title: In-syringe magnetic stirring-assisted dispersive liquid-liquid microextraction and silylation prior gas chromatography-mass spectrometry for ultraviolet filters determination in environmental water samples.
abstract: A novel online approach involving in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction and derivatization coupled to gas chromatography-mass spectrometry has been developed for the determination of seven UV filters extensively used in cosmetic products in environmental water samples. The effect of parameters such as the type and volume of extraction solvent, dispersive solvent and derivatization agent, pH, ionic strength and stirring time, was studied using multivariate experimental design. Extraction, derivatization and preconcentration were simultaneously performed using acetone as dispersive solvent, N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) as derivatization agent and trichloroethylene as extraction solvent. After stirring during 160s, the sedimented phase was transferred to a rotary micro-volume injection valve (3 μL) and introduced by an air stream into the injector of the GC through a stainless-steel tube used as interface. The detection limits were in the range of 0.023-0.16 μg L(-1) and good linearity was observed up to 500 μg L(-1) of the studied UV filters, with R(2) ranging between 0.9829 and 0.9963. The inter-day precision expressed as relative standard deviation (n=5) varied between 5.5 and 16.8%. Finally, the developed method was satisfactorily applied to assess the occurrence of the studied UV filters in seawater and pool water samples. Some of the studied UV filters were found in these samples and an add-recovery test was also successfully performed with recoveries between 82 and 111%.
authors.affiliation: Group of Analytical Chemistry, Automation and Environment, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain.
authors.forename: Sabrina
authors.initials: S
authors.lastname: Clavijo
authors.affiliation: Sciware Systems, S.L., Spin-off of the University of the Balearic Islands, C/Pi 37, 07193 Bunyola, Spain.
authors.forename: Jessica
authors.initials: J
authors.lastname: Avivar
authors.affiliation: Group of Analytical Chemistry, Automation and Environment, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain.
authors.forename: Ruth
authors.initials: R
authors.lastname: Suárez
authors.affiliation: Group of Analytical Chemistry, Automation and Environment, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain. Electronic address: victor.cerda@uib.es.
authors.forename: Víctor
authors.initials: V
authors.lastname: Cerdà
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000295:instrumentation*; D012623:Seawater / Q000737:chemistry*; D013473:Sunscreening Agents / Q000032:analysis*; D013594:Syringes; D014867:Water / Q000032:analysis / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D013473:Sunscreening Agents; D014874:Water Pollutants, Chemical; D014867:Water
keywords: Aqueous silylation; Environmental water samples; GC–MS; In-syringe magnetic-stirring-assisted dispersive liquid–liquid microextraction; Online sample treatment; UV filters