Determination of androgens and progestogens in environmental and biological samples using fabric phase sorptive extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry

• Published in: Journal of Chromatography A Vol. 1437; pp. 116 - 126
• Main Authors: Guedes-Alonso, Rayco, Ciofi, Lorenzo, Sosa-Ferrera, Zoraida, Santana-Rodríguez, José Juan, Bubba, Massimo del, Kabir, Abuzar, Furton, Kenneth G.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 11.03.2016
• Subjects: Androgens; Androgens - analysis; Androgens - urine; Biological; Chromatography, High Pressure Liquid; Endocrine disrupting compounds; Endocrine Disruptors - analysis; Environmental Monitoring - methods; Extraction; Fabrics; Liquid chromatography; Low concentrations; Mass spectrometry; Progestins - analysis; Progestins - urine; Progestogens; Solvents; Tandem Mass Spectrometry; Ultra high performance liquid chromatography; Urinalysis - methods; Urine; Waste Water - chemistry; Wastewater; Water - chemistry; Water Pollutants, Chemical - analysis; Urine; Progestogens; Androgens; Endocrine disrupting compounds; Wastewater; Ultra high performance liquid chromatography
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2016.01.077

•A new fabric phase sorptive extraction combined with UHPLC–MS/MS is proposed.•The method is optimized and validated to determine six androgens and four progestogens.•All extraction and desorption variables have been optimized.•Minimum quantities of sample and organic solvents and short extraction times are used.•Water and urine samples have been successfully analyzed using the proposed method. Androgens and progestogens are two important groups of endocrine disrupting compounds (EDCs) which are implicated to produce severe detrimental impact over aquatic biota, even at very low concentrations of ngL−1. For this reason, one of the major challenges to analytical chemists is the development of sensitive and selective extraction processes which allow the rapid and green determination of these emerging pollutants at low concentrations in environmental samples. Fabric phase sorptive extraction is a new, highly sensitive, efficient and solvent minimized technique which combine the advantages of sol–gel derived microextraction sorbents and the rich surface chemistry of cellulose fabric substrate. This process has several advantages such as minimum usage of organic solvents, short extraction times, small sample volumes and high analyte preconcentration factors. In this study, an extraction method based on sorptive fabric phase coupled to ultra-high-performance liquid chromatography tandem mass spectrometry detection (FPSE-UHPLC–MS/MS) has been developed for the determination of four progestogens and six androgens in environmental and biological samples. All the parameters involved in the extraction, such as sample volume, extraction and desorption times, desorption solvent volume and sample pH values have been optimized. The developed method provides satisfactory limits of detection (between 1.7 and 264ngL−1), good recoveries and low relative standard deviations (below 10% in tap and osmosis water and below 20% in wastewater and urine). Subsequently, the method was used to analyse tap water, wastewater treated with different processing technologies and urine samples. The concentrations of the detected hormones ranged from 28.3 to 227.3 ngL−1 in water samples and from 1.1 to 3.7μgL−1 in urine samples.