Extraction Of Tetracyclinic Antibiotic Residues From Fish Filet: Comparison And Optimization Of Different Procedures Using Liquid Chromatography With Fluorescence Detection.

dc.creatorOrlando, Eduardo Adilson
dc.creatorSimionato, Ana Valéria C
dc.date2013-Sep
dc.date2015-11-27T13:32:04Z
dc.date2015-11-27T13:32:04Z
dc.date.accessioned2018-03-29T01:18:21Z
dc.date.available2018-03-29T01:18:21Z
dc.identifierJournal Of Chromatography. A. v. 1307, p. 111-8, 2013-Sep.
dc.identifier1873-3778
dc.identifier10.1016/j.chroma.2013.07.084
dc.identifierhttp://www.ncbi.nlm.nih.gov/pubmed/23932025
dc.identifierhttp://repositorio.unicamp.br/jspui/handle/REPOSIP/200778
dc.identifier23932025
dc.identifier.urihttp://repositorioslatinoamericanos.uchile.cl/handle/2250/1301011
dc.descriptionAnti-microbials have been used to control the quality of the aquatic environment for both prophylactic and therapeutic purposes. Tetracyclines are among the main antimicrobials used in aquaculture, and present a particular difficulty for extraction, due to a complex structure and high interaction with components of the biological matrix. In this study, different techniques of extraction and clean-up of antimicrobials of the tetracycline class in tilapia filets have been optimized and compared, followed by validation of the methodology using the best procedure. Oxytetracycline, doxycycline, tetracycline and chlortetracycline were analyzed by HPLC-fluorescence under the following conditions: organic mobile phase composed of methanol:acetonitrile (1:1, v/v) and aqueous mobile phase containing sodium acetate (0.0375molL(-1)), calcium chloride (0.0175molL(-1)) and EDTA (0.0125molL(-1)) at pH 7.00. The chromatographic analysis was performed using a mobile phase gradient with a flow rate of 1mLmin(-1) and detection wavelength of 385/528nm (λexc/λem). Four extraction methods have been evaluated, namely: liquid-liquid partition; solid phase extraction (SPE) using phenyl, C18 and polymeric Oasis-HLB stationary phases; dispersive SPE (dSPE) using polymeric adsorbent XAD 16 resin; and QuEChERS. The methods have been optimized with fractional factorial experimental design and compared by the extraction efficiency. The liquid-liquid extraction and the QuEChERS methods showed low extraction efficiencies (14-30%) for the analytes. The use of dSPE showed good efficiency (40-60%), but with low precision and high consumption of time. Among the evaluated extraction techniques the use of SPE showed the best results, with emphasis on the phenyl phase (58-76%), and has been validated for analysis of residues of tetracyclines in tilapia muscle regarding selectivity, linearity, precision and limits of detection and quantification. The validated method was adequate for the investigation of the analytes at residue levels.
dc.description1307
dc.description111-8
dc.languageeng
dc.relationJournal Of Chromatography. A
dc.relationJ Chromatogr A
dc.rightsfechado
dc.rightsCopyright © 2013 Elsevier B.V. All rights reserved.
dc.sourcePubMed
dc.subjectAnimals
dc.subjectAnti-bacterial Agents
dc.subjectChromatography, High Pressure Liquid
dc.subjectDrug Residues
dc.subjectHydrogen-ion Concentration
dc.subjectLinear Models
dc.subjectLiquid-liquid Extraction
dc.subjectReproducibility Of Results
dc.subjectSeafood
dc.subjectSensitivity And Specificity
dc.subjectSolid Phase Extraction
dc.subjectSpectrometry, Fluorescence
dc.subjectTetracyclines
dc.subjectTilapia
dc.subjectExtraction
dc.subjectFactorial Experimental Design
dc.subjectFish
dc.subjectHplc
dc.subjectResidue
dc.subjectTetracyclines
dc.titleExtraction Of Tetracyclinic Antibiotic Residues From Fish Filet: Comparison And Optimization Of Different Procedures Using Liquid Chromatography With Fluorescence Detection.
dc.typeArtículos de revistas


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