levels suggests need for further exploration

Benefits and Practical Applications

The HS-SPME arrow GC-MS method delivers improved sensitivity, reproducibility, and reduced fiber fragility. It enables rapid screening of furan and alkylfurans in baby foods and beverages, supporting QA/QC workflows and regulatory monitoring.

Future Trends and Opportunities

Automation of SPME arrow sampling can increase throughput and consistency. Coupling with high-resolution or tandem mass spectrometry may lower detection limits. Expansion to diverse food matrices and development of real-time monitoring strategies will further advance food safety initiatives.

Conclusion

A validated headspace SPME arrow GC-MS method for furan and alkylfurans in baby formula and coffee has been established. Optimized extraction and instrumental conditions delivered reliable quantitation with acceptable accuracy and precision, demonstrating its applicability for routine food safety 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