Magnetic solid-phase extraction with dispersion of magnetic hypercrosslinked polystyrene with carbon dioxide for the isolation of amphenicols from honey and milk in their determination by HPLC-MS/MS

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Abstract

The magnetic solid phase extraction method with the dispersion of magnetic hypercrosslinked polystyrene (MHCPS) with carbon dioxide is proposed for the isolation and concentration of amphenicols (chloramphenicol, florfenicol and thiamphenicol) from honey and milk before their determination by HPLC-MS/MS. Effervescent tablets consisting of sodium bicarbonate, citric acid and MHCPS in the case of honey, sodium bicarbonate and MHCPS in case of milk were used. The conditions for the preparation of tablets (the amount and ratio of acid, base and MHCPS in the composition of the tablet and its mass) were selected, ensuring the quantitative isolation of amphenicols. Methods for the determination of amphenicols in honey and milk with dispersion of the sorbent with carbon dioxide and subsequent determination of compounds by HPLC-MS/MS have been developed. The limits of determination were 0.3–1 and 0.02–0.05 µg/kg for honey and milk, respectively.

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About the authors

N. O. Goncharov

Lomonosov Moscow State University

Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991

V. V. Tolmacheva

Lomonosov Moscow State University

Author for correspondence.
Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991

T. V. Lazarevich

Lomonosov Moscow State University; Universität Leipzig

Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991; Augustus pl., 10, 04109 Leipzig, Germany

A. O. Melekhin

Federal Center for Animal Health

Email: nikatolm@mail.ru
Russian Federation, Yuryevets, Vladimir, 6009101

I. D. Puryskin

Lomonosov Moscow State University

Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991

V. V. Apyari

Lomonosov Moscow State University

Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991

S. G. Dmitrienko

Lomonosov Moscow State University

Email: nikatolm@mail.ru

Faculty of Chemistry

Russian Federation, GSP-1, Leninskie gory, 1, p. 3, Moscow 119991

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2. Fig. 1. The degree of extraction of amphenicols depending on the molar ratio of hydrocarbonate and citric acid (a) and the content of MHCPS (b) in the composition of tablets for MTFE-CO2. V = 25 ml, mMCSPS = 10 mg (a), molar ratio NaHCO3 : C6H8O7 3 : 1 (b).

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3. Fig. 2. Mass chromatograms of isolated ions of honey (a) and milk (b) extracts with the addition of 100 and 8 μg/kg amphenicols, respectively, after purification by magnetic solid-phase extraction with dispersion of magnetic hyper-cross-linked polystyrene with carbon dioxide.

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