Abstract

This paper presents a novel and reliable approach for the determination of tilmicosin residues in poultry muscle and pork via gas chromatography–tandem mass spectrometry after precolumn derivatization. The samples were subjected to a quick, easy, cheap, effective, rugged, and safe preparation method, solid-phase extraction, hydrogenation, gel chromatography separation, acid hydrolysis, and derivatization with pyridine and acetic anhydride. For the blank spiked samples at the limit of quantification, 0.5 times the maximum residue limit (MRL), the MRL, and 2.0 times the MRL, the recoveries were from 76.91 to 87.99% with a precision of 2.04–5.47%. The limits of detection and quantification were 2.3–4.4 and 6.2–9.8 µg kg−1, respectively. The protocol was validated and real samples analyzed to demonstrate its practical application.

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