한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)

  • 제33권3호
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  • Pages.176-184
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  • 2018
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  • 1229-1153(pISSN)
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  • 2465-9223(eISSN)
한국식품위생안전성학회 (The Korean Society of Food Hygiene and Safety)
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축수산물에서 LC-MS/MS를 이용한 카라졸롤 및 아자페론 분석

Determination of Carazolol and Azaperone in Livestock and Fishery Products Using Liquid Chromatography-tandem Mass Spectrometry

  • 최수연 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강희승 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김주혜 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 천소영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정지윤 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 조병훈 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이강봉 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Choi, Soo Yeon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kang, Hui-Seung (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kim, Joohye (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Cheon, So-Young (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Jeong, Jiyoon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Cho, Byung-Hoon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Lee, Kang-Bong (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
  • 투고 : 2018.03.22
  • 심사 : 2018.05.17
  • 발행 : 2018.06.30
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초록

축수산물의 집약적인 양식과 수송으로 인한 스트레스로 품질이 떨어진 물퇘지고기(PSE)가 생성되면서 이를 방지하기 위하여 베타-수용체 차단제인 카라졸롤과 진정제인 아자페론이 사용되어왔다. 무분별한 사용으로 주사부위나 근육에 잔류한 카라졸롤과 아자페론이 소비자에게 현기증과 같은 부작용을 일으키는 것으로 밝혀지면서 JECFA(FAO/WHO)에서 근육 및 신장부위에 대한 잔류허용기준을 설정하였으며 우리나라를 비롯한 여러 나라에서 잔류허용기준에 따라 안전 관리를 수행하고 있다. 본 연구는 축수산물에서 기존의 규제 대상인 돼지와 소를 비롯한 닭고기, 계란, 우유, 넙치, 장어, 새우 등 다양한 검체에서 분석법을 개발하고 시험법 검증과정을 통하여 축수산물에 동시에 적용 가능한 시험법을 확립하였다. 시험법을 간편화 하기 위하여 시료의 무게를 줄이고 전처리 과정을 단순화하였으며 LC-MS/MS를 이용하여 최적조건으로 검증하였다. 실제 분석법을 활용하기 위하여 CODEX 기준에 따라 특이성, 정확성, 직선성, 정밀성, 검출한계, 정량한계 등을 검증하였다. 카라졸롤, 아자페론과 아자페론의 대사체인 아자페롤의 표준용액을 잔류허용기준의 농도에 따라 검량선을 작성한 결과, 0.99 이상의 직선성을 확인 할 수 있었다. 또한 평균 회수율은 67.9-105%, 변동계수는 0.55-7.93%로 CODEX 가이드라인에 만족함으로써 정확성 및 재현성이 우수함을 확인 할 수 있었다. 본 연구에서 확립된 분석법은 소와 돼지 뿐만 아니라 닭고기, 계란, 우유, 넙치, 장어, 새우에도 적용 가능한 시험법을 확립하였으며 이는 향후 축수산물에서 카라졸롤, 아자페론에 대한 안전 관리를 위한 기초자료로 활용 될 수 있을 것으로 판단된다.

