title: Occurrence of erythromycin residues in sheep milk. Validation of an analytical method.
abstract: 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.
authors: Department of Analytical Sciences, Faculty of Sciences, National University of Distance, Madrid 28040, Spain.
authors: M A
authors: MA
authors: García-Mayor
authors: Department of Analytical Sciences, Faculty of Sciences, National University of Distance, Madrid 28040, Spain.
authors: G
authors: G
authors: Paniagua-González
authors: Department of Chemistry, Faculty of Engineering, Universidad Católica Andrés Bello, Caracas, Venezuela.
authors: B
authors: B
authors: Soledad-Rodríguez
authors: Department of Analytical Sciences, Faculty of Sciences, National University of Distance, Madrid 28040, Spain. Electronic address: rmgarcinuno@ccia.uned.es.
authors: R M
authors: RM
authors: Garcinuño-Martínez
authors: Department of Analytical Sciences, Faculty of Sciences, National University of Distance, Madrid 28040, Spain.
authors: P
authors: P
authors: Fernández-Hernando
authors: Department of Analytical Sciences, Faculty of Sciences, National University of Distance, Madrid 28040, Spain.
authors: J S
authors: JS
authors: Durand-Alegría
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis*; D004917:Erythromycin / Q000032:analysis*; D005504:Food Analysis / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D011108:Polymers / Q000737:chemistry; D034561:Sheep, Domestic; D052616:Solid Phase Extraction
chemical_list: D000900:Anti-Bacterial Agents; D011108:Polymers; D004917:Erythromycin
keywords: Erythromycin; HPLC-DAD; Molecularly imprinted solid-phase extraction; Sheep milk