title: Development of a new sorptive extraction method based on simultaneous direct and headspace sampling modes for the screening of polycyclic aromatic hydrocarbons in water samples.
abstract: A new straightforward and inexpensive sample screening method for both EPA and EU priority polycyclic aromatic hydrocarbons (PAHs) in water has been developed. The method is based on combined direct immersion and headspace (DIHS) sorptive extraction, using low-cost disposable material, coupled to ultraperformance liquid chromatography with fluorescence and UV detection (UPLC-FD-UV). Extraction parameters, such as the sampling mode, extraction time and ionic strength were investigated in detail and optimized. Under optimized conditions, water samples (16 mL) were concentrated in silicone disks by headspace (HS) and direct immersion (DI) modes simultaneously, at room temperature for 9h for the majority of the 24 studied compounds. Ultrasound-assisted desorption of extracted analytes in acetonitrile was carried out also at room temperature. The optimized chromatographic method provided a good linearity (R≥0.9991) and a broad linear range for all studied PAHs. The proposed analytical procedure exhibited a good precision level with relative standard deviations below 15% for all analytes. Quantification limits between 0.7 and 2.3 µg L(-1) and 0.16 and 3.90 ng L(-1) were obtained for compounds analyzed by UV (acenaphtylene, cyclopenta[c,d]pyrene and benzo[j]fluoranthene) and fluorescence, respectively. Finally, the proposed method was applied to the determination of PAHs in different real tap, river and wastewater samples.
authors.affiliation: Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: Sara
authors.initials: S
authors.lastname: Triñanes
authors.affiliation: Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: Ma Teresa
authors.initials: MT
authors.lastname: Pena
authors.affiliation: Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain. Electronic address: carmela.casais@usc.es.
authors.forename: Ma Carmen
authors.initials: MC
authors.lastname: Casais
authors.affiliation: Departamento Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: Ma Carmen
authors.initials: MC
authors.lastname: Mejuto
mesh_terms: D000073:Acenaphthenes / Q000032:analysis; D000097:Acetonitriles; D000327:Adsorption; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D060766:Drinking Water / Q000737:chemistry*; D005449:Fluorenes / Q000032:analysis; D005618:Fresh Water / Q000737:chemistry*; D006801:Humans; D057230:Limit of Detection; D009994:Osmolar Concentration; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*; D011721:Pyrenes / Q000032:analysis; D012828:Silicones / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000379:methods*; D013010:Sonication; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000073:Acenaphthenes; D000097:Acetonitriles; D060766:Drinking Water; D005449:Fluorenes; D011084:Polycyclic Aromatic Hydrocarbons; D011721:Pyrenes; D012828:Silicones; D062065:Wastewater; D014874:Water Pollutants, Chemical; C042553:acenaphthylene; C027704:benzo(j)fluoranthene; C016328:cyclopenta(c,d)pyrene; C032159:acetonitrile
keywords: Polycyclic aromatic hydrocarbons; Silicone sorbents; Sorptive extraction; Ultra-high performance liquid chromatography; Water analysis