The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

키워드

참고문헌

  1. Chae H.S., Yoo Y.M., Jeong S.G., Ham J.S., Ahn C.N., Jang A.R., Yoo H.S.: Effect of holding time of broiler at slaughter house on color, PSE, appearance of chicken meat. Korean J. Poult. Sci., 35, 177-182 (2008). https://doi.org/10.5536/KJPS.2008.35.2.177
  2. Delahaut P., Levaux C., Eloy P., Dubois M.: Validation of a method for detecting and quantifying tranquillisers and a ${\beta}$-blocker in pig tissues by liquid chromatography-tandem mass spectrometry. Anal .Chim. Acta, 483, 335-340 (2003). https://doi.org/10.1016/S0003-2670(02)01024-3
  3. Delahaut P., Brasseur P.Y., Dubois M.: Multiresidue method for the detection of tranquillisers, xylazine, and a ${\beta}$-blocker in animal production by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A, 1054, 373-378 (2004). https://doi.org/10.1016/S0021-9673(04)01414-1
  4. Kay J.F., MacNeil J.D., Wang J.: Chemical analysis of non-antimicrobial veterinary drug residues in food. John Wiley & Sons, 1rd Ed. Wiley, Canada (2016).
  5. Mitrowska K., Posyniak A., Zmudzki J.: Rapid method for the determination of tranquilizers and a beta-blocker in porcine and bovine kidney by liquid chromatography with tandem mass spectrometry. Anal. Chim. Acta, 637, 185-192 (2009). https://doi.org/10.1016/j.aca.2008.10.030
  6. Korea animal health product association: statutes. 2001. Available online at: http://www.kahpa.or.kr/.
  7. Korea animal health product association: statistics.. 2018. Available online at: http://www.kahpa.or.kr/.
  8. Meenagh S.A., McEvoy J.D.G., Elliott C.H.: Determination of carazolol residues in porcine tissue by radioreceptor assay. Chim. Acta, 462, 149-156 (2002). https://doi.org/10.1016/S0003-2670(02)00338-0
  9. Van Ginkel L.A., Schwillens P.L.W.J., Olling M.: Liquid chromatographic method with on-line UV spectrum identification and off-line thin-layer chromatographic confirmation for the detection of tranquillizers and carazolol in pig kidneys. Anal. Chim. Acta, 225, 137-146 (1989). https://doi.org/10.1016/S0003-2670(00)84602-4
  10. Haagsma N., Bathelt E.R., Engelsma J.W.: Thin-layer chromatographic screening method for the tranquillizers azaperone, propiopromazine and carazolol in pig tissues. J. Chromatogr. A., 436, 73-79 (1988). https://doi.org/10.1016/S0021-9673(00)94567-9
  11. Quintana M.C., Blanco M.H., Lacal J., Hern-ndez L.: Analysis of pharmaceutical residues in bovine liver by HPLC. J. Liq Chromatogr. R. T., 24, 735-745 (2001). https://doi.org/10.1081/JLC-100103407
  12. Holland D.C., Munns R.K., Roybal J.E., Hurlbut J.A., Long A.R.: Simultaneous determination of xylazine and its major metabolite, 2, 6-dimethylaniline, in bovine and swine kidney by liquid chromatography. J. AOAC Int., 76, 720-724 (1993).
  13. Cerkvenik-Flajs V.: Determination of residues of azaperone in the kidneys by liquid chromatography with fluorescence detection. Anal. Chim. Acta, 586, 374-382 (2007). https://doi.org/10.1016/j.aca.2006.11.010
  14. Tetsuo M., Zhang C., Matsumoto H., Matsumoto L.: Gas chromatographic-mass spectrometric analysis of urinary sugar and sugar alcohols during pregnancy. J. Chromatogr. B Biomed. Sci. Appl., 731, 111-120 (1999). https://doi.org/10.1016/S0378-4347(99)00209-1
  15. Govaert Y., Batjoens P., Tsilikas K., Degroodt J.M., Srebrnik S.: Multi-residue analysis of tranquillizers in meat: confirmatory assays using mass spectrometry. Analyst., 123, 2507-2512 (1998). https://doi.org/10.1039/a805223i
  16. Zhang J., Shao B., Yin B., Yin J., Wu Y., Duan H.: Simultaneous detection of residues of ${\beta}$-adrenergic receptor blockers and sedatives in animal tissues by high-performance liquid chromatography-tandem mass spectrometry. J. Chromatogr. B, 877, 1915-1922 (2009). https://doi.org/10.1016/j.jchromb.2009.05.025
  17. Zhang L., Wu P., Jin Q., Ye H., Huang X., Liu S.: Simultaneous determination of eight tranquilizers in pork by ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry. Food Anal. Methods, 10, 354-362 (2017). https://doi.org/10.1007/s12161-016-0591-6
  18. Li J., Zhang J., Liu H., Wu L.: A comparative study of primary secondary amino (PSA) and multi-walled carbon nanotubes (MWCNTs) as QuEChERS absorbents for the rapid determination of diazepam and its major metabolites in fish samples by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry. J. Sci. Food Agric., 96, 555-560 (2016). https://doi.org/10.1002/jsfa.7123
  19. CCRVDF Codex Committee on Residues of Veterinary Drugs in Foods, 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 71-2009) Rome: Codex Alimentarius Commission. pp. 1-30 (2012).
  20. Haagsma N., Bathelt E.R., Engelsma J.W.: Thin-layer chromatographic screening method for the tranquillizers azaperone, propiopromazine and carazolol in pig tissues. J. Chromatogr. A. 436, 73-79 (1988). https://doi.org/10.1016/S0021-9673(00)94567-9
  21. Quintana M.C., Blanco M.H., Lacal J., Hern-ndez L.: Analysis of pharmaceutical residues in bovine liver by HPLC. J. Liq. Chromatogr. Relat. Technol., 24, 735-745 (2001). https://doi.org/10.1081/JLC-100103407
  22. Holland D.C., Munns R.K., Roybal J.E., Hurlbut J.A., Long A.R.: Simultaneous determination of xylazine and its major metabolite, 2, 6-dimethylaniline, in bovine and swine kidney by liquid chromatography. J. AOAC Int., 76, 720-724 (1993).
  23. Sell B., Posyniak A., Gbylik M.: Screening procedure for simultaneous determination of azaperone, carazolol, and chlorpromazine in animal urine. Bull Vet. Inst. Pulawy., 55, 513-517 (2011).
  24. Dinesh R., Prakash C., Poojary N., Kantharajan G., Abraham S.: Tobacco (Nicotiana tabacum)-A novel and futuristic sedative for fish transport in India. Int. J. Fish. Aquat. Stud., 5, 369-371 (2017).
  25. Trushenski J.T., Bowker J.D., Cooke S.J., Erdahl D., Bell T., MacMillan J.R., Yanong R.P., Hill J.E., Fabrizio M.C., Garvey J.E., Sharon S.: Issues regarding the use of sedatives in fisheries and the need for immediate-release options. Trans. Am. Fish Soc., 142, 156-170 (2013). https://doi.org/10.1080/00028487.2012.732651