title: Focused ultrasound assisted extraction for the determination of PBDEs in vegetables and amended soil.
abstract: Focused-ultrasound solid-liquid extraction was developed for the extraction of polybrominated diphenyl ethers in vegetables and amended soil. Firstly, solid-phase extraction clean-up using 2g and 5 g of Florisil and 2-g silica cartridges were evaluated and elution profile was also optimised. Similar recoveries were obtained for most compounds while better recoveries were obtained for 5-g Florisil in the case of the heavier PBDEs. FUSLE extraction time (2 min) guaranteed quantitative extraction of the target analytes in the four studied matrices (69-130%). Method detection limit values were in the range of 1-5 ng g(-1) for splitless injection in a gas chromatograph coupled to a mass spectrometer and no significant improvement was obtained for large volume injection. Relative standard deviation values were between 1% and 30%. Recoveries obtained using FUSLE were compared with those obtained with microwave assisted extraction and the developed method was also applied to a certify reference material of polybrominated diphenyl ethers and polychlorinared biphenyls in sediment. Similar values were obtained in the case of carrot and pepper matrices (77-130% for FUSLE and 77-112% for MAE). However, MAE provided extraction recoveries higher than 100% for most of the BDE congeners in lettuce and amended soil.
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain. Electronic address: ebizkarguenaga@gmail.com.
authors.forename: Ekhiñe
authors.initials: E
authors.lastname: Bizkarguenaga
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Arantza
authors.initials: A
authors.lastname: Iparragirre
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Itsaso
authors.initials: I
authors.lastname: Zabaleta
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Asier
authors.initials: A
authors.lastname: Vallejo
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Luis Angel
authors.initials: LA
authors.lastname: Fernández
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Ailette
authors.initials: A
authors.lastname: Prieto
authors.affiliation: Department of Analytical Chemistry, University of the Basque Country, 48080 Bilbao, Spain.
authors.forename: Olatz
authors.initials: O
authors.lastname: Zuloaga
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis* / Q000302:isolation & purification; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction; D008872:Microwaves; D012015:Reference Standards; D012989:Soil Pollutants / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction; D014465:Ultrasonics; D014675:Vegetables / Q000737:chemistry*
chemical_list: D055768:Halogenated Diphenyl Ethers; D012989:Soil Pollutants; C086401:pentabromodiphenyl ether
keywords: Amended soil; Focused ultrasound solid–liquid extraction; Microwave assisted extraction; Polybrominated diphenyl ethers; Vegetables