Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection

Cáceres, M. I. Rodríguez; Cabanillas, Agustina Guiberteau; Galeano-Dı́az, Teresa; Cañas, M.A. Martínez

doi:10.1016/j.jchromb.2009.12.012

Cited by 18 publications

(5 citation statements)

References 26 publications

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“…There are numerous studies and reviews about the determination of FQs in animal tissues , eggs , and bovine milk , but the number of studies about FQs in porcine plasma or serum is quite small. In general, FQs determination has been made by LC and CE .…”

Section: Introductionmentioning

confidence: 99%

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design

Vera‐Candioti

Teglia

Cámara³

2016

Electrophoresis

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A dispersive liquid-liquid microextraction procedure was developed to extract nine fluoroquinolones in porcine blood, six of which were quantified using a univariate calibration method. Extraction parameters including type and volume of extraction and dispersive solvent and pH, were optimized using a full factorial and a central composite designs. The optimum extraction parameters were a mixture of 250 μL dichloromethane (extract solvent) and 1250 μL ACN (dispersive solvent) in 500 μL of porcine blood reached to pH 6.80. After shaking and centrifugation, the upper phase was transferred in a glass tube and evaporated under N steam. The residue was resuspended into 50 μL of water-ACN (70:30, v/v) and determined by CE method with DAD, under optimum separation conditions. Consequently, a tenfold enrichment factor can potentially be reached with the pretreatment, taking into account the relationship between initial sample volume and final extract volume. Optimum separation conditions were as follows: BGE solution containing equal amounts of sodium borate (Na B O ) and di-sodium hydrogen phosphate (Na HPO ) with a final concentration of 23 mmol/L containing 0.2% of poly (diallyldimethylammonium chloride) and adjusted to pH 7.80. Separation was performed applying a negative potential of 25 kV, the cartridge was maintained at 25.0°C and the electropherograms were recorded at 275 nm during 4 min. The hydrodynamic injection was performed in the cathode by applying a pressure of 50 mbar for 10 s.

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Section: Introductionmentioning

confidence: 99%

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design

Vera‐Candioti

Teglia

Cámara³

2016

Electrophoresis

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“…In recent years, governmental agencies have set limitations on the acceptable levels of OFLX residues. Several traditional methods for the detection of OFLX residues, such as spectrophotometry, − high-performance liquid chromatography (HPLC), − capillary electrophoresis, − and microbiological assay, are well-proven and widely accepted, but these methods are often viewed as laborious and time intensive for sample pretreatment. Moreover, implementation of these methods involves a significant investment in equipment.…”

Section: Introductionmentioning

confidence: 99%

Crystal Structure of the Fab Fragment of an Anti-ofloxacin Antibody and Exploration of Its Specific Binding

Sheng

et al. 2016

J. Agric. Food Chem.

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The limited knowledge on the mechanism of interactions between small contaminants and the corresponding antibodies greatly inhibits the development of enzyme-linked immunosorbent assay methods. In this study, the crystal structure of a Fab fragment specific for ofloxacin was obtained. On the basis of the crystal characteristics, the modeling of the interactions between ofloxacin and the Fab revealed that TYR31 and HIS99 of the heavy chain and MET20 and GLN79 of the light chain formed a hydrophobic region and that SER52 and ALA97 of the heavy chain and TYR35 of the light chain formed a salt bridge and two hydrogen bonds for specific binding. The key roles of SER52 and ALA97 were further confirmed by site-directed mutation. A specificity analysis using 14 ofloxacin analogues indicates that the length of the bond formed between the piperazine ring and the antibody plays key roles in specific recognition. This work helps to clarify the mechanisms through which antibodies recognize small molecules and improve immune detection methods.

