| Summary: | This study explored the synthesis and application of amino-functionalised magnetic silica (Fe3O4 @mSiO2-NH2) nanocomposite as a selective sorbent for the extraction of penicillin antibiotics (PENs) from milk samples via magnetic micro-solid phase extraction (M-µ-SPE). The physicochemical characteristics of the synthesised sorbent were evaluated through important spectroscopy analyses. The adopted M-µ-SPE conditions were: 25 mg of Fe3O4 @mSiO2-NH2; pH 4; 3 min of extraction time; 1 min of desorption time; acetonitrile as the desorption solvent; 10 of salt addition; and 30 mL sample. Under the optimum conditions, the developed method demonstrated satisfactory from 10 to 500 µg/L (r2≥0.9986), low limits of detection (2.5–3.1 µg/L), high analytes recovery (85.2–106.7), and good precision (RSDs≤8,n = 5). The proposed method is rapid, simple, inexpensive, and shows good sensitivity when compared to previously developed methods. This study provides new insight into the development of a new sorbent for PENs and new microscale sample preparation for monitoring PENs in complex milk matrices.
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