Simultaneous determination of progestogens, androgens, estrogens and phenols in water, sediment and biological samples by enolisation–silylation with ASE-GPC-SPE-GC/MS

摘要: This research has developed an enolisation–silylation with accelerated solvent extraction (ASE)-automated gel permeation chromatography (GPC)-solid phase (SPE)-gas chromatography/mass spectrometry (GC/MS) analytical method for the simultaneous determination of twelve steroidal and phenolic endocrine disrupting chemicals (EDCs) in water, sediment biological samples. The parameters ASE have been optimized as follows: ethyl acetate solvent, a static time 5 min, 3 cycles at 80 °C 60 samples, respectively. Clean-up extracts was carried out by GPC Sep-Pak C18 cartridges. target compounds were eluted fraction from 7–14 min retention time, then obtained solid cartridges after elution 15 mL acetate. final sample derivatized using N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA)/trimethyliodosilane (TMIS)/dithioerythreitol (DTE) (1000 : 2 : 5; v/v/w) derivatization reagent. Quantification performed gas chromatography-mass (GC-MS) electron ionisation (EI) selected ion monitoring (SIM) mode. validated spiking experiments which showed low detection limits, good recovery (60.28% to 95.46%) reproducibility (RSD < 10%). proposed methods successfully applied EDCs environmental samples taken Laoyu River local market Yunnan, China. had better practicability feasibility progestogens, androgens, estrogens phenols technique is more fast, simple precise than some other methods, wide range applications. It beneficial study occurrence, fate bioaccumulation these environment.