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“…Sarafloxacin (SARA) is a fluoroquinolone (FQ) antibacterial agent that is used for the control of early mortality in growing turkeys and broiler chickens (Codex of Federal Regulations, 1997). SARA is the first FQ approved in the United States for use in food‐producing animals, but was recently withdrawn from the market owing to concerns about microbial resistance (Chu et al ., 2002; Rodríguez Cáceres et al ., 2010). In the Republic of Korea, SARA is not currently registered, but its maximum residue limits (MRLs) were established as 10–80 µg/kg for poultry by the Korea Food and Drug Administration (KFDA).…”

Section: Introductionmentioning

confidence: 99%

“…The KFDA was tasked with developing a regulatory residue method for SARA in chicken and pig muscles. A variety of methods for the simultaneous determination of the FQs, including SARA, in pig or chicken muscles have been reported on the basis of liquid chromatography with fluorometric (Rose et al ., 1998; Holtzapple et al ., 1999; Posyniak et al ., 1999; Yorke and Froc, 2000; Ramos et al ., 2003; Schneider et al ., 2007), ultraviolet (Barrón et al ., 2002; Hermo et al ., 2005; Christodoulou et al ., 2007; Tsai et al ., 2009), electrochemical (Rodríguez Cáceres et al ., 2010) or mass spectrometric detection (Schneider and Donoghue, 2002; Bailac et al ., 2006; Clemente et al ., 2006; Kaufmann et al ., 2008). In these previous studies, non‐routine sample preparation techniques including immunoaffinity (Holtzapple et al ., 1999), microwave (Hermo et al ., 2005), dispersive extraction (Tsai et al ., 2009) and capillary electrophoresis chromatographic separation (Barrón et al ., 2002) have been applied, but their regular use is rather limited, owing to their non‐routine nature.…”

Section: Introductionmentioning

confidence: 99%

“…In these previous studies, non‐routine sample preparation techniques including immunoaffinity (Holtzapple et al ., 1999), microwave (Hermo et al ., 2005), dispersive extraction (Tsai et al ., 2009) and capillary electrophoresis chromatographic separation (Barrón et al ., 2002) have been applied, but their regular use is rather limited, owing to their non‐routine nature. Although diverse solid‐phase extraction (SPE) cartridges (strong cation exchange, Rose et al ., 1998), C 18 (Ramos et al ., 2003; Christodoulou, et al ., 2007) and styrene or polystyrene divinylbenzene copolymers (Posyniak et al ., 1999; Rodríguez Cáceres et al ., 2010) were used in the sample preparation, the SARA recovery values ranged from 51 to 69% (Rose et al ., 1998) or from approximately 70 to 90% (Posyniak et al ., 1999; Ramos et al ., 2003; Rodríguez Cáceres et al ., 2010), except in the study of Christodoulou et al . (2007) (96.7–102.8%).…”

Section: Introductionmentioning

confidence: 99%

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Bufferized solvent extraction and HPLC fluorometric detection method for sarafloxacin in pig and chicken muscles

Choi

Mamun

et al. 2011

Biomedical Chromatography

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In this study, a method for the detection of sarafloxacin in pig and chicken muscles was developed using HPLC-FLD as a regulatory residue technique. Good extraction efficiency was achieved using a mixture of 1% orthophosphoric acid-0.2 m MgCl(2) in water and acetonitrile as an extraction solvent, and n-hexane partitioning and centrifugation for cleanup was used in the absence of dehydration. Specificity, linearity, detection and quantification limits, recovery, accuracy and precision were all validated, and all results were sufficient for the SARA regulatory residue method in pig and chicken muscles. The method developed and described herein was not only simple but also reliable, and was applied to market samples to determine their residue contents.

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Simultaneous determination of quinolones for veterinary use by high-performance liquid chromatography with electrochemical detection

Cited by 18 publications

References 26 publications

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design

Crystal Structure of the Fab Fragment of an Anti-ofloxacin Antibody and Exploration of Its Specific Binding

Bufferized solvent extraction and HPLC fluorometric detection method for sarafloxacin in pig and chicken muscles

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