title: Comparison of in-cell lipid removal efficiency of adsorbent mixtures for extraction of polybrominated diphenyl ethers in fish.
abstract: Polybrominated diphenyl ethers (PBDEs) have become ubiquitous environmental contaminants due to their incorporation into many consumer products. Their ability to bioaccumulate to alarming levels in fat-rich matrices such as fish demands fast and efficient methods to monitor these contaminants. We present an analytical method for selective-pressurised liquid extraction (S-PLE) of PBDEs from fish tissue. Fat removal performance of different mixtures of Florisil, silica gel and sulphuric acid-impregnated silica gel were evaluated using a response surface experimental design approach for determining the optimal fat-retaining mixture for S-PLE. Acid-silica gel had the greatest individual effect on fat retention; with a two-thirds acid-silica one-third Florisil mixture found to be the most efficient (>97%). Method validation was performed using recovery experiments at three spiked concentration levels (0.05, 0.5 and 5ngg(-1) ww). Mean recoveries of target analytes in spiked samples ranged from 70 to 124%, with relative standard deviations <27%. The S-PLE lipid removal efficiency combined with the sensitivity of triple quadrupole mass spectrometers provides a fast and comparatively inexpensive analytical method for analysis of PBDEs in fish samples.
authors.affiliation: School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, Vic. 3001, Australia.
authors.forename: Peter
authors.initials: P
authors.lastname: Wardrop
authors.affiliation: School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, Vic. 3001, Australia.
authors.forename: Paul D
authors.initials: PD
authors.lastname: Morrison
authors.affiliation: School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, Vic. 3001, Australia.
authors.forename: Jeff G
authors.initials: JG
authors.lastname: Hughes
authors.affiliation: School of Applied Sciences, RMIT University, GPO Box 2476, Melbourne, Vic. 3001, Australia. Electronic address: bradley.clarke@rmit.edu.au.
authors.forename: Bradley O
authors.initials: BO
authors.lastname: Clarke
mesh_terms: D000327:Adsorption; D000818:Animals; D005399:Fishes / Q000378:metabolism*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D016018:Least-Squares Analysis; D057230:Limit of Detection; D008055:Lipids / Q000302:isolation & purification; D059625:Liquid-Liquid Extraction / Q000379:methods*; D015203:Reproducibility of Results; D012822:Silicon Dioxide; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D055768:Halogenated Diphenyl Ethers; D008055:Lipids; D014874:Water Pollutants, Chemical; D012822:Silicon Dioxide
keywords: Accelerated solvent extraction; Fish; In-cell cleanup; Polybrominated diphenyl ethers; Pressurised liquid extraction; S-PLE