Volatile PFAS in Complex Juice Matrices: A Simple Approach Using HS-SPME GC/MS/MS for Volatile Contaminant Analysis

Importance of the topic

PFAS are synthetic compounds used in many consumer products and pose global health risks due to persistence and toxicity. Detecting volatile PFAS in complex food matrices such as juice is critical to safeguard food quality and public health, especially for vulnerable populations such as children.

Objectives and study overview

This study aimed to develop a precise and accurate analytical workflow for quantifying volatile PFAS in diverse juice matrices using headspace solid phase microextraction (HS-SPME) coupled with triple quadrupole gas chromatography mass spectrometry. The method sought minimal sample preparation and high sensitivity to complement existing LC/MS techniques for comprehensive food safety evaluation.

Použitá instrumentace

• Shimadzu GCMS-TQ8040 NX triple quadrupole mass spectrometer
• Shimadzu Nexis GC-2030 gas chromatograph
• Shimadzu AOC-6000 Plus multifunctional autosampler with HS-SPME module
• SPME fiber 50/30 µm DVB/CAR/PDMS

Methodology and sample preparation

Calibration standards spanned 1 to 2000 ng/L with isotope dilution for ten target PFAS classes including FTIs, FTACs, FTMACs, FTOHs and FASAs. Juice samples (apple and berry blends in carton and plastic) and reagent water controls were spiked with analytes and labeled standards then subjected to HS-SPME at 50 °C for 30 min. Salt addition and automated extraction reduced matrix interference. Method blanks, initial and continuing calibration verifications ensured instrument integrity and quantitation accuracy.

Main results and discussion

The calibration curves exhibited excellent linearity with R2 ≥ 0.993 for all PFAS. Method blanks showed no contamination. Initial calibration verification and continuing calibration recovery fell within 70–130%. Laboratory control samples demonstrated mean recoveries of 83–115% and precision (%RSD) < 7%. Juice matrices yielded recoveries of 69–120% and %RSD below 12% across four brands, validating method robustness. The use of compound-specific isotopic standards proved essential to compensate matrix effects and ensure accurate quantification.

Benefits and practical applications

• High sensitivity and selectivity enable low limits of quantitation
• Simplified sample preparation reduces operational errors
• Automated HS-SPME workflow suits high-throughput screening
• Complements LC/MS to provide a total solution for food safety

Future trends and possibilities

Expanding the method to additional beverages and complex food matrices will strengthen PFAS monitoring efforts. Development of new isotopically labeled standards for emerging PFAS will improve quantitation. Integration with high-resolution mass spectrometry and data analytics may enhance non-targeted screening and risk assessment strategies.

Conclusion

The HS-SPME GCMS-TQ8040 NX approach offers a simple, reliable and accurate workflow for volatile PFAS analysis in juice matrices with minimal preparation. Demonstrated linearity, recovery and precision meet rigorous criteria, supporting this method as a valuable tool for food safety laboratories seeking comprehensive PFAS monitoring.

References

1. Per and polyfluoroalkyl substances in cosmetics US Food and Drug Administration 2024
2. Phelps DW et al Environmental Science Technology 2024 58 5670 5684
3. Alazaiza MY et al Case Studies in Chemical and Environmental Engineering 2025 article 101127
4. Shimadzu Application News GCMS-2403 HS-SPME GC/MS/MS for water 2024
5. Shimadzu Application News GCMS-2404 drinking water analysis 2024
6. Shimadzu Application News GCMS-2405 bottled water analysis 2024