Abstract
Liquid chromatography tandem mass spectrometry method was developed and validated to confirm of resorcylic acid lactones: zeranol, taleranol, zearalanone, zearalenone, α and β-zearalenol and stilbenes in muscle tissue. The compounds were analyzed by LC-MS/MS QTrap 5500 apparatus in negative ionization mode. Chromatographic separation on Poroshell 120-EC C18 (150mm×2.1mm, 2.7μm) column was achieved at 45°C using isocratic elution of mobile phase - methanol/water (65:35, v/v). For the treatment of tissue samples prior to analysis, QuEChERS method was applied based on the extraction of analytes from muscle samples with ethyl acetate, separation of the aqueous and organic phases with application of magnesium sulphate and sodium acetate, the purification of the extract obtained by dispersive SPE with the use of sorbent C18, PSA and magnesium sulphate. The method was validated in accordance with the Commission Decision 2002/657/EC. Good recoveries were obtained (from 83% to 115%) as well as acceptable within-lab reproducibility (<22%). The values of the decision limit CCα and the detection capability CCβ for individual compounds are found to be below the recommended concentration set at 1μgkg(-1) and not exceed 0.23μgkg(-1) and 0.39μgkg(-1), respectively. The elaborated method meets the criteria for confirmatory methods and is used in the official control of hormones.
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