Fully Automated Workflow for Volatile PFAS Analysis in Food Contact Materials Using GC-Triple Quadrupole

Importance of the Topic

The occurrence of per- and polyfluoroalkyl substances (PFAS) in food contact materials (FCMs) raises significant health and environmental concerns. Regulatory bodies worldwide are tightening limits for PFAS migration, driving the need for reliable, high-throughput analytical methods. Gas chromatography coupled with triple quadrupole mass spectrometry (GC-TQ) delivers the sensitivity and selectivity required, but manual sample preparation can create workflow bottlenecks and variability.

Objectives and Study Overview

This study aimed to develop and validate a fully automated workflow for quantifying over 30 volatile PFAS in paper-based FCMs, such as coffee cups. The approach integrates automated sample preparation on the PAL3 Series 2 RTC autosampler with an Agilent 7010D GC/TQ system to streamline calibration, extraction, cleanup, and injection steps.

Methodology and Instrumentation

A paper cup matrix was cut, weighed (1 g ±0.01 g), and loaded into 10 mL vials on the PAL3 autosampler. The system performed liquid handling for calibration standards (1–500 ng/mL), solvent-based extraction, vortex mixing, incubation, centrifugation, micro-SPE filtration, and direct injection into the GC/TQ.

Instrumentation Used

• GC/TQ: Agilent 7010D with HES 2.0 ion source.
• GC: Agilent 8890 with multimode inlet (MMI) and splitless liner.
• Autosampler: CTC PAL3 Series 2 RTC.
• Software: MassHunter Acquisition 13.0, Optimizer, and SWARM autotune.

Main Results and Discussion

• Chromatographic Separation: A 30 m × 0.25 mm × 1.40 µm DB-624 column achieved baseline resolution of 34 PFAS targets, producing sharp, symmetric peaks for compounds such as 4:2, 6:2, 8:2, and 10:2 FTOH.
• Sensitivity and Linearity: Method detection limits (MDLs) were <2 µg/kg for most analytes. Limits of quantitation (LOQs) of 20 µg/kg were attained for 24 key PFAS. Calibration across nine levels (1–500 ng/mL) yielded correlation coefficients (R²) >0.99.
• Precision and Accuracy: Retention time RSDs were <0.05%. Quality control recoveries ranged from 65% to 135% with %RSD <20% at low, medium, and high spiking levels. Intra-batch %RSD for FTOHs was <10%.
• Blank Assessment: Reagent blanks showed target concentrations <25% of matrix blanks, indicating minimal background contamination. Detection of certain PFAS in matrix blanks confirmed sample leaching behavior.

Benefits and Practical Applications

• Fully automated workflow minimizes human error and reduces solvent consumption.
• Enhanced throughput supports routine regulatory compliance and safety testing of FCMs.
• Reproducible results facilitate reliable trace-level monitoring of volatile PFAS.

Future Trends and Applications

Ongoing improvements in ion source technology and software automation are expected to further boost sensitivity and throughput. Expansion to additional PFAS classes, complex matrices, and integration of machine-learning data analysis will enhance screening capabilities. Automated workflows can be adapted for multi-residue regulatory screening and environmental monitoring.

Conclusion

The fully automated PAL3 Series 2 RTC and Agilent 7010D GC/TQ workflow delivers robust, reproducible analysis of volatile PFAS in food contact materials. Achieving sub-ppb detection limits, excellent linearity, and high precision, the method streamlines sample preparation and accelerates routine PFAS monitoring to meet evolving regulatory demands.

References

1. Agilent Technologies. Fully Automated Workflow for Volatile PFAS Analysis in Food Contact Materials Using GC-Triple Quadrupole MS. Publication Number: 5994-8295 EN.