Application of microwave-assisted extraction and ultra-high performance liquid chromatography-tandem mass spectrometry for the analysis of sex hormones and corticosteroids in sewage sludge samples

Anal Bioanal Chem. 2016 Sep;408(24):6833-44. doi: 10.1007/s00216-016-9810-7. Epub 2016 Aug 8.

Abstract

Hormonal compounds are a concern to the international community because they can affect the aquatic biota and are therefore considered to be endocrine-disrupting compounds. These compounds have lipophilic properties, so they tend to accumulate in solid matrices, such as sewage sludge. This work presents the optimization of a microwave-assisted extraction process combined with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of 15 hormonal compounds in sludge samples. The proposed method has relative standard deviations below 23 %, good recoveries (over 71 %) for all compounds, detection limits that ranged from 1.1 to 7.9 ng g(-1) and quantification limits which ranged from 3.7 to 26.3 ng g(-1). The method was used to analyse sludge samples from four different wastewater treatment plants of Gran Canaria (Spain) with different wastewater treatments. 17β-estradiol, 17α-ethynylestradiol, norgestrel and cortisone were detected in sludge samples at concentrations that ranged from 17.3 to 1.44 × 10(3) ng g(-1). The developed method permits the use of small quantities of sample and organic solvents, presents short extractions times and is the first one based on microwave-assisted extraction for the analysis of both sex hormones and corticosteroids.

Keywords: Mass spectrometry; Microwave-assisted extraction; Sludge; Steroid hormones; Ultra-high performance liquid chromatography.

Publication types

  • Evaluation Study

MeSH terms

  • Adrenal Cortex Hormones / analysis*
  • Chromatography, High Pressure Liquid / methods*
  • Gonadal Steroid Hormones / analysis*
  • Limit of Detection
  • Microwaves
  • Sewage / analysis*
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods*
  • Water Pollutants, Chemical / analysis*

Substances

  • Adrenal Cortex Hormones
  • Gonadal Steroid Hormones
  • Sewage
  • Water Pollutants, Chemical