Determination of endocrine disruptors in bottom sediments using gas chromatography-mass spectrometry with analyte preconcentration by liquid-liquid and magnetic dispersive solid-phase extraction

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Abstract

A method is proposed for extracting and concentrating six common endocrine disruptors (dimethyl-, diethyl-, dibutyl phthalates, bisphenol A, octyl- and nonylphenols) from river bottom sediments. The analytes were extracted using a two-stage concentration approach. In the first stage, analytes were extracted from aqueous solution using an ionic liquid – 1-hexyl-3-methylimidazolium hexafluorophosphate – in the presence of a surfactant (sodium dodecylsulfonate). The volumes used were 200 μL of extractant and 0.5 mL of 12 % surfactant solution, with a 2-minute extraction time. In the second stage, magnetic dispersive solid-phase extraction was performed using magnetically active plant-based carbon modified with reverse-phase reagents – n-octyltrimethoxysilane and n-octadecyltrimethoxysilane. The analyte recovery was 91–99 % for liquid-liquid extraction and 89–99 % for magnetic dispersive extraction. Optimal extraction conditions were pH 5.2–7.0, 5 minutes sorption time using centrifugation at 4000 rpm, and 25 mg of sorbent. The two-stage concentration method, combined with gas chromatography-mass spectrometry, enabled detection of endocrine disruptors in bottom sediments at levels of 0.4–0.7 µg/kg.

About the authors

A. S. Gubin

Voronezh State University of Engineering Technologies

Email: goubinne@mail.ru
Revolution Avenue, 19, Voronezh, 394036 Russia

K. S. Sypko

Voronezh State University of Engineering Technologies; North-Caucasus Federal University

Revolution Avenue, 19, Voronezh, 394036 Russia; Pushkin Street, 1, Stavropol, 355017 Russia

A. A. Kushnir

Voronezh State University of Engineering Technologies

Revolution Avenue, 19, Voronezh, 394036 Russia

P. T. Sukhanov

Voronezh State University of Engineering Technologies

Revolution Avenue, 19, Voronezh, 394036 Russia

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