title: Pressurized hot water extraction followed by miniaturized membrane assisted solvent extraction for the green analysis of alkylphenols in sediments.
abstract: A novel and Green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol) in sediments was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane assisted solvent extraction (MASE) and liquid chromatography-electrospray ionization tandem mass spectrometry detection (LC-ESI-MS/MS). The extraction conditions were optimized by a Plackett-Burman design in order to minimize the number of assays according to Green principles. Matrix effect was studied and compensated using deuterated labeled standards as surrogate standards for the quantitation of the target compounds. The analytical features of the method were satisfactory: relative recoveries varied between 92 and 103% and repeatability and intermediate precision were <9% for all compounds. Quantitation limits of the method (MQL) ranged from 0.061 (4-n-nonylphenol) to 1.7ngg(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of the exposed methodology. Reagent consumption, analysis time and waste generation were minimized. The "greenness" of the proposed method was evaluated using an analytical Eco-Scale approach and satisfactory results were obtained. The applicability of the proposed method was demonstrated analysing sediment samples of Galicia coast (NW of Spain) and the ubiquity of alkylphenols in the environment was demonstrated.
authors: 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: N
authors: N
authors: Salgueiro-González
authors: 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: I
authors: I
authors: Turnes-Carou
authors: 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: S
authors: S
authors: Muniategui-Lorenzo
authors: 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: P
authors: P
authors: López-Mahía
authors: 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: D
authors: D
authors: Prada-Rodríguez
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D019015:Geologic Sediments / Q000737:chemistry*; D055772:Green Chemistry Technology; D006358:Hot Temperature; D059625:Liquid-Liquid Extraction; D008904:Miniaturization; D010636:Phenols / Q000032:analysis* / Q000302:isolation & purification; D011312:Pressure; D021241:Spectrometry, Mass, Electrospray Ionization; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D010636:Phenols; D014874:Water Pollutants, Chemical; D014867:Water; C025256:nonylphenol; C080417:4-octylphenol; C041594:4-nonylphenol; C105260:4-tert-octylphenol
keywords: Alkylphenols; Analytical Eco-Scale; Green Chemistry; Liquid chromatography tandem mass spectrometry; Miniaturized membrane assisted solvent extraction; Pressurized hot water extraction