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Determination of perfluorooctane sulfonate and perfluorooctanoic acid in human plasma by large volume injection capillary column switching liquid chromatography coupled to electrospray ionization mass spectrometry
Author(s) -
Holm Anders,
Wilson Steven R.,
Molander Paal,
Lundanes Elsa,
Greibrokk Tyge
Publication year - 2004
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301647
Subject(s) - chemistry , chromatography , perfluorooctanoic acid , electrospray ionization , mass spectrometry , electrospray , analytical chemistry (journal) , detection limit , analyte , elution , sulfonate , environmental chemistry , organic chemistry , sodium
Rapid, selective, and sensitive methodology for the quantification of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in human plasma using packed capillary liquid chromatography coupled to electrospray ionization ion‐trap mass spectrometry has been developed. Plasma proteins were precipitated using acetonitrile and the resulting supernatant was diluted 1 + 1 with water containing 10 mM ammonium acetate (NH 4 Ac) prior to injection. Sample volumes of 250 μL were loaded onto a 30 mm×0.32 mm ID 10 μm Kromasil C 18 precolumn by a carrier solution consisting of 10 mM NH 4 Ac in ACN/H 2 O (5/95, v/v ) at a flow rate of 100 μL/min, providing on‐line analyte enrichment and sample clean‐up. Backflushed elution onto a 100 mm×0.32 mm ID 3.5 μm Kromasil C 18 analytical column was conducted using an ACN/H 2 O solvent gradient containing 10 mM NH 4 Ac. In order to improve the robustness and performance of the method, perfluoroheptanoic acid (PFHA) was used as internal standard. Separation and detection of PFOA, PFHA, and PFOS were achieved within 10 minutes. Ionization was performed in the negative mode in the m/z range 250–550. The method was validated over the concentration range 1–200 ng/mL for PFOA and over the range 5–200 ng/mL untreated plasma for PFOS, yielding correlation coefficients of 0.997 (PFOA) and 0.996 (PFOS), respectively. The within‐assay ( n = 6) and between‐assay ( n = 6) precisions were in the range 2.1–9.2 and 5.6–12%, respectively. The concentration limits of detection (cLOD) of PFOA was 0.5 ng/mL while the cLOD of PFOS was estimated to be 0.2 ng/mL in untreated plasma.