Effective determination of ampicillin in cow milk using a molecularly imprinted polymer as sorbent for sample preconcentration.

The aim of this study was to prepare molecularly imprinted polymers (MIPs) with ampicillin (AMP) and to evaluate the feasibility of these materials for being used as solid phase extraction sorbent for the selective preconcentration and determination of AMP in cow milk samples. MIPs were synthesized by bulk polymerization using methacrylic acid or methyl methacrylate as monomer and ethylene glycol dimethacrylate as cross-linker at different ratios. Characterization of the MIPs were carried out by Fourier-transform infrared spectrometry. The variables affecting the molecularly imprinted solid-phase extraction (MISPE) procedure were optimized. AMP recoveries were higher than 98%, and RSD less than 7%. A preconcentration factor of 20 was reached, which was sufficient to determine AMP at levels allowed by the EU (4µgkg-1) in cow milk. The selectivity of the AMP-MIP was evaluated in presence of other structurally related ß-lactam antibiotics (amoxicillin, oxacillin, penicillin G).

Occurrence of erythromycin residues in sheep milk. Validation of an analytical method.

The paper describes a new and selective analytical sample treatment for quantitative extraction and preconcentration of erythromycin in presence of other macrolide antibiotics in sheep milk samples. The methodology is based on the use of a molecular imprinted polymer (MIP) employed as solid phase extraction sorbent (MISPE). The synthesized material by bulk polymerization using erythromycin (ERY) as template was evaluated as solid phase extraction sorbent, in a novel sample treatment technique that can be coupled to high-performance liquid chromatography with diode-array detector (HPLC-DAD). MIP selectivity was studied for other macrolide antibiotics with similar structures, such as tylosin (TYL), spiramycin (SPI), josamycin (JOS), roxithromycin (ROX) and ivermectin (IVER) getting recoveries for these interferents lower than 35%, for all cases except for ROX, which recoveries were around 85%. The variables affecting the molecularly imprinted solid-phase extraction (MISPE) procedure were optimized to select the best conditions of selectivity and sensitivity to determine ERY at concentration levels established by EU legislation in sheep milk. Under the selected experimental conditions, quantification limit was 24.1 µg kg(-1). Recoveries were higher than 98%, with RSDs between 0.7% and 2%. The proposed MISPE-HPLC method was validated and successfully applied to ERY analysis in sheep milk samples.