Korean Journal of Environmental Agriculture (한국환경농학회지)

The Korean Society of Environmental Agriculture (한국환경농학회)
권호 표지
DOI QR코드

DOI QR Code

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

HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발

  • Cho, Yoon-Jae (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chae, Young-Sik (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Jae-Eun (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Jae-Young (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kang, Ilhyun (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Sang-Mok (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Do, Jung-Ah (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Oh, Jae-Ho (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chang, Moon-Ik (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Hong, Jin-Hwan (Residues of Pesticide and Veterinary Drugs in Foods Division, Department of Food safety Evaluation, National Institute of Food & Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 채영식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김재은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김재영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강일현 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이상목 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 오재호 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 홍진환 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2013.01.02
  • Accepted : 2013.03.25
  • Published : 2013.03.31
Download PDF
⟨ Previous Next ⟩

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 ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/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.

우리나라는 2007년부터 원료축산물에 대한 동물용의약품 잔류허용기준 설정을 강화하면서 관련 시험법을 식품공전에 등재하여 활용하고 있다. 더불어 국외에서는 국제식품규격위원회와 유럽연합의 규제 강화 추이에 따라 불검출기준 물질에 대한 MRL 설정 등 낮은 농도의 정량한계를 가지는 검증된 분석법 개발 등이 활발히 진행되고 있다. 따라서 본 연구는 가금류 중 잔류허용기준은 아직 설정되어 있지 않으나, 식품안전성 조사 및 연구 등을 위해서는 시험법의 확립이 필요한 nitroxoline의 닭고기 근육 중 잔류시험법을 개발하고자 하였다. 분석에 사용된 검체는 닭고기의 근육을 이용하였다. 검체에 아세트로니트릴을 가하여 추출한 후, 이를 감압 농축하여 메탄올로 녹인 다음 MCX 카트리지로 정제한 후 HPLC-PDA에 주입하였다. 기기분석은 C18 컬럼을 사용하였고, 0.1 % TBAOH-인산용액과 메탄올을 기울기 조건으로 하여 360 nm에서 측정하였다. 또한, 액체크로마토그래프-질량분석기를 통해 확인시험을 수행하였으며, 모든 검증은 CAC 가이드라인(CAC/GL 16, 1993; CAC/GL 71, 2009) 규정에 따라 실시하였다. 그 결과, nitroxoline의 LOQ는 0.02 mg/kg 수준이었고, 회수율은 72.9~88.1 %로 나타났다. 또한, 변동계수는 2.5~11.7 %로 CAC 가이드라인(CAC/GL 16, 1993; CAC/GL 71, 2009) 규정에 만족하는 수준이었다. 따라서 개발된 분석법은 잔류동물용의약품의 분석에 있어 보다 신속하고 경제적인 분석 및 모니터링에 적용 가능할 것으로 기대된다.

Keywords

References

  1. Codex Alimentarius Commission, 1993. 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/GL 16, CODEX, Italy.
  2. Codex Alimentarius Commission, 2009. 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/GL 71, Codex, Italy.
  3. Ghoneim, M.M., El-Desoky, H.S., 2011. Electrochemistry of the antibacterial and antifungal drug nitroxoline and its determination in bulk form, pharmaceutical formulation and human blood, Bioelectroch. 80, 162-168. https://doi.org/10.1016/j.bioelechem.2010.08.003
  4. Kang, X., Wang, Z., 2003. Quantitative high-performance liquid chromatographic analysis of nitroxoline and structurally related compounds, Chromatographia 57, 405-408 https://doi.org/10.1007/BF02492415
  5. Karpińska, G., Mazurek, A.P., Dobrowolski, J.C., 2010. On tautomerism and substituent effect in 8-hydroxyquinoline-derived medicine molecules, J. Mol. Struc. Theochem. 961, 101-106. https://doi.org/10.1016/j.theochem.2010.09.006
  6. Lee, Y.D., 2012. Practical book of Korea Food Code pesticide residue analysis method, pp. 79, Korea Food & Drug Administration, Korea.
  7. Pelletier, C., Prognon, P., Bourlioux, P., 1995. Roles of divalent cations and pH in mechanism of action of nitroxoline against Escherichia coli strains, Antimicrob, Agents Chemother. 39, 707-713. https://doi.org/10.1128/AAC.39.3.707
  8. Shin, H.C., Kim, T.S., 2012. Development of management system and standardization for veterinary drug residue, pp. 7-8, Korea Food & Drug Administration, Korea.
  9. Stefane, B., Pozgan, F., Sosic, I, Gobec, S., 2012. A microwave-assisted nucelophilic substitution reaction on a quinoline system: the syntehsis of amino analogues of nitroxoline, Tetrahedron Lett. 53, 1964-1967. https://doi.org/10.1016/j.tetlet.2012.02.017
  10. Szabo, G., Guczi, J., 1995. 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, 1717-1727. https://doi.org/10.1016/0045-6535(95)00057-F
  11. Wang, H., Wang, S.W., Zhang, H.S., 2001. Spectrofluorimetic determination of cysteine based on the fluorescence inhibition of Cd(II)-8-hydroxyquinoline-5-sulphonic acid complex by cysteine, Talanta. 53, 1015-1019. https://doi.org/10.1016/S0039-9140(00)00595-6