title: Determination of perfluorooctanesulfonate and perfluorooctanoic acid in sewage sludge samples using liquid chromatography/quadrupole time-of-flight mass spectrometry.
abstract: A new method is developed for the determination of perfluorooctanesulfonate (PFOS) and perfluorooctanoic acid (PFOA) in sewage sludge samples. The analytes in sewage sludge samples are extracted by methanol and formic acid, cleaned by C18 solid-phase extraction, then separated, identified and quantitated by liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). A C18 column (150 mm x 2.1 mm, 3.5 microm) with gradient elution of MeOH-H(2)O (60:40) containing 5 mmol/L ammonium acetate and MeOH-H(2)O (80:20) is used for the chromatographic separation. [M-K](-) ions at m/z 498.93 for PFOS and [M-COOH](-) ion at m/z 368.97 for PFOA are selected for QTOF-MS in the negative electrospray ionization mode. The detection limits for PFOS and PFOA in sewage sludge samples are 0.5 and 0.8 ng/g, respectively. The spiked recoveries are in the range of 85-114 and 71-98% for PFOS and PFOA, respectively. The proposed method is successfully applied to the analysis of PFOS and PFOA in 16 sewage sludge samples from China. PFOS and PFOA are detected in most sewage sludge samples and the concentrations of PFOS and PFOA are up to 5383 and 4780 ng/g (oven dry weight), respectively.
authors.affiliation: State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.
authors.forename: Rui
authors.initials: R
authors.lastname: Guo
authors.forename: Qunfang
authors.initials: Q
authors.lastname: Zhou
authors.forename: Yaqi
authors.initials: Y
authors.lastname: Cai
authors.forename: Guibin
authors.initials: G
authors.lastname: Jiang
mesh_terms: D017738:Alkanesulfonic Acids / Q000032:analysis*; D002210:Caprylates / Q000032:analysis*; D002681:China; D002853:Chromatography, Liquid / Q000379:methods*; D005466:Fluorocarbons / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity; D012722:Sewage / Q000032:analysis* / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D017738:Alkanesulfonic Acids; D002210:Caprylates; D005466:Fluorocarbons; D012722:Sewage; D014874:Water Pollutants, Chemical; C023036:perfluorooctanoic acid; C076994:perfluorooctane sulfonic acid