Liquid chromatographic separation of fluoroquinolone antibacterials used as veterinary drugs

SummaryThis paper describes the analysis of marbofloxacin at low levels in pig plasma by capillary electrophoresis (CE). To increase the sensitivity of CE we studied I',,vo on-column stacking systems, field-amplified sample injection (FASI) and isotachophoresis (ITP), and optimized several conditions to obtain the best sensitivity with each. The best results were obtained by use of ITP-CZE with 10 mM sodium monohydrogen phosphate (pH 9.0) as the leading and background electrolytes and 10 mM/?-alanine (pH 9.0) as the terminating electrolyte. This system was 75 times more sensitive than conventional CE -the enhanced detection limit (LOD) was 20 Ixg kg 1.. A sample of pig plasma was analyzed after clean-up by solid-phase extraction on Oasis HLB cartridges and elution with methanol. Recoveries were approximately 100%.

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“…The sensitivity obtained by use of this CE method is similar to that obtained by liquid chromatography [1,3,5,6].…”

Section: Analysis Of Plasma Samplesmentioning

confidence: 55%

“…This kind of sample is characterized by its complexity and so must be treated before CE analysis by deproteinization [2], liquid-liquid extraction (LLE) [1,5], and/ or solid-phase extraction (SPE) [4,6], etc.…”

Section: Introductionmentioning

confidence: 99%

Study of on-line stacking procedures for analyzing marbofloxacin by capillary zone electrophoresis

2002

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“…In a previous study [16], we reported the use of a mobile phase consisting of an AN-H20 mixture containing oxalic acid as a buffer for the separation of a series of 7-piperazinylquinolones, resulting in good peak symmetry. An analogous mobile phase was tested for the separation of FLU and OXO here.…”

Section: Chromatographic Proceduresmentioning

confidence: 99%

Analysis of flumequine and oxolinic acid in edible animal tissues by LC with fluorimetric detection

2000

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KeywordsColumn liquid chromatography Oxolinic acid Flumequine Residue analysis Edible animal tissue SummaryA simple rapid method has been developed for the determination of flumequine and oxolinic acid in edible animal tissues. Analytes are extracted from the sample matrix using dichloromethane in neutral conditions, then back-extracted in 0.01 M sodium hydroxide and determined by reversed-phase liquid chromatography with fluorimetric detection. The method has been applied to pork, salmon and chicken muscle with recoveries higher than 77% in all matrices. The detection limits achieved (< 1 lag kg -1) allow the determination of these drugs at a residue level far below their MRL. Moreover, some variables that may affect the spiking process have been studied.

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“…Most of them involve liquid chromatography with ultraviolet (LC-UV; Gigosos et al, 2000;Pecorelli et al, 2003;Bailac et al, 2004;Christodoulou and Samanidou, 2007), fluorescence (LC-FD;Eng et al, 1998;Hernández-Arteseros et al, 2000;Chu et al, 2002;EspinosaMansilla et al, 2005;Hassouan et al, 2007) or mass spectrometric detection (Van Vyncht et al, 2002;Toussaint et al, 2002Toussaint et al, , 2005aSchneider et al, 2005;Van Hoof et al, 2005;Hermo et al, 2006;Bailac et al, 2006;Rubies et al, 2007).…”

Section: Introductionmentioning

confidence: 98%

Simultaneous determination of quinolone antibacterials in bovine milk by liquid chromatography–mass spectrometry

Zafra-Gómez

Garballo

Ballesteros

et al. 2008

Biomedical Chromatography

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A new liquid chromatography-mass spectrometry (LC-MS) method has been developed and validated for the simultaneous determination of eight quinolone antibacterials for veterinary use in processed bovine milk samples. The quinolones studied included marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid and flumequine. Also, a new sample-treatment procedure was used for extraction and preconcentration of these compounds. It involved defatting by centrifugation, protein precipitation by adding a mixture of glacial acetic acid-acetonitrile and removing acetonitrile with dichloromethane; finally, the acidified aqueous layer was evaporated to dryness in a speed vac system, resuspended in the mobile phase and filtered prior to LC injection. The mobile phase was composed of a formic acid aqueous solution 0.1% (v/v) and acetonitrile, with an initial composition of water-acetonitrile 95: 5 (v/v) and using linear gradient elution. Norfloxacin was used as internal standard. The limits of quantification found (2-7 ng g(-1)) were in all cases lower than the maximum residue limits tolerated by the European Union for these compounds in milk.

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Liquid chromatographic separation of fluoroquinolone antibacterials used as veterinary drugs

Cited by 27 publications

References 21 publications

Study of on-line stacking procedures for analyzing marbofloxacin by capillary zone electrophoresis

Study of on-line stacking procedures for analyzing marbofloxacin by capillary zone electrophoresis

Analysis of flumequine and oxolinic acid in edible animal tissues by LC with fluorimetric detection

Simultaneous determination of quinolone antibacterials in bovine milk by liquid chromatography–mass spectrometry

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