Development of a liquid chromatography-tandem mass spectrometry procedure for determination of endocrine disrupting compounds in fish from Mediterranean rivers

J Chromatogr A. 2013 Sep 6;1306:44-58. doi: 10.1016/j.chroma.2013.07.050. Epub 2013 Jul 17.


A new, sensitive and rapid method based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach followed by ultra high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) was developed for the determination of nineteen endocrine disruptors (EDCs) and related compounds belonging to different classes in various fish species. Matrix effect on the analytical performance was evaluated, and thus, internal sample calibration was chosen as the most appropriate approach when analyzing such complex matrices as biota. The procedure provided adequate recoveries in the range from 40% to 103% for most of the compounds, low method detection limits (MDLs) in the range from 0.002 to 3.09ng/g for fish homogenates and high accuracy <20%. The developed method was applied for the analysis of target compounds in homogenates of different fish species from four impacted Mediterranean rivers: Ebro, Llobregat, Júcar and Guadalquivir. Eleven out of the nineteen target EDCs were found at least once in fish homogenates. Llobregat was identified as the most polluted river, where high concentrations were measured in fish homogenates especially for bisphenol A (223.91±11.51ng/g). Tris (2-butoxyethyl) phosphate (TBEP), caffeine, and methyl and benzyl paraben were found in fish from the four river basins.

Keywords: Endocrine disrupting compounds; Fish; Hormones; QuEChERS; UHPLC–MS/MS.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Chromatography, High Pressure Liquid / methods*
  • Endocrine Disruptors / analysis
  • Endocrine Disruptors / metabolism
  • Fishes* / metabolism
  • Mediterranean Region
  • Muscle, Skeletal / chemistry*
  • Muscle, Skeletal / metabolism
  • Rivers / chemistry
  • Tandem Mass Spectrometry / methods*
  • Water Pollutants, Chemical / analysis*
  • Water Pollutants, Chemical / metabolism


  • Endocrine Disruptors
  • Water Pollutants, Chemical