Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry

LC-MS/MS를 이용한 수산물 중 콜리스틴 분석법 개발

  • Shin, Dasom (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) ;
  • Lee, Soo-Bin (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Cho, Yoon-Jae (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) ;
  • Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
  • 신다솜 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강희승 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이수빈 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 천소영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정지윤 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2016.07.11
  • Accepted : 2016.09.06
  • Published : 2016.10.28
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Abstract

Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

LC-MS/MS를 이용하여 폴리펩타이드계 동물용의약품인 콜리스틴에 대한 시험법을 확립하여 정량성 및 정밀성을 확보하였으며, 확립된 시험법의 적용성 검증을 위해 국제식품규격위원회 기준에 따라 특이성, 정확성, 직선성, 정밀성, 검출한계, 정량한계 등을 검증하였다. 콜리스틴 표준용액을 잔류허용기준의 농도에 따라 검량선을 작성한 결과 0.99 이상의 직선성을 확인 할 수 있었으며, 본 실험에서의 평균 회수율은 85.9~107%이었다. 또한, 분석오차는 11.8% 이하로 정확성 및 재현성이 우수하였으며, 검출한계는 0.02 mg/kg, 정량한계는 0.05 mg/kg이었다. 또한, 실험실간 교차검증을 통하여 신뢰성을 확보하였다. 확립된 분석법은 양식 수산물 중 잔류할 수 있는 동물용의약품인 콜리스틴에 대한 안전관리에 활용 할 수 있을 것으로 판단된다.

Keywords

References

  1. J. A. Orwa, A. V. Gerven, E. Roets, J. Hoogmartens: Validation of a Liquid Chromatography Method for Analysis of Colistin Sulphate. Chromatographia, 51, No. 7/8 (2000).
  2. V. Pintado, Lucia Garcia San Miguel, G. Fabio, M. Blanca, C. Javier, F. Jesu's, M. D. Pilar, M. Santiago: Intravenous colistin sulphomethate sodium for therapy of infections due to multidrug-resistant gram-negative bacteria. J. of Infection, 56, 185-190 (2008). https://doi.org/10.1016/j.jinf.2008.01.003
  3. C. Boudewijn, C. Marco, B. Keith, G. Kari, G. Kornelia, H. Anja, J. Helen, L. Ernesto, L. N. Antonio, et al.: Use of colistin-containing products within the European Union and European Economic Area (EU/EEA): development of resistance in animals and possible impact on human and animal health. Int. J. of Antimicrob. Agents, 46, 297-306 (2015). https://doi.org/10.1016/j.ijantimicag.2015.06.005
  4. Y. H. Choi, MD.: Treatment of drug resistant bacteria: new bugs, old drugs, and new therapeutic approaches. J. Korean Med. Assoc., 57(10), 837-844 (2014). https://doi.org/10.5124/jkma.2014.57.10.837
  5. M. Joseph B and L. Shawn: From Pigs to Patients: Transmissible, Single Gene-mediated Resistandce to Colistin. J. of Med. Microbiol. & Diagnosis, 5:1 (2016).
  6. Ministry of Health, Labour and Welfare (MHLW), Available from: http://www.mhlw.go.jp/english/. Accessed (2002).
  7. European Medicines Evaluation Agency (EMEA), Available from: http://www.ema.europa.eu/ema/. Accessed (2006).
  8. Ministry of Helth and Welfare: Korea National Health and Nutrition Examination Survey, Available from: http://knhanes.cdc.go.kr/. Accessed (2014).
  9. Codex guidelines for the establishment of a regulatory program for control of veterinary drug residues in foods. CAC/GL 16, 1-46 (1993).
  10. Codex Alimentarius Committee. Guidelines for the design and implementation of national regulatory food safty assurance programme associated with the use of veterinary drugs in food producing animals. CAC/GL 71 (2012).
  11. Korean Food Standards Codex: Ministry of Food and Drug Safety (2016).
  12. Jian Li, W. M. Robert, L. N. Roger, J. D. Turnidge and Kingsley Coulthard: Stability of Colistin and Colistin Methanesulfonate in Aqueous Media and Plasma as Determined by High-Performance Liquid Chromatography. Antimicrob. Agents and Chemother., 47, 1364-1370 (2003). https://doi.org/10.1128/AAC.47.4.1364-1370.2003
  13. C. H. W. Eric, C. Ho, W. M. S. Della, Y. C. Wong: Detection of residual bacitracin A, colistin A, and colistin B in milk and animal tissues by liquid chromatography tandem mass spectrometry. Anal. Bioanal. Chem., 385, 181-188 (2006). https://doi.org/10.1007/s00216-006-0325-5
  14. M. Zheng, J. Wang, P. G. Jacobus, W. M. Robert: Determination of colistin in human plasma, urine and other biological samples using LC-MS/MS. J. of chromatography B, 826, 205-212 (2008).
  15. Y. Xu, X. Tian, C. Ren, H. Huang, X. Zhang, X. Gong, H. Liu, Z. Yu, L. Zhang: Analysis of colistin A and B in fishery products by ultra performance liquid chromatography with positive electrospray ionization tandem mass spectrometry. J. of chromatography B, 899, 14-20 (2012). https://doi.org/10.1016/j.jchromb.2012.04.028
  16. M. Thomas, T. Frederic, G. Celine, C. Natascia, W. Stephane, G. Monia, C. Chantal, B. Thierry, C. William, M. Oscar, A. L. Decosterd: High-throughput hydrophilic interaction chromatography coupled totandem mass spectrometry for the optimized quantification of theanti-Gram-negatives antibiotic colistin A/B and its pro-drugcolistimethate. J. of chromatography A, 1369, 52-63 (2014). https://doi.org/10.1016/j.chroma.2014.09.063
  17. K. Matti, UPPSALA UNIVERSITET: Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Medicine. 889.
  18. EMA: Use of colistin products in animals within the European Union: development of resistance and possible impact on human and animal health. EUROPEAN MEDICINES AGENCY, 755938 (2012).