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
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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 × 103 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.
KeywordsMass spectrometry Microwave-assisted extraction Sludge Steroid hormones Ultra-high performance liquid chromatography
This work was supported by funds provided by the Spanish Ministry of Economy and Competitiveness, Research Project CTM2015-66095-C2-1-R. Rayco Guedes-Alonso thanks the University of Las Palmas de Gran Canaria (Spain) for his Ph.D. student grant. The authors would also like to thank Emalsa S.A., Acciona S.A. and Consejo Insular de Aguas de Gran Canaria for allowing the sampling of sludge at the different wastewater treatment plants.
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Conflict of interest
The authors declare that they have no competing interests.
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