Determination of 26 endocrine disrupting chemicals in fish and water using modified QuEChERS combined with solid-phase extraction and UHPLC-MS/MS

Abstract

Endocrine-disrupting chemicals (EDCs) in the environment have adverse effects on humans and wildlife. A method based on ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the determination of 26 EDCs (including five estrogens, eight androgens, three progestogens, six glucocorticoids, two mineralocorticoids and two thyroid hormones) in fish and water was developed. Various experimental parameters that could affect the extraction efficiencies were investigated in detail. The sample was extracted by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method with 20 mL of acetonitrile (for fish) or 5 mL of ethyl acetate (for water), and then cleaned-up using an Oasis HLB SPE (solid-phase extraction) cartridge. The analytes were quantified using an isotope-labelled internal standard and recoveries between 69.1% and 120.5% were obtained. The relative standard deviation of inter- and intra-day analyses for all the compounds was below 20%. The detection limits ranged from 0.01 to 0.98 ng mL⁻¹ for water and 0.01 to 9.04 ng g⁻¹ for fish. For real samples, progesterone and trenbolone were detected in zebrafish (Danio rerio) samples at 5.73 ± 0.21 and 7.45 ± 0.34 ng g⁻¹, respectively. There was no target analyte detected in tap-water samples. The developed method would be useful for monitoring EDC abuse in fishery, potential EDC screening and risk assessment in aquatic toxicology.