title: Headspace solid phase microextraction in-situ supercritical fluid extraction coupled to gas chromatography-tandem mass spectrometry for simultaneous determination of perfluorocarboxylic acids in sediments.
abstract: 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).
authors.affiliation: Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan.
authors.forename: Wen-Lin
authors.initials: WL
authors.lastname: Liu
authors.forename: Bao-Huey
authors.initials: BH
authors.lastname: Hwang
authors.forename: Zu-Guang
authors.initials: ZG
authors.lastname: Li
authors.forename: Jen-Fon
authors.initials: JF
authors.lastname: Jen
authors.forename: Maw-Rong
authors.initials: MR
authors.lastname: Lee
mesh_terms: D025924:Chromatography, Supercritical Fluid / Q000379:methods; D005466:Fluorocarbons / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D011312:Pressure; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D013696:Temperature; D014874:Water Pollutants, Chemical / Q000032:analysis
chemical_list: D005466:Fluorocarbons; D014874:Water Pollutants, Chemical