title: Design of experiment approach for the optimization of polybrominated diphenyl ethers determination in fine airborne particulate matter by microwave-assisted extraction and gas chromatography coupled to tandem mass spectrometry.
abstract: A sensitive and selective procedure for the determination of 12 polybrominated diphenyl ethers (BDE-28, BDE-49, BDE-47, BDE-66, BDE-100, BDE-119, BDE-99, BDE-155, BDE-154, BDE-153, BDE-139 and BDE-183) in airbone particulate matter (PM2.5) at trace level has been developed. The proposed method includes extraction PM2.5-bound PBDEs by microwave-assisted extraction (MAE) followed by gel permeation chromatography (GPC) clean-up and determination by GC-MS/MS using a programmed temperature vaporizer (PTV) in large volume injection (LVI) mode to introduce the sample to the chromatographic system. A design of experiment (DoE) approach was used for the optimization of large volume injection and microwave-assisted extraction parameters to improve these techniques efficiency. Other conditions of the method were studied: GC-MS/MS parameters, extraction solvent and matrix effect. The limit of quantification ranged from 0.063pgm(-3) to 0.210pgm(-3) when air volumes of 723m(3) were collected. Recoveries ranged from 80% to 106%. The method was successfully applied to eight real samples collected from a residential area of the monitoring network of the Region of Valencia Government (Spain) during April-August 2012. BDE-47 and BDE-99 were quantified in six and five samples respectively. The concentrations were ranged from 0.063 to 0.112pgm(-3) for BDE-47, and from 0.107 to 0.212pgm(-3) for BDE-99.
authors.affiliation: Public Health Laboratory of Valencia -FISABIO, Av. Catalunya, 21, 46020 Valencia, Spain.
authors.forename: Maria Isabel
authors.initials: MI
authors.lastname: Beser
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda Sos Baynat s/n, 12071 Castellón, Spain.
authors.forename: Joaquim
authors.initials: J
authors.lastname: Beltrán
authors.affiliation: Public Health Laboratory of Valencia -FISABIO, Av. Catalunya, 21, 46020 Valencia, Spain; Department of Analytical Chemistry, University of Valencia, Doctor Moliner 50, 46100 Burjassot, Spain. Electronic address: yusa_vic@gva.es.
authors.forename: Vicent
authors.initials: V
authors.lastname: Yusà
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis* / Q000737:chemistry*; D008872:Microwaves; D052638:Particulate Matter / Q000737:chemistry*; D013030:Spain; D053719:Tandem Mass Spectrometry; D013696:Temperature
chemical_list: D055768:Halogenated Diphenyl Ethers; D052638:Particulate Matter
keywords: Experimental design; GC-MS/MS; Microwave assisted extraction (MAE); PBDEs; PM2.5; Programmed temperature vaporizer (PTV)