A simple and sensitive UFLC-fluorescence method for endocrine disrupters determination in marine waters

作者：Li**oa Normando S; Fahning Cristiane S; Cotrim Gabriel; dos Anjos Jeancarlo P; de Andrade Jailson B; Hatje Vanessa; da Rocha Gisele O^*

来源：Talanta, 2013, 117: 168-175.

DOI：10.1016/j.talanta.2013.08.006

• Endocrine disrupters
• Seawater
• Liquid chromatography with fluorescence detection
• Todos os Santos Bay
• Contaminants of emerging concern

The present study proposes a fast and simple analytical methodology employing 08 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 (El), 17 beta-estradiol (E2) and 17 alpha-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 x 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 degrees 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 (El), 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.

• 出版日期2013-12-15