Determination of quinolones in animal tissues and eggs by high-performance liquid chromatography with photodiode-array detection

Gigosos, P. González; Revesado, P.R; Cadahı́a, O; Fente, C.; Vázquez, Beatriz; Franco, Carlos; Cepeda, Alberto

doi:10.1016/s0021-9673(99)01048-1

Cited by 104 publications

(67 citation statements)

References 20 publications

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“…They act via inhibition of DNA-gyrase, abolishing its activity by interfering with the DNA rejoining reaction. (Gigosos et al, 2000).…”

Section: Introductionmentioning

confidence: 99%

The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

Park¹,

Kim²,

Han³

et al. 2013

Korean Journal for Food Science of Animal Resources

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This study aimed to apply the Parallux system to detect (fluoro)quinone antibiotics residues in raw bovine milk. The immunogen enabled the generation of a specific antiserum with a titer of 1/40,000. The Parallux TM kit using the antibody displayed IC 50 value of 10 to 150 ppb for (fluoro)quinolone antibiotics. Parallux TM kit was also sensitive for the detection of incurred (fluoro)quinolone at Korean Maximum Residual Levels in raw bovine milk as the result of dose response test. Cross reactivities of the antibody with the common (fluoro)quinolones were determined to be norfloxacin, 100%; enrofloxacin, 100%; ciprofloxacin, 100%; danofloxacin, 100%; nalidixic acid, 40%. Lower detection limit (LOD) values of the Parallux TM kit in raw bovine milk were determined to be norfloxacin, 4 ppb; enrofloxacin, 5 ppb; danofloxacin, 5 ppb; ciprofloxacin, 5 ppb and nalidixic acid, 10 ppb. The Parallux TM kit was run 8 times with five different concentrations of norfloxacin to determine the coefficient of variation (CV, %) of intra-assay, which was between 2.7% and 11.8%. To confirm the precision among kit batches for the inter-assay, five different batch kits were tested with 2 different concentration of norfloxacin. The CVs of the inter assay were 4.2% at 50 ppb, and 7.2% at 10 ppb norfloxacin, respectively.

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“…They act via inhibition of DNA-gyrase, abolishing its activity by interfering with the DNA rejoining reaction. (Gigosos et al, 2000).…”

Section: Introductionmentioning

confidence: 99%

The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

Park¹,

Kim²,

Han³

et al. 2013

Korean Journal for Food Science of Animal Resources

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“…In letteratura sono descritti diversi metodi per la ricerca di residui di chinoloni nel latte; le tecniche microbiologiche non hanno sensibilità adeguata a soddisfare i requisiti richiesti dalla normativa vigente; le tecniche immunochimiche (Haasnoot et al, 2007;Wang et al, 2010), la cromatografia su strato sottile (TLC) (Chroma et al, 1999;Juhel-Gaugain e Abejan, 1998), la gas cromatografia (GC) e la cromatografia liquida ad alte prestazioni (HPLC) accoppiata con rivelatore spettrofluorimetrico (FLD), a sequenza di diodi (DAD) o a spettrometria di massa (MS) (Gigosos et al, 2000;Yorke e Froc, 2000;Ramos et al, 2003;Ho et al, 2004;Marazuela e Moreno-Bondi, 2004;Van Hoof et al, 2005;Zhao et al, 2007;Bohm et al, 2009;Zhang et al, 2009) sono invece maggiormente sensibili e in taluni casi idonee a una inequivocabile identificazione degli analiti. Tuttavia questi metodi di solito comprendono solo una delle sottoclassi di chinoloni (derivati dell'acido piridoncarbossilico o fluorochinoloni con sostituente piperazinile al C-7).…”

Section: Introduzioneunclassified

Multiresidue confirmatory method for determination of quinolones in milk by HPLC: method development and validation according to the criteria of Commission Decision 2002/657/EC

