Online fully automated SPE-HPLC-MS/MS determination of ceftiofur in bovine milk samples employing a silica-anchored ionic liquid as sorbent

Autor(es)

Ferreira, Debora Cecatto ^[1] ; de Toffoli, Ana Lucia ^[1] ; Soares Maciel, Edvaldo Vasconcelos ^[1] ; Lancas, Fernando Mauro ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Inst Chem Sao Carlos, Postal Code 780, BR-13560970 Sao Carlos, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: ELECTROPHORESIS; v. 39, n. 17, p. 2210-2217, SEP 2018.
• Citações Web of Science: 3

Resumo

Solid-phase extraction coupled online with high performance liquid chromatography and tandem mass spectrometry was successfully applied to determine low concentrations of ceftiofur antibiotic in bovine milk samples. A silica-anchored ionic liquid was applied as sorbent material to be used as extraction phase in the proposed online system. The material was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. In order to improve the system reproducibility, the following experimental parameters were optimized: organic solvent percentage, time and sample loading flow rate. Subsequently, the method was validated presenting satisfactory results as adequate selectivity, good linearity and correlation coefficient higher than 0.98. The limit of detection and quantification were 0.1 and 0.7 mu g/L, respectively. The precision of the methodology was evaluated as repeatability and intermediate precision, with relative standard deviation values lower than 15%. The accuracy of the method ranged from 72.8 to 137% and the minimum and maximum recovery values were 73.4 and 111.3%, respectively. After the validation, seven milk samples were analyzed and although ceftiofur was not detected in any of them the method was demonstrated to be efficient when applied to the analysis of milk samples fortified with the pollutant of interest. (AU)

• Processo FAPESP: 15/15462-5 - Emprego do grafeno como material sorvente em técnicas miniaturizadas de preparo de amostra.
• Beneficiário: Bruno Henrique Fumes
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 14/07347-9 - Desenvolvimento de novos materiais e dispositivos para técnicas miniaturizadas de preparo de amostras na área de segurança alimentar
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Regular