title: Optimization of pressurized liquid extraction and purification conditions for gas chromatography-mass spectrometry determination of UV filters in sludge.
abstract: This work presents an effective sample preparation method for the determination of eight UV filter compounds, belonging to different chemical classes, in freeze-dried sludge samples. Pressurized liquid extraction (PLE) and gas chromatography-mass spectrometry (GC-MS) were selected as extraction and determination techniques, respectively. Normal-phase, reversed-phase and anionic exchange materials were tested as clean-up sorbents to reduce the complexity of raw PLE extracts. Under final working conditions, graphitized carbon (0.5 g) was used as in-cell purification sorbent for the retention of co-extracted pigments. Thereafter, a solid-phase extraction cartridge, containing 0.5 g of primary secondary amine (PSA) bonded silica, was employed for off-line removal of other interferences, mainly fatty acids, overlapping the chromatographic peaks of some UV filters. Extractions were performed with a n-hexane:dichloromethane (80:20, v:v) solution at 75°C, using a single extraction cycle of 5 min at 1500 psi. Flush volume and purge time were set at 100% and 2 min, respectively. Considering 0.5 g of sample and 1 mL as the final volume of the purified extract, the developed method provided recoveries between 73% and 112%, with limits of quantification (LOQs) from 17 to 61 ng g(-1) and a linear response range up to 10 μg g(-1). Total solvent consumption remained around 30 mL per sample. The analysis of non-spiked samples confirmed the sorption of significant amounts of several UV filters in sludge with average concentrations above 0.6 μg g(-1) for 3-(4-methylbenzylidene) camphor (4-MBC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OC).
authors.affiliation: 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.
authors.forename: N
authors.initials: N
authors.lastname: Negreira
authors.forename: I
authors.initials: I
authors.lastname: Rodríguez
authors.forename: E
authors.initials: E
authors.lastname: Rubí
authors.forename: R
authors.initials: R
authors.lastname: Cela
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry*; D013473:Sunscreening Agents / Q000032:analysis* / Q000302:isolation & purification; D013696:Temperature; D013997:Time Factors
chemical_list: D012722:Sewage; D013473:Sunscreening Agents