title: Matrix solid-phase dispersion of polybrominated diphenyl ethers and their hydroxylated and methoxylated analogues in lettuce, carrot and soil.
abstract: In the present work, a novel analytical method for the simultaneous determination of ten polybrominated diphenyl ethers (PBDEs), eight methoxylated PBDEs (MeO-PBDEs) and seven hydroxylated PBDEs (OH-PBDEs) in soil, lettuce and carrot samples was developed. The procedure was based on matrix solid-phase dispersion (MSPD) followed by gas chromatography coupled to negative chemical ionization-mass spectrometry (GC-NCI-MS). Under optimum conditions, 0.5g of sample (freeze-dried in the case of lettuce and carrot samples) was dispersed with 0.5g of octadecyl-functionalized silica (C18) and 1.75g of acidified silica (10% H2SO4, w/w) was used as clean-up sorbent. A two-step fractionated elution was carried out. First, PBDEs and MeO-PBDEs were eluted in 75:25% (v/v) n-hexane/dichloromethane mixture and, then, the retained OH-PBDEs were eluted in pure dichloromethane. Both extracts were analyzed by GC-NCI-MS separately, in the case of OH-PBDEs after derivatization with N-methyl-N-(trimethylsilyl) trifluoroacetamide. The developed method was validated in terms of accuracy for soil, lettuce and carrot matrices, spiked at two fortification levels (5 and 25ngg(-1)). After correction with the corresponding surrogate, apparent recovery values (defined as the recovery obtained after correction with the corresponding surrogate) were in the 80-129% range. Precision (as relative standard deviation) in the 1-21% range and method detection limits (MDLs) in the 0.003 and 0.3ngg(-1) range for soil and in the 0.003-0.4ngg(-1) range (dry weight) for lettuce and carrot samples were obtained. For PBDEs the method was also validated with a standard reference material (SRM-2585) of house dust. Finally, the method was applied for the determination of target analytes in soil, lettuce and carrot.
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), 48080 Bilbao, Spain. Electronic address: arantza.iparraguirre@ehu.es.
authors.forename: A
authors.initials: A
authors.lastname: Iparraguirre
authors.affiliation: Department of Analytical Chemistry, Nutrition and Food Science, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Rodil
authors.affiliation: Department of Analytical Chemistry, Nutrition and Food Science, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: J B
authors.initials: JB
authors.lastname: Quintana
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), 48080 Bilbao, Spain.
authors.forename: E
authors.initials: E
authors.lastname: Bizkarguenaga
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), 48080 Bilbao, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Prieto
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), 48080 Bilbao, Spain.
authors.forename: O
authors.initials: O
authors.lastname: Zuloaga
authors.affiliation: Department of Analytical Chemistry, Nutrition and Food Science, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Cela
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), 48080 Bilbao, Spain.
authors.forename: L A
authors.initials: LA
authors.lastname: Fernández
mesh_terms: D018552:Daucus carota / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D055768:Halogenated Diphenyl Ethers / Q000032:analysis* / Q000737:chemistry; D006900:Hydroxylation; D018545:Lactuca / Q000737:chemistry*; D057230:Limit of Detection; D012987:Soil / Q000737:chemistry*
chemical_list: D055768:Halogenated Diphenyl Ethers; D012987:Soil
keywords: Carrot; Gas chromatography-negative chemical ionization-mass spectrometry; Lettuce; Matrix solid-phase extraction; Polybrominated diphenyl ethers; Soil