title: Trace analysis of mono-, di-, tri-substituted polyfluoroalkyl phosphates and perfluorinated phosphonic acids in sewage sludge by high performance liquid chromatography tandem mass spectrometry.
abstract: A new method using ultrasonic extraction and solid phase extraction (SPE) clean-up pretreatments was developed for the analysis of mono-, di- and tri-substituted polyfluoroalkyl phosphates (abbreviated as mono-PAPs, di-PAPs and tri-PAPs) and perfluorinated phosphonic acids (PFPAs) in sludge from wastewater treatment plants (WWTPs). For the ultrasonic extraction of three mono-PAPs, three di-PAPs and three PFPAs in sludge samples, a mixture of tetrahydrofuran/acetic acid (1:1, v/v) was found to be the most suitable extraction solvent. The subsequently optimized clean-up and enrichment procedures were carried out with weak anion exchange (WAX) cartridges in-line coupled with graphitized carbon black (ENVI-Carb) tubes. Two tri-PAPs were ultrasonically extracted by acetonitrile/tetrahydrofuran (1:1, v/v) and cleaned by mixed-mode anion exchange (MAX) in-line coupled with ENVI-Carb cartridges. The analytes were analyzed by optimized high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method either in negative or positive ionization mode. The method quantification limits (MQLs) of the 11 analytes in sludge ranged from 0.6 to 5.1 ng/g, meanwhile the total recoveries of the pretreatment varied from 24% (6:2 mono-PAP) to 107% (PFDPA). The method was successfully applied to analyze 16 sewage sludge samples collected from seven provinces in China, and two mono-PAPs were identified with concentrations ranging from <MQLs to 10.7 ng/g.
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: Runzeng
authors.initials: R
authors.lastname: Liu
authors.forename: Ting
authors.initials: T
authors.lastname: Ruan
authors.forename: Thanh
authors.initials: T
authors.lastname: Wang
authors.forename: Shanjun
authors.initials: S
authors.lastname: Song
authors.forename: Miao
authors.initials: M
authors.lastname: Yu
authors.forename: Yan
authors.initials: Y
authors.lastname: Gao
authors.forename: Junjuan
authors.initials: J
authors.lastname: Shao
authors.forename: Guibin
authors.initials: G
authors.lastname: Jiang
mesh_terms: D002681:China; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D005466:Fluorocarbons / Q000737:chemistry; D005843:Geography; D015394:Molecular Structure; D010755:Organophosphates / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D063065:Organophosphonates / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D015203:Reproducibility of Results; D012722:Sewage / Q000737:chemistry*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D005466:Fluorocarbons; D010755:Organophosphates; D063065:Organophosphonates; D012722:Sewage; D014874:Water Pollutants, Chemical