Comprehensive PFAS Analysis in Textiles Using Triple Quadrupole GC/MS and LC/MS Workflows

Significance of the topic

Per- and polyfluoroalkyl substances (PFAS) are widely applied in textiles to impart water-, oil- and stain-repellency. Growing evidence of environmental persistence and human-health concerns, together with tightened regulatory frameworks (for example EN 17681-1:2025, REACH/POPs and industry initiatives such as ZDHC, OEKO-TEX, AFIRM and Bluesign), requires analytical workflows that are sensitive, robust and traceable across diverse textile matrices. This study presents a standardized, end-to-end analytical solution capable of quantifying both volatile and non-volatile PFAS classes in common garments, addressing routine laboratory throughput and regulatory monitoring needs.

Objectives and study overview

The study aimed to demonstrate a dual-platform, EN 17681-1:2025-aligned workflow for comprehensive PFAS coverage in textiles. Specific goals were to:

• Establish extraction protocols compatible with both GC/TQ and LC/TQ analysis.
• Quantify a broad panel of PFAS (>100 analytes across 14 chemical classes) in representative textile items (T-shirts, waterproof shorts, socks).
• Validate method performance in terms of recovery, linearity, sensitivity (LOQs), and reproducibility to meet industry/regulatory limits such as ZDHC.

Methodology

Sample preparation followed Annex E of EN 17681-1:2025 using heat- and ultrasound-assisted (HUA) extraction. Key procedural steps were:

• Weigh 1.0 ± 0.05 g textile sample into a 50 mL tube.
• Spike with surrogate/internal standards and, where applicable, target mixes for QCs.
• For volatile PFAS (GC/TQ): methanol extraction, sonication at 60 °C for 1 hour, cooling by shaking (1500 rpm, 10 min), centrifugation (4200 rpm, 5 min), filtration (nylon syringe filter), dilution with ethyl acetate and addition of ISTD prior to GC injection.
• For non-volatile PFAS (LC/TQ): alkalized methanol extraction, identical sonication and centrifugation, take 1 mL supernatant and adjust to pH 6–7 with acetic acid, filter, dilute, add ISTD and inject to LC.

The workflow intentionally avoids labor-intensive evaporation and reconstitution steps to improve lab throughput and reduce potential analyte loss.

Used Instrumentation

The dual-platform analytical configuration comprised:

• GC/TQ: Agilent 8890 gas chromatograph coupled to a 7010D triple quadrupole MS using a DB-624 column for volatile PFAS (more than 30 volatile analytes analyzed).
• LC/TQ: Agilent 1290 Infinity III UHPLC coupled to a 6475A triple quadrupole MS with a ZORBAX RRHD Eclipse Plus C18 column for non-volatile PFAS (over 70 non-volatile analytes analyzed).
• All consumables and standards were sourced and PFAS-verified from Agilent to minimize background contamination.

Main results and discussion

Coverage and sensitivity:

• The combined approach quantified over 100 PFAS across 14 chemical classes, separating volatile and non-volatile subsets to optimize analytical conditions for each group.
• Calibration performance was excellent for both platforms: volatile PFAS used eight levels (0.5–100 ng/mL) with R2 > 0.99; non-volatile PFAS used twelve levels (0.001–50 ng/mL) with R2 > 0.99 across at least five calibration points.

Extraction efficiency and recoveries:

• More than 80% of analytes demonstrated recoveries within the acceptance range of 60–140% across QC levels on both platforms.
• Typical volatile FTOHs recovered at 70–120% and PFAS mandated by EN 17681 and ZDHC recovered between 96–109%, indicating strong extraction efficiency across chemical classes.

Limits of quantification (LOQs):

• LOQs were determined from matrix-spiked QC levels and identification criteria. For volatile FTOHs (e.g., 4:2, 6:2, 8:2, 10:2) LOQs reached 10 µg/kg, well below typical formulation limits such as ZDHC’s 1000 µg/kg.
• On the LC/TQ platform, 58 of 74 non-volatile PFAS achieved LOQs of 10 µg/kg, satisfying EN 17681-1:2025 and ZDHC sensitivity requirements.

Reproducibility and robustness:

• Within-batch precision (n=6) for spiked QC recoveries showed relative standard deviations below 20% for all analytes, demonstrating reproducible method performance suitable for routine testing.
• MRM chromatogram overlays of representative compounds (PFOA, PFNA) showed consistent peak shapes and retention times across technical preparations.

Figures and tables in the original study summarized LOQ distributions for each platform, recovery distributions at LOQ levels for volatile and selected non-volatile PFAS, and calibration/precision data supporting method performance.

Benefits and practical applications of the method

Key advantages include:

• Comprehensive PFAS coverage by combining GC/TQ for volatile analytes and LC/TQ for non-volatile analytes.
• High sensitivity and compliance with regulatory thresholds (EN 17681-1:2025, ZDHC), enabling detection at trace µg/kg levels for many analytes.
• Streamlined sample preparation that eliminates evaporation/reconstitution, improving throughput and reducing analyte loss.
• Reproducible performance suitable for routine quality control, supplier screening, regulatory compliance testing and product stewardship across textile supply chains.

Limitations and considerations

Operational and analytical caveats to note:

• PFAS background contamination is a known risk; rigorous use of PFAS-clean consumables and verification is essential.
• Volatile vs non-volatile partitioning requires two platforms, which increases instrumentation demands and method complexity in resource-limited labs.
• Availability of certified reference materials and isotopically labeled surrogates remains a limiting factor for absolute quantification of some analytes.

Future trends and potential applications

Anticipated developments and opportunities include:

• Extension of targeted panels and incorporation of high-resolution mass spectrometry (HRMS) for non-target screening to detect novel or transformed PFAS species in textiles.
• Automation and miniaturization of sample preparation (for example solid-phase microextraction or on-line cleanup) to further increase throughput and reduce solvent use.
• Harmonization of interlaboratory protocols and expansion of certified reference materials to improve comparability across regulatory programs.
• Integration of data workflows and predictive informatics to support risk-based prioritization of PFAS in product supply chains.

Conclusions

The reported dual-platform workflow—based on heat- and ultrasound-assisted extraction and separate GC/TQ and LC/TQ analyses—delivers comprehensive, sensitive and reproducible quantification of PFAS in textile matrices. Performance metrics (recoveries, LOQs, linearity and precision) meet EN 17681-1:2025 and industry requirement thresholds such as ZDHC in most cases. The simplified sample-preparation protocol increases laboratory efficiency and supports routine monitoring and regulatory compliance across textile supply chains.

References

• Agilent publication: Quantitative Volatile PFAS Analysis in Textiles (Publication Number: 5994-8966 EN).
• European Committee for Standardization (CEN), EN 17681-1:2025.