title: Application of solid-phase extraction coupled with freezing-lipid filtration clean-up for the determination of endocrine-disrupting phenols in fish.
abstract: An analytical method has been developed for the determination of endocrine-disrupting phenols (eight alkylphenols and bisphenol A) in fish samples. The extraction of nine phenols from fish samples was carried out by ultrasonification. After the extraction, high levels of lipids were removed by freezing-lipid filtration instead of the traditional methods of column chromatography or saponification. During freezing-lipid filtration, about 90% of the lipids were eliminated without any significant loss of phenolic compounds. For further purification, hydrophilic-lipophilic balanced copolymer (HLB) sorbent with a poly(divinylbenzene-co-N-vinylpyrrolidone) phase and Florisil-solid-phase extraction (SPE) cartridges were used to eliminate the remaining interferences. Silyl-derivatization, with N,N'-methyl-(tert-butyldimethylsilyl) trifluoroacetamide (MTBSTFA), was applied to enhance the sensitivity of detection of phenolic compounds. Quantification was performed by gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) mode, using deuterium-labeled internal standards. Spiking experiments were carried out to determine the recovery, precision and detection limit of the method. The overall recoveries ranged between 70 and 120%, with relative standard deviations of 3-17% for the entire procedure. The detection limits of the method for the nine phenols ranged from 0.02 to 0.41 ng g(-1). The method provided simultaneous screening and accurate confirmation of each phenol when applied to biological samples.
authors.affiliation: Hazardous Substance Research Team, Korea Basic Science Institute, Seoul 136-701, South Korea.
authors.forename: Yun Gyong
authors.initials: YG
authors.lastname: Ahn
authors.forename: Jeoung Hwa
authors.initials: JH
authors.lastname: Shin
authors.forename: Hye-Young
authors.initials: HY
authors.lastname: Kim
authors.forename: Jeehyeong
authors.initials: J
authors.lastname: Khim
authors.forename: Mi-Kyoung
authors.initials: MK
authors.lastname: Lee
authors.forename: Jongki
authors.initials: J
authors.lastname: Hong
mesh_terms: D000818:Animals; D002138:Calibration; D052244:Endocrine Disruptors / Q000032:analysis* / Q000493:pharmacokinetics; D004784:Environmental Monitoring / Q000379:methods*; D005615:Freezing; D008401:Gas Chromatography-Mass Spectrometry; D008055:Lipids / Q000737:chemistry*; D010473:Perciformes / Q000378:metabolism*; D010636:Phenols / Q000032:analysis* / Q000493:pharmacokinetics; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction; D013010:Sonication; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000493:pharmacokinetics
chemical_list: D052244:Endocrine Disruptors; D008055:Lipids; D010636:Phenols; D014874:Water Pollutants, Chemical