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Optimization of matrix solid-phase dispersion conditions for UV filters determination in biota samples
Authors:Noelia Negreira  Isaac Rodríguez  Rosario Rodil  Elisa Rubí  Rafael Cela
Institution:1. Departamento de Química Analítica, Nutrición y Bromatología , Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela , Santiago de Compostela 15782 , Spain noelia.negreira@idaea.csic.es;3. Departamento de Química Analítica, Nutrición y Bromatología , Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela , Santiago de Compostela 15782 , Spain
Abstract:A low solvent consumption method for the determination of eight ultraviolet (UV) filters, displaying low to medium polarities, in freeze-dried samples of marine bivalves and fish is proposed. Matrix solid-phase dispersion (MSPD) and gas chromatography with mass spectrometry (GC-MS) were used as sample preparation and determination techniques, respectively. This work describes the influence of several parameters (type and amount of dispersant and clean-up sorbents, as well as elution solvent) on the yield and the selectivity of the MSPD extraction. Under optimized conditions, samples (0.5?g) were ground with 2?g of Florisil in a mortar with a pestle and transferred into a polypropylene syringe, which contained 1?g of C18 as clean-up sorbent. Analytes were eluted with 5?mL of acetonitrile. This extract was concentrated to dryness, re-constituted with 1?mL of ethyl acetate and injected in the GC-MS system without any further clean-up. The global average recoveries, measured for three different biota samples, spiked at three different levels (between 50 and 1000?ng?g?1), ranged from 80% to 101% with associated standard deviations below 10%. The inter-day precision of the method varied from 4% to 15% and the achieved LOQs (defined for a signal to noise ratio of 10) ranged from 4 to 28?ng?g?1, referred to the freeze-dried matrix. Octocrylene (OCR) was found in some samples of fish and mussels at concentrations between 15 and 20?ng?g?1, referred to dry mass.
Keywords:matrix solid-phase dispersion  UV filters  biota  gas chromatography-mass spectrometry
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