Simplified sample preparation method for triclosan and methyltriclosan determination in biota and foodstuff samples.
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 (SiO2-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 microL 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 1-2 ng g(-1) and a considerable simplicity in comparison with previously developed sample preparation approaches. Experiments carried out placing sliced food samples in direct contact with TCS-treated kitchenware surfaces showed the capability of the biocide to migrate into foodstuffs.
Canosa
P
P
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, Avda de las Ciencias s/n., Santiago de Compostela 15782, Spain.
Rodríguez
I
I
Rubí
E
E
Ramil
M
M
Cela
R
R
D053000:Analytic Sample Preparation Methods / Q000379:methods*; D000818:Animals; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D008055:Lipids / Q000302:isolation & purification; D012822:Silicon Dioxide / Q000737:chemistry; D012997:Solvents / Q000737:chemistry; D013464:Sulfuric Acids / Q000737:chemistry; D013997:Time Factors; D014260:Triclosan / Q000031:analogs & derivatives* / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification
D008055:Lipids; D012997:Solvents; D013464:Sulfuric Acids; D014260:Triclosan; D012822:Silicon Dioxide; C033158:sulfuric acid