Evaluation of the application of electric potential in solid phase extraction for the determination of sulfonamides and fluoroquinolones in eggs

Author(s)

Cyntia Cabral Ribeiro

• Document type: Doctoral Thesis
• Press: Campinas, SP.
• Institution: Universidade Estadual de Campinas (UNICAMP). Faculdade de Engenharia de Alimentos
• Defense date: 2014-12-18

Examining board members

Felix Guillermo Reyes Reyes; Isabel Cristina Sales Fontes Jardim; Eduardo Vicente; Sonia Claudia do Nascimento de Queiroz; Adriana Pavesi Arisseto Bragotto

• Advisor: Felix Guillermo Reyes Reyes; Susanne Rath

Abstract

Sulfonamides and fluoroquinolones are veterinary drugs widely used in the poultry production for the prevention and treatment of diseases and, when good veterinary practices are not observed, residues of these drugs can be found above the maximum residue limit and may represent a risk to the consumers health. Since egg is a complex biological matrix, significant amounts of interferents can hinder the determination of analytes by liquid chromatography, particularly residues of veterinary drugs, which are at levels in the order of ng g-1. Among the various sample preparation techniques capable to eliminate interferences and concentrate the analyte of interest, the solid phase extraction (SPE) stands out for its efficiency, robustness, selectivity and low solvent consumption. Nevertheless, due to the complexity of the matrix and the low concentration of the analytes, the establishment of sample preparation methods with selectivity in removing interferents and appropriate extraction efficiency is still a challenge in residue analysis. Thus, in order to overcome the limitations of conventional SPE, this thesis aimed to evaluate the application of electrical potential in SPE (E-SPE) for the determination of sulfonamides and fluoroquinolones residues in eggs by high efficient (HPLC) and ultra efficient (UHPLC) performance liquid chromatography associated with a photodiode array (DAD), fluorescence (FLD) or sequential mass spectrometer (MS/MS) detectors. The E-SPE parameters were evaluated to obtain the best condition for sample preparation and the method for the determination of sulfonamides and fluoroquinolones residues in eggs by E-SPE UHPLC-MS/MS was evaluated for linearity, precision, accuracy, in addition to the effects of suppression or increase of the analytical signal (matrix effect) (AU)

• FAPESP's process: 12/11401-3 - Evaluation of the application of electric potential in solid phase extraction for the determination of sulfonamides in eggs by HPLC-DAD and LC-MS/MS
• Grantee: Cyntia Cabral Ribeiro
• Support Opportunities: Scholarships in Brazil - Doctorate (Direct)