Quantitative Volatile PFAS Analysis in Textiles

Importance of the topic

Per- and polyfluoroalkyl substances (PFAS) have been widely applied in textile finishing to impart water-, stain-, and oil-repellent properties. Growing evidence of environmental persistence and health risks, combined with tightening regulatory frameworks (REACH/POPs) and industry restricted substance lists (ZDHC, OEKO-TEX, AFIRM, bluesign), increases demand for reliable analytical methods that can detect and quantify trace levels of volatile PFAS in complex textile matrices. Analytical methods that meet or exceed new standards (for example EN 17681-1:2025) are essential for compliance testing, product stewardship, and risk assessment.

Objectives and overview of the study

This application note evaluates a gas chromatography–triple quadrupole mass spectrometry (GC–TQ) workflow for quantitative analysis of volatile PFAS in textiles. The study aimed to demonstrate method sensitivity, linearity, recoveries, repeatability, and applicability across apparel matrices using the Agilent 8890 GC coupled with the Agilent 7010D GC/TQ system. The method targeted 34 native volatile PFAS plus four isotopically labeled internal standards and followed established sample preparation guidance consistent with EN 17681-1:2025.

Methodology

Key procedural elements included:

• Standards: Native and isotopically labeled PFAS standards prepared from commercial sources. Stock and intermediate mixes prepared in ethyl acetate; calibration range covered eight levels from 0.5 to 100 ng/mL (ppb) with a constant ISTD at 5 ng/mL.
• Calibration: Linear regression with 1/x weighting, calibration linearity R2 > 0.99 (minimum five calibration points).
• Sample extraction: Based on Annex E of EN 17681-1:2025 using methanol. Typical preparation: weigh ~1.0 g textile, spike ISTD and analyte spikes as required, sonicate at 60 °C for 1 hour, cool, centrifuge, filter, dilute into ethyl acetate, and perform a 20-fold dilution prior to GC injection.
• Quality control: A T‑shirt used as QC sample and spiked at three levels—10 µg/kg (low), 25 µg/kg (mid), 200 µg/kg (high)—with procedural and matrix blanks included. MDLs were calculated from nine continuous QC injections.

Used instrumentation

• Agilent 8890 gas chromatograph coupled with Agilent 7010D GC/TQ equipped with HES 2.0 ion source.
• Agilent multimode inlet (MMI) with splitless liner (part number 5190-2293).
• Agilent J&W DB-624 column, 30 m × 0.25 mm, 1.40 µm (part number 122-1334UI).
• Data acquisition and quantitation used Agilent MassHunter Quantitative Analysis software (version 12).

Main results and discussion

Analytical performance highlights:

• Sensitivity: Sub‑ppb method detection limits (MDLs) were achieved for all 34 targeted volatile PFAS in the textile matrix, demonstrating high instrument sensitivity within matrix extracts.
• Limits of quantification (LOQs): For 28 compounds the workflow achieved LOQs of 10 µg/kg; three compounds had LOQs of 25 µg/kg. Two compounds (PFODA and 1H,1H‑perfluorooctyl acrylate) did not meet LOQ criteria due to poor recoveries (≈40–53%), so LOQs were not established for them.
• Recoveries: More than 80% of analytes met the acceptance range of 60–140% recovery at spiked QC levels. Many fluorotelomer alcohols (FTOHs) showed recoveries of ~70–120%, indicating efficient extraction for volatile PFAS classes.
• Precision: Repeatability across sample preparations demonstrated %RSD ≤ 20% for all analytes at the mid QC level, supporting robust reproducibility for routine analyses.
• Calibration performance: All targets exhibited strong linear response (R2 > 0.99) across the tested calibration range (0.5–100 ppb).
• Application to real samples: In waterproof shorts two analytes (8:2 FTOH and 10:2 FTOH) were detected above MDLs but their concentrations remained below ZDHC formulation limits. This illustrates the method’s ability to detect relevant volatile PFAS at levels important for regulatory compliance and industry screening.

Practical benefits and applications

• Regulatory and compliance testing: The method meets sensitivity and quantitation requirements needed to support compliance with industry standards and regulatory limits, including the ZDHC MRSL and guidance in EN 17681-1:2025.
• Routine laboratory workflow: Demonstrated reproducibility (%RSD ≤ 20%), robust recoveries for most analytes, and a straightforward methanol extraction make the workflow suitable for high‑throughput screening in contract and in‑house QC laboratories.
• Matrix applicability: Performance was demonstrated across multiple textile types (T‑shirt, waterproof shorts, socks), confirming broad applicability to apparel and related materials.

Future trends and potential applications

• Extended and harmonized analyte panels: Expansion of target lists to include additional volatile PFAS, transformation products, and homologues will improve screening completeness as new substances enter commerce.
• Coupled workflows: Integration of GC–TQ for volatile PFAS with LC–MS/MS workflows for ionic/nonvolatile PFAS in a complementary testing strategy will provide comprehensive coverage across PFAS classes.
• Lower detection limits and non‑target screening: Advances in ion source design, MS acquisition strategies, and data processing will enable lower MDLs and improved non-target/ suspect screening capabilities.
• Improved sample preparation: Development of standardized cleanup steps and matrix-matched calibration strategies could further reduce matrix effects and improve recoveries for problematic compounds.
• Regulatory alignment: Continued harmonization with standards such as EN 17681-1:2025 and industry RSL updates will drive method adoption and inter-laboratory comparability.

Conclusion

The presented GC–TQ workflow using the Agilent 8890/7010D platform provides a sensitive, accurate, and reproducible approach for quantitative volatile PFAS analysis in textile matrices. Sub‑ppb MDLs for all targets, LOQs of 10 µg/kg for the majority of analytes, acceptable recoveries for most compounds, and %RSD ≤ 20% demonstrate suitability for routine compliance and screening. The method supports industry and regulatory needs for detecting low-level volatile PFAS in apparel and similar materials.

References

1. Quante J.M. Safer Treatments to Create Water & Oil Repellent Fabrics. AATCC Review, 2023, 23(4).
2. National Council of Textile Organizations. Home.
3. U.S. Environmental Protection Agency. Our Current Understanding of the Human Health and Environmental Risks of PFAS.
4. World Health Organization. Assessing the Occurrence and Human Health Risk of Per and Polyfluoroalkyl Substances.
5. National Cancer Institute. PFAS Exposure and Risk of Cancer.
6. European Chemicals Agency. List of Substances Subject to POPs Regulation.
7. ZDHC Foundation. ZDHC Manufacturing Restricted Substance List (MRSL).
8. OEKO‑TEX Association. STANDARD 100, Edition 04.2025.
9. AFIRM Group. Restricted Substances List (RSL), Version 10.1, 2025.
10. bluesign Association. bluesign System Black Limits (BSBL), Version 7.0, July 1, 2025.
11. European Committee for Standardization (CEN). EN 17681-1:2025. Textiles and Textile Products—Per and Polyfluoroalkyl Substances (PFAS)—Part 1: Analysis of an Alkaline Extract Using Liquid Chromatography and Tandem Mass Spectrometry; June 17, 2025.
12. Agilent Technologies. Fully Automated Workflow for Volatile PFAS Analysis in Food Contact Materials Using GC‑Triple Quadrupole MS. Application note 5994‑8295EN, 2025.
13. Doyle H., Flexman K., Keyte I., et al. An Assessment on PFAS in Textiles in Europe’s Circular Economy. European Environment Agency, No. 70110421; February 16, 2024.