title: A simple and sensitive UFLC-fluorescence method for endocrine disrupters determination in marine waters.
abstract: The present study proposes a fast and simple analytical methodology employing C18 SPE cartridges (for preconcentration and clean-up), and a ultra-fast liquid chromatography coupled to fluorescence detector (UFLC-FLD) for determination of the following endocrine disrupters (ED): bisphenol A (BPA), 4-n-nonylphenol (4NNP), 4-n-octylphenol (4NOP), 4-t-octylphenol (4TOP), estriol (E3), estrone (E1), 17β-estradiol (E2) and 17α-ethynylestradiol (EE2) in seawater. The proposed method was developed, optimized and validated. Separation was done by a total running time of 10 min in a Shim-pack XR-ODS C-18 (2.0 mm ID × 50 mm) chromatographic column, mobile phases were acetonitrile/ultra-pure water under gradient programming; eluent flow rate at 0.120 mL min(-1); column temperature set at 60 °C; emission wavelength of 306 nm and excitation wavelength of 280 nm. The method was validated through assessment of the following parameters: linear range, linearity, selectiveness, precision, recovery test, limit of detection (LOD), and limit of quantification (LOQ). Recoveries ranged from 91% (for EE2) to 104% (for 4NNP) and also was found a suitable repeatability (RSD <4.5%) for all considered compounds. LOD and LOQ ranged from 2.0 ng L(-1) (EE2) to 23 ng L(-1) (E1) and 9.3 ng L(-1) (EE2) to 96 ng L(-1) (E1), respectively. The analytical method using SPE UFLC-FLD was applied to seawater samples collected from Todos os Santos Bay (BTS), Brazil to determine the concentration of eight ED.
authors.affiliation: Instituto de Química, Universidade Federal da Bahia, 40170-290 Salvador, BA, Brazil.
authors.forename: Normando S
authors.initials: NS
authors.lastname: Lisboa
authors.forename: Cristiane S
authors.initials: CS
authors.lastname: Fahning
authors.forename: Gabriel
authors.initials: G
authors.lastname: Cotrim
authors.forename: Jeancarlo P
authors.initials: JP
authors.lastname: dos Anjos
authors.forename: Jailson B
authors.initials: JB
authors.lastname: de Andrade
authors.forename: Vanessa
authors.initials: V
authors.lastname: Hatje
authors.forename: Gisele O
authors.initials: GO
authors.lastname: da Rocha
mesh_terms: D000097:Acetonitriles; D001938:Brazil; D002853:Chromatography, Liquid / Q000379:methods*; D052244:Endocrine Disruptors / Q000032:analysis*; D004958:Estradiol / Q000031:analogs & derivatives / Q000032:analysis*; D005453:Fluorescence; D057230:Limit of Detection; D010636:Phenols / Q000032:analysis*; D015203:Reproducibility of Results; D012623:Seawater / Q000737:chemistry*
chemical_list: D000097:Acetonitriles; D052244:Endocrine Disruptors; D010636:Phenols; D004958:Estradiol; C032159:acetonitrile
keywords: Contaminants of emerging concern; Endocrine disrupters; Liquid chromatography with fluorescence detection; Seawater; Todos os Santos Bay