et al. 2013

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Veterinary drugs have become an integral part of the livestock production and play an important role in maintaining animal welfare. The use of veterinary medicines may be cause of the presence of drug residues in animal food products if appropriate withdrawal periods are not respected or if contaminated feeds are used. This work presents the development of an high performance liquid chromatography with postcolumn fluorescence derivatization (HPLC-FLD) method for the quantitative detection of eight quinolones -norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, oxolinic acid, nalidixic acid, and flumequine -in bovine milk. After deproteination and extraction with a metaphosphoric acid 1% w/v/methanol/acetonitrile (60/20/20 v/v/v) solution, the sample is partially evaporated and cleaned up on a reversed phase solid phase extraction (SPE) cartridge. The extract is analyzed using an HPLC-FLD. Mean recovery ranged between 65-88%. The method is validated as a confirmatory method according to Decision 2002/657/EC. All the verified parameters (linearity, selectivity/specificity, trueness, precision, CC , CC , ruggedness and stability) were satisfactory and the method is able to quantify all the analytes in milk in the concentration range 15-60 µg/Kg for danofloxacin and 25-150 µg/Kg for the other quinolones. IntroduzioneI chinoloni sono chemioterapici antibatterici di sintesi caratterizzati da ampio spettro d'azione, in quanto esplicano la loro attività nei confronti di batteri Gram positivi e Gram negativi (Christian, 1996;Dougherty et al., 2001); sono composti caratterizzati da una struttura chimica comune consistente in un eterociclo aromatico con anelli condensati, un gruppo chetonico in posizione 4, una funzione carbossilica in posizione 3 e un sostituente in posizione 1 costituito da etile, ciclo propile o anello condensato (Figura 1). I chinoloni sono autorizzati in medicina veterinaria per il trattamento delle infezioni urinarie, della diarrea da salmonella e shigella, delle infezioni respiratorie da Haemophilus, streptococcus e pseudomonas. Sono somministrati come forma farmaceutica o in mangimi medicati e acqua di abbeverata.Un utilizzo massivo, improprio o abusivo di antibiotici in zootecnica è causa sia di sviluppo di ceppi batterici resistenti e trasmissibili all'uomo attraverso gli alimenti, sia di presenza residuale di farmaci negli alimenti di origine animale. Il regolamento 470 della Commissione Europea (2009) definisce come residui di farmaci tutte le sostanze farmacologicamente attive, espresse in mg/Kg o µg/Kg, e i loro metaboliti che rimangono negli alimenti ottenuti da animali. L'impiego di farmaci negli animali da reddito deve avvenire in modo da garantire che, al momento del consumo, l'alimento non contenga residui in quantità nociva per il consumatore. L'impatto sulla sicurezza alimentare è pertanto tale da aver indotto l'Unione Europea (UE) a stabilire precise regole in merito all'autorizzazione all'utilizzo dei farmaci negli animali in produzione e al controllo uffici...

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“…I campioni ufficiali, prelevati dall'autorità competente, sono analizzati in laboratori autorizzati attraverso metodi di screening e, in caso di positività, analizzati nuovamente con metodi di conferma. In letteratura sono descritti diversi metodi per la ricerca di residui di chinoloni nel latte; le tecniche microbiologiche non hanno sensibilità adeguata a soddisfare i requisiti richiesti dalla normativa vigente; le tecniche immunochimiche (Haasnoot et al, 2007;Wang et al, 2010), la cromatografia su strato sottile (TLC) (Chroma et al, 1999;Juhel-Gaugain et al, 1998), la gas cromatografia (GC) e la cromatografia liquida ad alte prestazioni (HPLC) accoppiata con rivelatore spettrofluorimetrico (FLD), a sequenza di diodi (DAD) o a spettrometria di massa (MS) (Yorke et al, 2000;Ramos et al, 2003;Zhao et al, 2007;Ho et al, 2004;Gigosos et al, 2000;Zhang et al, 2009;Bohm et al, 2009) sono invece maggiormente sensibili e in alcuni casi ido-nee ad un'inequivocabile identificazione degli analiti. Tuttavia questi metodi di solito comprendono solo una delle sottoclassi di chinoloni (derivati dell'acido piridoncarbossilico o fluorochinoloni con sostituente piperazinile al C-7).…”

Section: Introduzioneunclassified

Quantitative determination of quinolones residues in milk by HPLC-FLD

et al. 2012

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Veterinary drugs have become an integral part of the livestock production and play an important role in maintenance of animal welfare. The use of veterinary medicines may be cause of the presence of drug residues in animal food products if appropriate withdrawal periods are not respected or if contaminated feeds are used. This work presents the development of an HPLC-FLD method for the quantitative detection of eight quinolones -norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine-in bovine milk. After deproteination and extraction with a metaphosphoric acid 1% w/v / methanol / acetonitrile (60/20/20 v/v/v) solution, the sample is partially evaporated and cleaned up on a reversed phase SPE cartridge.The extract is analyzed using an high performance liquid chromatograph with fluorescence detector. Mean recovery ranged between 65% -88%. All the analytes can be identified and quantified in the concentration range 15 -60 µg/Kg for danofloxacin and 25 -150 µg/Kg for the other quinolones.

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Determination of quinolones in animal tissues and eggs by high-performance liquid chromatography with photodiode-array detection

Cited by 104 publications

References 20 publications

The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

Multiresidue confirmatory method for determination of quinolones in milk by HPLC: method development and validation according to the criteria of Commission Decision 2002/657/EC

Quantitative determination of quinolones residues in milk by HPLC-FLD

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Determination of quinolones in animal tissues and eggs by high-performance liquid chromatography with photodiode-array detection

Cited by 104 publications

References 20 publications

The Application of ParalluxTMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

The Application of ParalluxTMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

Multiresidue confirmatory method for determination of quinolones in milk by HPLC: method development and validation according to the criteria of Commission Decision 2002/657/EC

Quantitative determination of quinolones residues in milk by HPLC-FLD

Contact Info

Product

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The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk

The Application of Parallux^TMSystem for Multi-Detection of (Fluoro)quinolone Class Antibiotics Residues in Raw Bovine Milk