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

Talanta. 2013 Dec 15:117:168-75. doi: 10.1016/j.talanta.2013.08.006. Epub 2013 Sep 9.

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.

Keywords: Contaminants of emerging concern; Endocrine disrupters; Liquid chromatography with fluorescence detection; Seawater; Todos os Santos Bay.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles
  • Brazil
  • Chromatography, Liquid / methods*
  • Endocrine Disruptors / analysis*
  • Estradiol / analogs & derivatives
  • Estradiol / analysis*
  • Fluorescence
  • Limit of Detection
  • Phenols / analysis*
  • Reproducibility of Results
  • Seawater / chemistry*

Substances

  • Acetonitriles
  • Endocrine Disruptors
  • Phenols
  • Estradiol
  • acetonitrile