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HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발

Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA

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BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient (r2) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02mg/kg, and average recoveries ranged from 72.9 to 88.1 %in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity,repeatability and reproducibility.

Abstract

BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient (r2) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02mg/kg, and average recoveries ranged from 72.9 to 88.1 %in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity,repeatability and reproducibility.

참고문헌 (11)

  1. Codex Alimentarius Commission, "Codex Guidelines for the Establishment of a Regulatory Programme for Control of Veterinary Drug Residues in Foods", Codex Committee on Residues of Veterinary Drugs in Foods; CAC, 1993
  2. Codex Alimentarius Commission, "Guidelines for the design and implementation of national regulatory food safety assurance programme associated with the use of veterinary drugs in food producing animals", CAC, 2009
  3. Ghoneim, M. M., "Electrochemistry of the antibacterial and antifungal drug nitroxoline and its determination in bulk form, pharmaceutical formulation and human blood", Bioelectroch, 80, pp.162~168 (2011)
  4. Kang, X., "Quantitative high-performance liquid chromatographic analysis of nitroxoline and structurally related compounds", Chromatographia, 57, pp.405~408 (2003)
  5. Karpińska, G., "On tautomerism and substituent effect in 8-hydroxyquinoline-derived medicine molecules", J. Mol. Struc. Theochem, 961, pp.101~106 (2010)
  6. Lee, Y. D., "Practical book of Korea Food Code pesticide residue analysis method", pp.79~ (2012), Korea Food & Drug Administration
  7. Pelletier, C., "Roles of divalent cations and pH in mechanism of action of nitroxoline against Escherichia coli strains", Antimicrob, Agents Chemother, 39, pp.707~713 (1995)
  8. Shin, H. C., "Development of management system and standardization for veterinary drug residue" (2012), Korea Food & Drug Administration
  9. Štefane, B., "A microwave-assisted nucelophilic substitution reaction on a quinoline system: the syntehsis of amino analogues of nitroxoline", Tetrahedron Lett, 53, pp.1964~1967 (2012)
  10. Szabó, G., "Examination of silica-salicylic acid and silica-8-hydroxyquinoline HPLC stationary phases for estimation of the adsorption coefficient of soil for some aromatic hydrocarbons", Chemosphere, 30, pp.1717~1727 (1995)
  11. Wang, H., "Spectrofluorimetic determination of cysteine based on the fluorescence inhibition of Cd(Ⅱ)-8-hydroxyquinoline-5-sulphonic acid complex by cysteine", Talanta, 53, pp.1015~1019 (2001)

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