Determination of stilbenes and resorcylic acid lactones in bovine, porcine and poultry muscle tissue by liquid chromatography–negative ion electrospray mass spectrometry and QuEChERS for sample preparation

• A LC–MS/MS method was developed and validated for quantification and confirmation of RALs and stilbenes in muscle tissue.
• Application of QuEChERS simplifies sample preparation by reducing number of steps and shortens the time of analysis.
• Core–shell, smaller pore size chromatography column improves chromatography.
• The method was proved to be sensitive, rapid, accurate and steady.

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 (150 mm × 2.1 mm, 2.7 μm) 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 1 μg kg−1 and not exceed 0.23 μg kg−1 and 0.39 μg kg−1, respectively. The elaborated method meets the criteria for confirmatory methods and is used in the official control of hormones.