Application of solid-phase extraction coupled with freezing-lipid filtration clean-up for the determination of endocrine-disrupting phenols in fish

Yun Gyong Ahn, Jeoung Hwa Shin, Hye Young Kim, Jeehyeong Khim, Mi Kyoung Lee, Jongki Hong

Research output: Contribution to journalArticle

60 Citations (Scopus)

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.

Original languageEnglish
Pages (from-to)67-75
Number of pages9
JournalAnalytica Chimica Acta
Volume603
Issue number1
DOIs
Publication statusPublished - 2007 Nov 5

Keywords

  • Endocrine-disrupting phenols
  • Fish
  • Freezing-lipid filtration
  • Gas chromatography/mass spectrometry
  • Silyl-derivatization
  • Solid-phase extraction

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Environmental Chemistry
  • Spectroscopy

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