A method for the low-level (ng g −1) determination of perfluorooctanoate in paper and textile by liquid chromatography with tandem mass spectrometry

• Published in: Journal of Chromatography A Vol. 1123; no. 1; pp. 10 - 14
• Main Authors: Stadalius, Marilyn, Connolly, Paul, L’Empereur, Karen, Flaherty, John M., Isemura, Tsuguhide, Kaiser, Mary A., Knaup, Wolfgang, Noguchi, Masahiro
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 04.08.2006; Elsevier
• Subjects: Analytical chemistry; Applied sciences; Caprylates - analysis; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Exact sciences and technology; Fibers and threads; Fluorocarbons - analysis; Fluorotelomer; Forms of application and semi-finished materials; LC–MS/MS; Mass Spectrometry - methods; Organofluorine compounds; Other chromatographic methods; Paper, paperboard, non wovens; Perfluorooctanoic acid; PFOA; Polymer industry, paints, wood; Reference Standards; Sensitivity and Specificity; Technology of polymers; Textiles - analysis; Wood. Paper. Non wovens; Fluorotelomer; Perfluorooctanoic acid; Organofluorine compounds; PFOA; LC–MS/MS; Trace analysis; Validation; Chemical analysis; Textile; Organic perhalocompound; Coupled method; HPLC chromatography; Isocratic condition; Electrospray; LC-MS/MS; Reversed phase chromatography; Residue; Mass spectrometry MS/MS; Paper; Fluorine Organic compounds; Quantitative analysis
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2006.03.037

The determination of perfluorooctanoate (PFO) in articles of commerce has become increasingly important to understand if treated products are a possible source of PFO. An LC–MS/MS method for the determination of PFO in paper and textile using a dual labeled 13C-PFOA internal standard was successfully developed and validated. Residues of PFO were determined using an isocratic, reversed-phase high-performance liquid chromatography (HPLC) method with an ammonium acetate/methanol buffer. Ions monitored were 413 (parent) and 369 (daughter) for PFO and 415 (parent) and 370 (daughter) for dual labeled 13C-PFOA internal standard. As a precaution against ubiquitous PFO that occasionally occurs in mobile phase or instrument components, two Hypercarb™ cartridges (4 mm) were placed before the HPLC injector. Any PFO that was captured by the cartridges was removed before each injection by flushing the system with 100% methanol prior to equilibration with the isocratic mobile phase. Overall recovery and standard deviation over a 3 day validation regimen for samples ( n = 54–55) fortified with PFOA at 5, 50, and 200 ng g −1 were 114 ± 4.9% for textile and 110 ± 7.6% for paper. The results also established a limit of detection (LOD) of 1 ng g −1 in textile and 2 ng g −1 in paper based upon S/N of the 5.0 ng g −1 fortification versus the untreated paper and textile.