A new analytical framework for multi-residue analysis of chemically diverse endocrine disruptors in complex environmental matrices utilising ultra-performance liquid chromatography coupled with high-resolution tandem quadrupole time-of-flight mass spectrometry

Anal Bioanal Chem. 2019 Jan;411(3):689-704. doi: 10.1007/s00216-018-1483-y. Epub 2018 Nov 22.

Abstract

This manuscript presents a comprehensive analytical framework for identification and quantification of chemically diverse endocrine disrupting chemicals (EDCs) used in personal care and consumer products in diverse solid and liquid environmental matrices with an ultimate goal of evaluating public exposure to EDCs via water fingerprinting. Liquid chromatography coupled with tandem quadrupole time-of-flight mass spectrometry (UHPLC-ESI-MS/MS) was used for targeted analysis of selected EDCs as well as to identify and quantify a few metabolites using post-acquisition data mining. Solid-phase extraction (SPE) was applied to liquid matrices in order to reduce matrix effects and provide required sample concentration and ultimately, high sensitivity and selectivity of measurements. SPE recoveries in liquid samples ranged from 49 to 140% with method quantification limits not exceeding 1 ng L-1 for the majority of EDCs. Microwave-assisted extraction (MAE) was applied to solid samples and when followed by SPE, it permitted the analysis of EDCs in digested sludge. MAE/SPE recoveries varied from 11 to 186% and MQLs between 0.03 and 8.1 ng g-1 with the majority of compounds showing MQLs below 2 ng g-1. Mass error for quantifier and qualifier ions was below 5 ppm when analysing river water and effluent wastewater and below 10 ppm when analysing influent wastewater and solid samples. The method was successfully applied to environmental samples, with 33 EDCs identified and quantified in wastewater and receiving waters. In addition, several EDCs were found in digested sludge, which confirms that for a more comprehensive understanding of exposure patterns and environmental impact, analysis of solids cannot be neglected. Finally, post-acquisition data mining permitted the identification and quantification of a metabolite of BPA and the identification of a metabolite of 4-Cl-3-methylphenol. Graphical abstract ᅟ.

Keywords: Endocrine disruptor; Environment; High-resolution LC-MS; Personal care products; Sludge; Wastewater.

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Cosmetics / chemistry
  • Endocrine Disruptors / analysis*
  • Endocrine Disruptors / standards
  • Environmental Monitoring / methods
  • Fresh Water / chemistry
  • Limit of Detection
  • Reference Standards
  • Reproducibility of Results
  • Rivers / chemistry
  • Sewage / chemistry
  • Solid Phase Extraction / methods
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Tandem Mass Spectrometry / methods*
  • Wastewater / chemistry
  • Water Pollutants, Chemical / analysis*
  • Water Pollutants, Chemical / standards

Substances

  • Cosmetics
  • Endocrine Disruptors
  • Sewage
  • Waste Water
  • Water Pollutants, Chemical