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Determination of sulfonamides in beeswax by liquid chromatography coupled to tandem mass spectrometry

Mitrowska, Kamila, Antczak, Maja
Journal of Chromatography B 2015 v.1006 pp. 179-186
acetic acid, acetonitrile, beeswax, cation exchange, cleaning, detection limit, hexane, isopropyl alcohol, liquid chromatography, melting, solid phase extraction, sulfonamides, tandem mass spectrometry
The manuscript presents the development of a new method for the quantification of 16 sulfonamides in beeswax. Different sample preparation techniques were tested and modified to maximise the recovery of the target analytes and minimise the amount of coeluted impurities under conditions that provide reproducible results. The proposed method consisted of melting and dilution of beeswax in a mixture of n-hexane and isopropanol followed by extraction with 2% acetic acid. The extract was cleaned up by solid-phase extraction using strong cation exchange phase. Determination of the sulfonamides was achieved by liquid chromatography coupled to tandem mass spectrometry with the use of a pentafluorophenyl analytical column and applying a gradient elution with acetonitrile and 0.01% acetic acid as mobile phases. The limits of detection and limits of quantification ranged from 1 to 2μg/kg and from 2 to 5μg/kg, respectively. The recoveries varied between 65.2% and 117.8% while coefficient of variation of the method was less than 24.2% under intermediate precision conditions. Finally, the method was applied to the analysis of real samples of beeswax from beekeepers and commercial foundations manufacturers.