The headspace solid-phase microextraction (HS-SPME) method with two different coatings synthesized by sol–gel technology [such as poly(ethylene glycol) (PEG) and PEG reinforced with multi-walled carbon nanotubes (PEG/CNTs)] coupled with gas chromatography–flame ionization detector (GC–FID) was proposed for the determination of furan at trace levels in food samples. Under optimized conditions, the linear range for furan with PEG and PEG/CNTs fibers was 0.005–10 and 0.0005–10 ng/mL, the limit of detection (S/N = 3) was 0.001 and 0.00025 ng/mL and the limit of quantification (LOQ) was 0.005 and 0.0005 ng/mL, respectively. For PEG and PEG/CNTs fibers, repeatability (n = 5) was 6.2% and 4.9% and reproducibility (n = 3) was 6.6% and 5.3%, respectively. Relative recoveries for the spiked samples with 0.1 ng/mL of furan were ranged from 92% to 103%. The proposed HS-SPME–GC–FID method was successfully applied for the extraction of furan in two environmental food samples (baby food and fruit juice).

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