Analysis of Perfluoroalkyl Substances in Textile and Leather Using the Agilent 6470 Triple Quadrupole LC/MS

Importance of Topic

Per- and polyfluoroalkyl substances (PFAS) are widely used to impart stain and water resistance in textiles and leather but raise environmental and health concerns due to their persistence and toxicity

Objectives and Study Overview

This study aimed to develop and validate a fast, sensitive method for detecting 33 PFAS in textile and leather matrices using an Agilent 6470 triple quadrupole LC/MS coupled with an Infinity II HPLC fitted with a PFC-Free Conversion Kit

Methodology and Instrumentation

Sample Preparation

• Cuts of fabric (100 cm2 or 1 g) and leather (100 cm2 or 1 g) were sonicated in methanol at 60 °C followed by concentration and addition of 13C-MPFOS internal standard and mixed PFAS standards
• Textiles were quantified by external solvent calibration and leather by standard addition to compensate for matrix effects

Instrumentation

• HPLC: Agilent 1290 Infinity II with PFC-Free Conversion Kit, high-speed pump, multisampler with multiwash, C18 analytical column and PFC delay column
• MS: Agilent 6470 triple quadrupole in dynamic multiple reaction monitoring mode with Jet Stream electrospray ionization
• Mobile phases: aqueous ammonium acetate and acetonitrile gradient; total run time 17 minutes

Main Results and Discussion

Calibration and Sensitivity

• Linear response for all PFAS from 0.5 to 20 µg/L with R2 > 0.996
• Instrument detection limits (IDLs) ranged from 0.01 to 0.09 µg/L with precision below 7% RSD
• Method detection limits (MDLs) in textile matrices were 0.00031–0.00312 mg/kg (1 g) and 0.027–0.23 µg/m2 (100 cm2); in leather matrices 0.00034–0.0017 mg/kg and 0.023–0.26 µg/m2

Recovery and Precision

• Textile recoveries at multiple spiking levels ranged 92.9–110% with RSD < 20%
• Leather recoveries improved from variable values using solvent calibration to 95.7–109% with standard addition and RSD < 20%
• Carryover was minimized by the PFC-Free kit, enabling reproducible analysis

Benefits and Practical Applications

This rapid method achieves separation of 33 PFAS in 17 minutes versus 37 minutes in standard EPA protocols, offering high throughput and low detection limits suited to compliance monitoring of consumer textiles and leather goods

Future Trends and Applications

Advances may include automation of sample prep, extension to other PFAS and related compounds, integration with high-resolution MS for nontarget screening, and adaptation for onsite or field-deployable systems to meet regulatory driving points

Conclusion

The presented LC/MS/MS approach combining a PFC-Free HPLC kit and triple quadrupole MS offers fast, sensitive and accurate quantification of PFAS in complex textile and leather matrices, meeting ISO performance requirements and supporting environmental and consumer safety initiatives

Reference

• United States Environmental Protection Agency Research on Per and Polyfluoroalkyl Substances PFAS 2017
• ISO 23702-1 2018 Leather Organic Fluorine Part 1 Liquid Chromatography Tandem Mass Spectrometry
• Shoemaker and Tettenhorst Method 537.1 Determination of Selected Per and Polyfluorinated Alkyl Substances in Drinking Water by LC/MS/MS US EPA 2018