Headspace solid phase microextraction in-situ supercritical fluid extraction coupled to gas chromatography–tandem mass spectrometry for simultaneous determination of perfluorocarboxylic acids in sediments

Headspace solid phase microextraction (HS-SPME) in-situ supercritical fluid extraction (SFE) was investigated for the determination of trace amounts of perfluorocarboxylic acids (PFCAs) in sediments. Quantitation was performed by using gas chromatography coupled to negative chemical ionization–tandem mass spectrometry (GC–NCI–MS/MS). The optimum conditions of HS-SPME following SFE were obtained using 500 μL n-butanol as a derivatization reagent in supercritical carbon dioxide with static extraction for 10 min, then dynamic extraction for 20 min at 30 MPa and 70 °C and simultaneous collected with 100 μm film thickness PDMS fiber. The linear range of proposed method was from 5 to 5000 ng g−1, with limit of detection ranging from 0.39 to 0.54 ng g−1 and limit of quantitation ranging from 1.30 to 1.80 ng g−1. The developed method was successfully applied to analyze PFCAs in sediments from rivers and beach near industrial areas. The concentrations of PFCAs determined are from 282 to 4473 ng g−1.

► Headspace solid phase microextraction in-situ supercritical fluid extraction was investigated for the determination of PFCAs in sediments.
► Quantitation was performed by using GC–NCI–MS/MS.
► The linear range was from 5 to 5000 ng g−1, with LOD ranging from 0.39 to 0.54 ng g−1 and LOQ ranging from 1.30 to 1.80 ng g−1.
► This method was successfully applied to analyze PFCAs in sediments from rivers and beach near industrial areas.
► The concentrations of PFCAs from real samples determined are from 282 to 4473 ng g−1.