Application of a magnetic sorbent based on humate in combination with GC-MS for the determination of phenolic xenoestrogens in bottom sediments
Abstract
A sorbent with magnetic properties, functionalized with humates, in combination with gas chromatography–mass spectrometry (GC-MS) was proposed for the determination of phenolic xenoestrogens (ED) in bottom sediments. The following ED were chosen as objects of the study: octylphenol (OP), nonylphenol (NP), bisphenol A (BPA). Together with ED, the distribution of the naturally occurring estrogen, 17β-estradiol (E2), was studied. Previously, ED was extracted from bottom sediments with hexane under short-term sonication with ultrasound. The degree of component extraction was 75-89%. Sorption concentration was carried out under dynamic conditions: a sorbent weighing 0.5 g was placed in a borosilicate glass column, on both sides of which magnets were placed to immobilize the sorbent. The hexane extract was passed through a column filled with a magnetic sorbent based on humates. The analytes were then desorbed with 1 cm3 methanol and their derivatization was carried out with a mixture of N,O-bis(trimethylsilyl)-trifluoroacetamide and trimethylchlorosilane.
The analytical characteristics of the determination method were established using model samples of bottom sediments selected in a background area with minimal anthropogenic impact. The determination limit of ED was 30-60 ng/kg (dry weight). In real objects, the sensitivity of the method was reduced by 3-4 times due to matrix effects caused by the presence of petroleum products in waters. The monitoring of ED content in bottom sediments at the site of waste water discharge into the River Don near the city of Voronezh, as well as on the Black Sea coast of the Caucasus (area of the city of Tuapse and Olginka settlement) was carried out. The maximum concentrations of OP, NP, BPA and E2 in bottom sediments were established in the area of the port of Tuapse, where they were 5.7, 8.1, 6.2, and 0.9 µg/kg, respectively.
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