4.6 Article

Simplified sample preparation method for triclosan and methyltriclosan determination in biota and foodstuff samples

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1188, Issue 2, Pages 132-139

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2008.02.064

Keywords

triclosan; biota samples; matrix solid-phase dispersion; gas chromatography tandem mass spectrometry

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An improved method for the determination of triclosan (TCS) and methyltriclosan (MTCS) in fish and foodstuff samples is presented. Analytes were simultaneously extracted and purified using the matrix solid-phase dispersion (MSPD) technique, and then selectively determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Several combinations of dispersants, clean-up co-sorbents and extraction solvents were tested in order to obtain lipid-free extracts and quantitative recoveries for TCS and MTCS. Under optimised conditions, 0.5 g samples were dispersed using 1.5 g of neutral silica in a mortar with a pestle, and transferred to a polypropylene cartridge containing 3 g of silica impregnated with 10% of sulphuric acid NO2-H2SO4, 10%, w/w). Analytes were recovered with 10 mL of dichloromethane whereas lipids were oxidized in the layer of acidic silica. The extract was concentrated to dryness and re-constituted with 1 mL of ethyl acetate. Then, a fraction of 0.5 mL was mixed with 50 mu L of N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) and injected in the GC-MS/MS system. The developed method provided absolute recoveries between 77 and 120% for different samples spiked at the low ng g(-1) level, quantification limits in the range of. and a considerable simplicity in comparison with previously developed sample preparation approaches. Experiments carried out placing 1-2 ng g(-1) sliced food samples in direct contact with TCS-treated kitchenware surfaces showed the capability of the biocide to migrate into foodstuffs. (C) 2008 Elsevier B.V. All rights reserved.

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