Fast and simple determination of estrogens in milk powders by magnetic solid-phase extraction using carbon nitride compo
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RESEARCH PAPER
Fast and simple determination of estrogens in milk powders by magnetic solid-phase extraction using carbon nitride composites prior to HPLC Na Li 1 & Tengwen Zhao 1 & Li Du 1 & Ziyang Zhang 1 & Qixun Nian 1 & Manman Wang 1 Received: 29 June 2020 / Revised: 25 September 2020 / Accepted: 6 October 2020 # Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract A graphitic carbon nitride (g-C3N4/Fe3O4)–based magnetic solid-phase extraction (MSPE) approach was established for fast and simple analysis of estrogens in milk powders. The composites were characterized by X-ray diffractometer, scanning electron microscope, and Brunauer-Emmett-Teller surface area and pore size distribution analyzer. Compared with the bulk g-C3N4, gC3N4/Fe3O4 gave a narrower distribution of mesopores and provided an enhanced surface area from 77.1 to 113.7 m2/g. Polar analytes of estrogens were selected as model compounds and the extraction of four estrogens was achieved in n-hexane using 15 mg of adsorbent within only 2 min. Possible extraction mechanism of g-C3N4/Fe3O4 for these estrogens was explored in terms of the polarity of the analytes and the adsorption performance of the adsorbent. The hydrophobicity and the hydrogen-bond interaction between the estrogens and g-C3N4 were responsible for the efficient adsorption. Combined with HPLC, MSPE with the prepared adsorbent gave the enhancement factors of 20 to 24 and the linear ranges of 2–200 μg/kg for 17β-estradiol and 17αethinylestradiol, 1.5–150 μg/kg for estrone, and 3–300 μg/kg for hexestrol. The detection limits and quantification limits for the estrogens in milk powders were 0.5–0.9 μg/kg and 1.5–3.0 μg/kg, respectively. The recoveries varied from 75.1 to 97.2%, with the intra-day and inter-day precisions ≤ 14.2%. Furthermore, the enrichment of the analytes and the clean-up of fat and protein interferences were achieved simultaneously with one-step g-C3N4-based MSPE. The present method was convenient, fast, and sensitive, and therefore could be successfully applied for the determination of estrogens in milk powders. Keywords Graphitic carbon nitride . Magnetic solid-phase extraction . Estrogens . Milk powder . High-performance liquid chromatography
Introduction Estrogens as a class of steroid hormones are responsible for the function of the endocrine system both in wildlife and in human beings at low concentrations in terms of the high estrogenic activities. These compounds may block or mimic the normal effect of hormones and adjust hormone receptor levels [1, 2]. Considering their use in stock farming for growth Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02993-y) contains supplementary material, which is available to authorized users. * Manman Wang [email protected] 1
School of Public Health, North China University of Science and Technology, No.21 Bohai Road, Caofeidian, Tangshan 063210, Hebei, China
promotion and milk production increase, hexestrol (HEX) and ethinylestradiol (EE) are listed
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