title: Microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography with mass spectrometry detection (MAE-HSSPME-GC-MS/MS) for determination of polybrominated compounds in aquaculture samples.
abstract: This paper describes the first validated method for the extraction, purification and determination of trace levels of a number of pollutants of growing concern, including polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs), in aquaculture feeds and products. The new procedure comprises microwave-assisted extraction (MAE; optimized, using a central composite experimental design, to 15 min at 85 degrees C in 14 mL of 1:1 hexane/dichloromethane), and concentration by headspace solid-phase microextraction (HSSPME), and separation/quantification by gas chromatography with mass spectrometry detection (GC-MS/MS). The method was validated on the reference materials IAEA-406 and WMF-01. Limits of detection for fourteen of the fifteen analytes considered range from 10 to 600 pg g(-1), and limits of quantification from 50 pg g(-1) to 1.9 ng g(-1). Linear ranges, accuracies and precisions are reported.
authors.affiliation: Instituto de Investigación y Análisis Alimentario, Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de Santiago de Compostela, Santiago de Compostela, Spain. qntuchi@usc.es
authors.forename: A M
authors.initials: AM
authors.lastname: Carro
authors.forename: R A
authors.initials: RA
authors.lastname: Lorenzo
authors.forename: F
authors.initials: F
authors.lastname: Fernández
authors.forename: R
authors.initials: R
authors.lastname: Phan-Tan-Luu
authors.forename: R
authors.initials: R
authors.lastname: Cela
mesh_terms: D053000:Analytic Sample Preparation Methods / Q000379:methods*; D017756:Aquaculture / Q000295:instrumentation*; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002849:Chromatography, Gas / Q000379:methods*; D004784:Environmental Monitoring / Q000295:instrumentation* / Q000379:methods; D004987:Ethers / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D007477:Ions; D013058:Mass Spectrometry / Q000379:methods*; D008872:Microwaves; D011075:Polybrominated Biphenyls / Q000737:chemistry; D012016:Reference Values; D053719:Tandem Mass Spectrometry / Q000379:methods; D013696:Temperature; D014873:Water Pollutants
chemical_list: D004987:Ethers; D007477:Ions; D011075:Polybrominated Biphenyls; D014873:Water Pollutants