Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
권호 표지

Analysis of Flumeqnine in Meats

식육 중 항생제 flumequine의 분석

  • Kuk, Ju-Hee (Gwangju Regional Korea Food and Drug Administration) ;
  • Ko, Yong-Seok (Gwangju Regional Korea Food and Drug Administration) ;
  • Kim, Yong-Hoon (Seoul Regional Korea Food and Drug Administration) ;
  • Yoon, Chang-Yong (National Institute of Toxicological Research) ;
  • Sun, Nam-Kyu (Daejeon Regional Korea Food and Drug Administration) ;
  • Kim, Eun-Jung (Gwangju Regional Korea Food and Drug Administration) ;
  • Seo, Jee-Woo (Gwangju Regional Korea Food and Drug Administration) ;
  • Park, Ji-Won (Gwangju Regional Korea Food and Drug Administration) ;
  • Kang, Kil-Jin (Korea Food and Drug Administration)
  • 국주희 (광주지방식품의약품안전청) ;
  • 고용석 (광주지방식품의약품안전청) ;
  • 김용훈 (서울지방식품의약품안전청) ;
  • 윤창용 (국립독성과학원) ;
  • 선남규 (대전지방식품의약품안전청) ;
  • 김은정 (광주지방식품의약품안전청) ;
  • 서지우 (광주지방식품의약품안전청) ;
  • 박지원 (광주지방식품의약품안전청) ;
  • 강길진 (식품의약품안전청 영양기능식품국)
  • Published : 2009.02.28
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Abstract

An analytical method for the determination of flumequine in meats was developed and validated using high-performance liquid chromatography with fluorescence detection. The samples were mixed with sodium sulfate and extracted with ethyl acetate. After clean-up, the residues were dissolved in mobile phase. The calibration curves showed high linearity ($r^2$=0.9979) within the concentration range of 0.1-1.0 mg/kg. The limit of detection and limit of quantification were validated at 0.005 and 0.017 mg/kg, respectively. The recoveries in fortified meats ranged from 90.8 to 101.1%. The method was then validated in correspondence with the CODEX guidelines for flumequine residue in meats. Herein we monitored 150 samples of meats that were purchased in Korea (Seoul, Busan, Daegu, Daejeon, and Gwangju). Among the tested samples, flumequine was detected in 1 of beef and 1 of pork at levels in the range of 0.048-0.080 mg/kg. Overall, the flumequine residues in the tested samples were within the Maximun residue limit.

플루메퀸의 분석은 시료를 ethyl acetate로 추출 농축한 후 이 농축액에 acetonitrile과 n-hexane을 가하여 분리하고, 분리된 acetonitrile층을 농축하였다. 이를 이동상에 녹여 여과한 후 $C_{18}$ 컬럼을 이용한 HPLC-FLD로 분석하였다. 분석법은 표준물질 0.1-1.0mg/kg의 농도범위에서 직선성($r^2$=0.9979)을 나타냈으며, 검출한계는 0.005 mg/kg, 정량한계는 0.017 mg/kg이었다. 또한 회수율은 쇠고기에서 90.8-96.7%, 돼지고기에서 96.4-96.6%, 닭고기에서 94.0-101.1%이었으며, 상대표준편차(RSD)는 쇠고기, 돼지고기, 닭고기에서 각각 5.3-8.6%, 3.0-6.8%, 3.1-4.1%이었다. 확립된 분석방법으로 유통 중인 식육(쇠고기, 돼지고기, 닭고기) 150건을 전국 지역(서울, 부산, 대구, 대전, 광주)별로 수거하여 플루메퀸의 잔류 실태를 조사한 결과, 쇠고기 1건(0.080 mg/kg), 돼지고기 1건 (0.048 mg/kg)에서 검출되었으며, 조사한 식육 150건의 플루메퀸 잔류량은 모두 잔류허용기준 이하의 수준이었다.

