Determination of Difloxacin and Sarafloxacin in Chicken Muscle Using Solid-Phase Extraction and Capillary Electrophoresis

Department Analytical Chemistry, University of Barcelona, Barcino, Catalonia, Spain
Journal of Chromatography B (Impact Factor: 2.73). 03/2002; 767(2):313-9. DOI: 10.1016/S1570-0232(01)00587-6
Source: PubMed


This paper describes a method for residue analysis of difloxacin and sarafloxacin in chicken muscle. Clean-up and preconcentration of the samples are effected by solid-phase extraction (C18) and the determination is carried out by capillary electrophoresis using a photodiode array detection system. The method was validated with satisfying results. The calibration graphs are linear for difloxacin and sarafloxacin from 50 to 300 microg/kg. The limit of detection obtained for difloxacin and sarafloxacin are 10 and 25 microg/kg, respectively, which allows the detection of positive muscle samples at the required maximum residue limits of European Union.

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    • "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. 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) "
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    ABSTRACT: 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.
    Biomedical Chromatography 03/2011; 25(3):405-11. DOI:10.1002/bmc.1463 · 1.72 Impact Factor
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    • "Also, Zhang et al. (2011) measured the inhibitory effects of sarafloxacin in comparison with enrofloxacin and marbofloxacin on the enzyme activity, protein levels and mRNA expression of liver cytochrome P450 (CYP) 1A and 3A in broilers and the results revealed that sarafloxacin didn't inhibit CYP in chick liver raising the possibility of drugs interaction when using those compounds. Sarafloxacin tissue residues in different tissues and eggs of birds were comprehensively examined by Maxwell et al. (1999), Chu et al. (2000), Posyniak et al. (2001), Barrón et al. (2002), Schneider and Donoghue (2002), Christodoulou et al. (2007), Durden and MacPherson (2007), Herranz et al. (2007), Zhao et al. (2007), Guo et al. (2009), Lin (2009), Rodríguez Cáceres et al. (2009), Zhao et al. (2009), Anadón et al. (2010), Cho et al. (2010), Pena et al. (2010) and Rodríguez Cáceres et al. (2010) and all of them proved that sarafloxacin has very low tissue and egg residual effect indicating its safety which will directly reflect on the health hazard of human. So, the objective of this study was to evaluate the efficacy of using sarafloxacin in the drinking water of broiler chickens for the treatment of experimental E. coli infection. "
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    ABSTRACT: This work was conducted to detect the effect of using sarafloxacin (5 mg/kg body weight) in the drinking water of broiler chickens to control experimental colisepticaemia in broiler chickens. One hundred and seventy, day old broiler chicks were used in the study. Twenty chicks at the day of arrival were sacrificed and cultured to ensure absence of E. coli infection. One hundred and fifty chicks were divided into three equal groups, each consists of 50 birds. Group (1) was challenged with E. coli and not treated with sarafloxacin (control positive), group (2) was challenged with E. coli and treated with sarafloxacin, while group (3) was neither challenged with E. coli nor sarafloxacin treated (blank control). Challenge was done intramuscularly (I/M) at 2 weeks of age in groups (1 and 2) as each bird received 0.5 ml of the nutrient broth culture containing 10 8 colony forming unit (CFU) E. coli O78 / ml. One appearance of signs, sarafloxacin was added to the drinking water for 3 successive days. All the birds were kept under complete observation for 6 weeks for estimating the bird's performance (body weight and feed conversion rate) and recording signs, mortalities, gross lesions, re-isolation of the organism and microscopical examination of the organs. The obtained results indicated significant (P<0.05) improvement in chickens performance in chickens challenged with E. coli and treated with sarafloxacin than those challenged and not treated. On the other hand, significant (P<0.05) decrease in morbidity and mortality rates, gross organs lesion score and re-isolation of E. coli O78 from the internal organs of chickens treated with sarafloxacin when compared with E. coli challenged non treated birds. Also, improvement of the microcscopical lesion scores was also detected in sarafloxacin treated group. It could be concluded from the above results that sarafloxacin used in a dose of 5 mg/kg body weight in the drinking water for 3 consecutive days is very effective in controlling of colisepticaemia in broiler chickens. 1. Introduction Escherichia coli (E. coli) is a normal inhabitant chicken's microflora. Some avian E. coli serotypes are pathogenic and induce significant economic problems in broiler chickens (Goodwin et al., 1993, Yogaratnam, 1995, Jakob et al., 1998, Dho-Moulin and Fairbrother, 1999 and Russell, 2003). Serogroups O78, O2 and O8 are common serotypes usually associated with colisepticaemia in poultry (Wray and Carroll, 1993). Colisepticaemia is the primary cause of death associated with an early respiratory disease complex (RDC) characterized by depression, respiratory distress and increased mortality in broiler chickens (Tablante et al., 1999 and Barnes et al., 2008). Typical lesions among birds with field and experimentally induced colisepticemia are airsacculitis, pericarditis and perihepatitis (Wray et al., 1996). The response of coliform infections to various medications is erratic and often difficult to evaluate. Significant increase in appearance of drug resistant strains of E. coli isolated from poultry has complicated the problem (Scioli et al., 1983, Alimehr et al., 1999 and Geornaras et al., 2001). Laboratory tests to determine the sensitivity of E. coli to the various drugs are useful to select the most beneficial drugs (Vandemaele et al., 2002).
    Life Science Journal 01/2011; 8(3):318-328. · 0.17 Impact Factor
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    ABSTRACT: A new chemiluminescence method for the determination of the fluoroquinolone sarafloxacin is described. The method is based on the measurement of the chemiluminescent (CL) radiation emitted in the reaction of sarafloxacin with Ce (IV) in sulfuric acid medium and in the presence of $ \mathrm{Ru}(\mathrm{bipy})_3^{2+ } $ as sensitizer. Since the method allows the recording of the whole CL intensity-versus-time profile, the use of measurement parameters such as the maximum CL emission is possible, which is proportional to the analyte concentration. The optimum chemical and experimental conditions for the CL emission of the reaction were researched. The calibration graph was lineal in the concentration range from 5.0 to 30.0 mg L−1 of sarafloxacin. The limit of detection, according to Clayton et al. (Anal Chem 59:2506–2514, 1987), was 1.17 mg L−1. After analyzing a series of ten solutions of 10.0 mg L−1 of sarafloxacin, the estimated average concentration was 10.30 mg L−1 with a standard deviation of 0.42 mg L−1 (confidence level, 95 %). The effect on the sarafloxacin CL signal of some common excipients (sucrose, lactose, and starch) used widely in pharmaceutical preparations was also tested, as well as that of others fluoroquinolones (namely, enrofloxacin and ciprofloxacin). Finally, the proposed method was applied to the determination of sarafloxacin in different spiked egg samples by using the standard addition methodology, obtaining excellent recoveries in all cases (close to 100 %).
    Food Analytical Methods 08/2012; 6(4). DOI:10.1007/s12161-012-9522-3 · 1.96 Impact Factor
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