GC-MS determination of parabens,triclosan and methyl triclosan in water by in situ derivatisation and stir-bar sorptive extraction |
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Authors: | Ana María Casas Ferreira Monika Möder María Esther Fernández Laespada |
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Institution: | 1.Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas,Universidad de Salamanca,Salamanca,Spain;2.Helmholtz Centre for Environmental Research–UFZ,Leipzig,Germany |
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Abstract: | Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption–gas chromatography–mass
spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both
the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same
time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline
conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature)
were optimised using a Box–Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben
(22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The
feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated
wastewater. |
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