Korean Journal of Veterinary Service (한국동물위생학회지)

The Korean Society of Veterinary Service (한국동물위생학회)
권호 표지

Study on analytical method of fluoroquinolone residues in eggs by LC/MS/MS

LC/MS/MS를 이용한 식용란 중 fluoroquinolone계 항균물질의 분석법에 관한 연구

  • 최유정 (경상남도축산진흥연구소) ;
  • 윤이란 (경상남도축산진흥연구소) ;
  • 남상윤 (경상남도축산진흥연구소) ;
  • 박영호 (경상남도축산진흥연구소) ;
  • 김병훈 (경상남도축산진흥연구소) ;
  • 손성기 (경상남도축산진흥연구소)
  • Published : 2007.03.30
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Abstract

An atmospheric pressure chemical ionization (APcI) LC/MS/MS method was developed for the simultaneous analysis of fluoroquinolones (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin) residues in eggs. The spiked and blank samples were extracted from whole eggs using 50mM phosphate buffer (pH 7.4). The extract was cleaned up by passage though $Oasis^{(R)}$ MAX extraction cartridge for solid-phase extraction followed by elution with 4% formic acid in methanol. The extract of sample was separated on a Waters $Atlantis^{TM}$ $dC_{18}$ reversed-phase column ($4.6{\times}150mm,\;5{\mu}m$) and analyzed by APcI positive mode mass spectrometry. The mobile phase consists of aqueous 0.2% nonafluoropentanoic acid (NFPA) and methanol. Multiple reaction monitoring (MRM) using the precursor to product ion combinations of m/z $320\;{\dashrightarrow}\;302,\;332\;{\dashrightarrow}\;314,\;360\;{\dashrightarrow}\;342$ and m/z $358\;{\dashrightarrow}\;340$ were used to quantify norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR) and danofloxacin (DAN), respectively. The limits of quantification (LOQ) were 7.8ppb for NOR, 8.5ppb for CIP, 8.9ppb for ENR, and 4.8ppb for DAN. Average recoveries of fortified sample at levels of 0.025 to 0.1 ppm were estimated 71.29% for NOR, 75.27% for CIP, 85.51% for ENR and 81.22% for DAN. These results could be applied for the confirmation and quantification in eggs.

