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Easy sample treatment for the determination of enrofloxacin and ciprofloxacin residues in raw bovine milk by capillary electrophoresis
Author(s) -
Piñero MaríaYsabel,
GarridoDelgado Rocío,
Bauza Roberto,
Arce Lourdes,
Valcárcel Miguel
Publication year - 2012
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.201200316
Subject(s) - enrofloxacin , chromatography , chemistry , residue (chemistry) , capillary electrophoresis , phosphoric acid , raw milk , protein precipitation , extraction (chemistry) , centrifugation , cartridge , sample preparation , electrophoresis , ciprofloxacin , materials science , biochemistry , food science , organic chemistry , metallurgy , antibiotics
An easy, selective, and sensitive method has been developed for the determination of enrofloxacin ( ENR ) and its main active metabolite, ciprofloxacin ( CIP ), in raw bovine milk using CE with UV detection at 268 nm. Milk samples were prepared by a clean‐up/extraction procedure based on protein precipitation with hydrochloride acid followed by being defatted by centrifugation and SPE using a hydrophilic‐lipophilic balance cartridge. Optimum separation was obtained using a 50 mM phosphoric acid at pH 8.4 and the total electrophoretic run time was 6 min. Sample preparation by this method yielded clean extracts with quantitative and consistent mean recoveries from 89 to 97% for CIP and from 93 to 98% for ENR . LOD s obtained were lower to the maximum residue limits for these fluoroquinolones. The precision of the ensuing method is acceptable; thus, the RSD for peak area and migration time was less than 8.5 and 0.5% for CIP and 9.9 and 0.9% for ENR , respectively. The results showed that the proposed method was efficient showing good recoveries, sensitivity, and precision for the studied compounds and could be satisfactorily applied in routine analysis for the monitoring of ENR and CIP residues in milk, due to its ruggedness and feasibility demonstrated.