Keywords

References

  1. KFDA. MRLs for veterinary drugs in foods. Korea Food & Drug Administration, Seoul, Korea. pp. 9-31 (2007)
  2. KFDA. Korea food code. Korea Food & Drug Administration, Seoul, Korea (2008)
  3. Pecorelli I, Galarini R, Bibi R, Floridi A, Casciarri E, Floridi A. Simultaneous determination of 13 quinolones from feeds using accelerated solvent extraction and liquid chromatography. Anal. Chim. Acta 483:81-89 (2003) https://doi.org/10.1016/S0003-2670(02)01401-0
  4. Ramos M, Aranda A, Garcia E, Reuvers T, Hooghuis H. Simple and sensitive determination of five quinolones in food by liquid chromatography with fluorescence detection. J. Chromatogr. B 789: 373-381 (2003) https://doi.org/10.1016/S1570-0232(03)00212-5
  5. Roudaut B, Yorke JC. High-performance liquid chromatographic method with fluorescence detection for the screening and quantification quantification of oxolinic acid, flumequine, and sarafloxacin in fish. J. Chromatogr. B 780: 481-485 (2002) https://doi.org/10.1016/S1570-0232(02)00641-4
  6. Hassouan MK, Ballesteros O, Taoufiki J, Vilchez JL, Cabrera-Aguilera M, Navalõn A. Multiresidue determination of quinolone antibacterials in eggs of laying hens by liquid chromatography with fluoresccence detection. J. Chromatogr. B 852: 625-630 (2007) https://doi.org/10.1016/j.jchromb.2006.12.039
  7. Clare H, Sin DWM, Tang HPO, Chung LPK, Siu SMP. Determination and on-line clean-up of (fluoro)quinolones in cattle milk using column-switching liquid chromatography fluorescence detection. J. Chromatogr. A 1061: 123-131 (2004) https://doi.org/10.1016/j.chroma.2004.11.003
  8. Pilorz K, Choma I. Isocratic reversed-phase high-performance liquid chromatographic separation of tetracyclines and flumequine controlled by a chaotropic effect. J. Chromatogr. A 1031: 303-305 (2004) https://doi.org/10.1016/j.chroma.2003.12.024
  9. Karbiwnyk CM, Carr LE, Turnipseed SB, Andersen WC, MillerKE. Determination of quinolone residues in shrimp using liquid chromatography with fluorescence detection and residue confirmation by mass spectrometry. Anal. Chim. Acta 596: 257-263 (2007) https://doi.org/10.1016/j.aca.2007.06.018
  10. Delmas JM, Chapel AM, Sanders P. Determination of flumequine and 7-hydroxyflumequine in plasma of sheep by high-performance liquid chromatography. J. Chromatogr. B 712: 263-268 (1998) https://doi.org/10.1016/S0378-4347(98)00159-5
  11. Touraki M, Ladoukakis M, Prokopiou C. High-performance liquid chromatographic determination of oxolinic acid and flumequine in the live fish feed Artemia. J. Chromatogr. B 751: 247-256 (2001) https://doi.org/10.1016/S0378-4347(00)00474-6
  12. Clemente M, Hermo MP, Barron D, Barbosa J. Confirmatory and quantitative analysis using experimental design for the extraction and liquid chromatography-UV, liquid chromatography-mass spectrometry and liquid chromatography-mass spectry/mass spectrometry determination of quinolones in turkey muscle. J. Chromatogr. A 1135: 170-178 (2006) https://doi.org/10.1016/j.chroma.2006.09.041
  13. Hoof NV, Wasch KD, Okerman L, Reybroeck W, Poelmans S, Noppe H, Brabander HD. Validation of a liquid chromatographytandem mass spectrometric method for the quantification of eight quinolones in cattle muscle, milk, and aquacultured products. Anal Chim. Acta. 529: 265-272 (2005) https://doi.org/10.1016/j.aca.2004.07.055
  14. Vyncht GV, Janosi A, Bordin G, Toussaint B, Maghuin-Rogister G, Pauw ED, Rodriguez AR. Multiresidue determination of (fluoro)quinolone antibiotics in swine kidney using liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 952: 121-129 (2002) https://doi.org/10.1016/S0021-9673(02)00092-4
  15. Johnston L, Mackay L, Croft M. Determination of quinolones and fluoroquinolones in fish tissue and seafood by high-performance liquid chromatography with electrospray ionisation tandem mass spectrometric detection. J. Chromatogr. A 982: 97-109 (2002) https://doi.org/10.1016/S0021-9673(02)01407-3
  16. Toussaint B, Bordin G, Rodriguez AR. Validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of 11 (fluoro)quinolone antibiotics in swine kidney. J. Chromatogr. A 976: 195-206 (2002) https://doi.org/10.1016/S0021-9673(02)00948-2
  17. CODEX guidelines for the establishment of a regulatory program for control of veterinary drug residues in foods (CAC/GL16). Available from:http://www.codexalimentarius.net/download/standards/47/CXG_016e.pdf. Accessed Jul. 20, 2008