Keywords

References

  1. Gigosos PG, Revesado PR, Cadahia O, et al. 2000. Determination of quinol- ones in animal tissues and eggs by high-performance liquid chromatogra- phy with photodiode-array detection. J Chromatogr A 871(1-2) : 31-36 https://doi.org/10.1016/S0021-9673(99)00917-6
  2. Wright DH, Herman VK, Konstantini-des FN, et al. 1998. Determination of quinolone antibiotics in growth media by reversed-phase high-performance liquid chromatography. J Chromatogr B Biomed Sci Appl 709(1) : 97-104 https://doi.org/10.1016/S0378-4347(98)00006-1
  3. 서계원 이재일, 이채용 등. 2002. MSPD법과 HPLC를 이용한 계란내 플루오로퀴놀론계 항균물질의 동시 다성분 정량분석. 한국공중보건학회지 26(4) : 269-281
  4. Yorke JC, Froc P. 2000. Quantitation of nine quinolones in chicken tissues by high-performance liquid chromato-graphy with fluorescence detection. J Chromatogr A 882(1-2) : 63-77 https://doi.org/10.1016/S0021-9673(00)00212-0
  5. Herikstad H, Hayes P, Mokhtar M, et al. 1997. Emerging quinolone-resistant Salmonella in the United States. Emerg Infect Dis 3(3):371-372 https://doi.org/10.3201/eid0303.970316
  6. Smith KE, Besser JM, Hedberg CW, et al. 1999. Quinolone-resistant Cam-pylobacter jejuni infections in Minne-sota, 1992-1998. Investigation Team. N Engl J Med 340(20):1525-1532 https://doi.org/10.1056/NEJM199906243402510
  7. Barry C. 1993. The analytical testing followed by laboratory services divisi-on of agriculture Canada for veterinary drug residue in eggs, in procee‐dings of the euroresidues II conference on residues of veterinary drugs in food, Veldhoven, The Netherlands 3-5, 170-175
  8. Posyniak A, Zmudzki J, Semeniuk S, et al. 1999. Determination of fluoroquinolone residues in animal tissues by liquid chromatography. Biomed Chromatogr 13(4):279-285 https://doi.org/10.1002/(SICI)1099-0801(199906)13:4<279::AID-BMC844>3.0.CO;2-A
  9. Horie M, Saito K, Nose N, et al. 1994. Simultaneous determination of benofloxacin, danofloxacin, enrofloxacin and ofloxacin in chicken tissue by high-performance liquid chromatogra-phy. J Chromatogr B Biomed Appl 653(1):69-76 https://doi.org/10.1016/0378-4347(93)E0428-S
  10. Yorke JC, Froc P. 2000. Quantitation of nine quinolones in chicken tissues by high-performance liquid chromatography with fluorescence detection. J Chromatogr A 882(1-2) : 63-77 https://doi.org/10.1016/S0021-9673(00)00212-0
  11. 사단법인 한국동물약품협의회 : 동물용의약품등 편람. 2001
  12. Watanabe H, Satake A, Kido Y, et al. 2002. Monoclonal-based enzyme-linked immunosorbent assay and immunochromatographic assay for enrofloxacin in biological matrices. Analyst 127(1) : 98-103 https://doi.org/10.1039/b109427k
  13. Juhel GM, Abjeun JP. 1998. Screening of quinolones residues in pig muscle by planer chromatography. Chromatographia 47(12) : 101-104 https://doi.org/10.1007/BF02466795
  14. Hussain MS, Chukwumaeze-Obiajunwa V, Micetich RG. 1995. Sensitive high-performance liquid chromatographic assay for norfloxacin utilizing fluorescence detection. J Chromatogr B Biomed Appl 663(2):379-384 https://doi.org/10.1016/0378-4347(94)00465-H
  15. Kung K, Riond JL, Wanner M. 1993. Pharmacokinetics of enrofloxacin and its metabolite ciprofloxacin after intravenous and oral administration of enrofloxacin in dogs. J Vet Pharmacol Ther 16(4):462-468 https://doi.org/10.1111/j.1365-2885.1993.tb00212.x
  16. Schneider MJ, Donoghue DJ. 2000. Multiresidue determination of fluoroqu-inolones in eggs. J AOAC Int 83(6):1306-1312
  17. Johnston L, Mackay L, Croft M. 2002. Determination of quinolones and fluoroquinolones in fish tissue and seafood by high-performance liquid chromatography with electro‐spray ionization tandem mass spectro‐metric detection. J Chromatogr A 982(1):97-109 https://doi.org/10.1016/S0021-9673(02)01407-3
  18. Yamada R, Kozono M, Ohmori T, et al. 2006. Simultaneous determination of residual veterinary drugs in bovine, porcine, and chicken muscle using liquid chromatography coupled with electrospray ionization tandem mass spectrometry. Biosci Biotechnol Biochem 70(1) : 54-65 https://doi.org/10.1271/bbb.70.54
  19. 박수정, 조병훈, 임채미 등. 2005. HPLC를 이용한 닭고기 및 계란내 Fluoroquinolone계 항균물질의 동시 분석법. 한국공중보건학회지 29(1) : 45-55
  20. Schneider RP, Ericson JF, Lynch MJ, et al. 1993. Confirmation of danoflox- acin residues in chicken and cattle liver by microbore high-performance liquid chromatography electrospray ionization tandem mass spectrometry. Biol Mass Spectrom 22(10):595-599 https://doi.org/10.1002/bms.1200221007
  21. Barron D, Jimenez-Lozano E, Bailac S, et al. 2002. Determination of difloxacin and sarafloxacin in chicken muscle using solid-phase extraction and capillary electrophoresis. J Chromatogr B 767(2) : 313-319 https://doi.org/10.1016/S1570-0232(01)00587-6
  22. 강환구, 손성환, 이혜숙 등. 1997. 시료고체상분산(matrix solid phase disper-‐sion)전처리법과 액체크로마토그라피를 이용한 돈육중 enrofloxacin 및 cipro-‐floxacin 분석. 대한수의학회지 37(1):195-202
  23. Barker SA. 2000. Matrix solid-phase dispersion. J Chromatogr A 885(1-2):115-127 https://doi.org/10.1016/S0021-9673(00)00249-1
  24. 식품의약품안전청. 2005. 식품의 기준 및 규격
  25. 국립수의과학검역원. 2006. 축산물 중 유해물질 분석법 편람
  26. Lolo M, Pedreira S, Fente C, et al. 2005. Study of enrofloxacin depletion in the eggs of laying hens using diphasic dialysis extraction/purification and determinative HPLC-MS analysis. J Agric Food Chem 53(8):2849-2852 https://doi.org/10.1021/jf048015u