title: Analysis of endocrine disruptor compounds in marine sediments by in cell clean up-pressurized liquid extraction-liquid chromatography tandem mass spectrometry determination.
abstract: A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found.
authors.affiliation: Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
authors.forename: N
authors.initials: N
authors.lastname: Salgueiro-González
authors.affiliation: Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
authors.forename: I
authors.initials: I
authors.lastname: Turnes-Carou
authors.affiliation: Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain. Electronic address: smuniat@udc.es.
authors.forename: S
authors.initials: S
authors.lastname: Muniategui-Lorenzo
authors.affiliation: Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
authors.forename: P
authors.initials: P
authors.lastname: López-Mahía
authors.affiliation: Grupo Química Analítica Aplicada (QANAP), Instituto Universitario de Medio Ambiente (IUMA), Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus de A Coruña, E-15071 A Coruña, Spain.
authors.forename: D
authors.initials: D
authors.lastname: Prada-Rodríguez
mesh_terms: D001559:Benzhydryl Compounds / Q000032:analysis; D002853:Chromatography, Liquid / Q000379:methods; D052244:Endocrine Disruptors / Q000032:analysis*; D019015:Geologic Sediments / Q000032:analysis*; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods*; D010636:Phenols / Q000032:analysis; D011312:Pressure; D053719:Tandem Mass Spectrometry / Q000379:methods*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D052244:Endocrine Disruptors; D010636:Phenols; C025256:nonylphenol; C080417:4-octylphenol; C041594:4-nonylphenol; C105260:4-tert-octylphenol; C006780:bisphenol A; D000098826:Bisphenol A Compounds
keywords: Alkylphenols; Bisphenol A; Liquid chromatography tandem mass spectrometry; Marine environment; Pressurized liquid extraction; Sediment