[보고서]축·수산물 내 유해물질의 기기분석법 비교·개선 및 위해평가를 위한 잔류실태조사 (2013년)

축·수산물 내 유해물질의 기기분석법 비교·개선 및 위해평가를 위한 잔류실태조사 (2013년)
Method improvement and monitoring on residues of veterinary drugs in foods (2013) 원문보기

보고서 정보
주관연구기관	식품위해평가부
보고서유형	최종보고서
발행국가	대한민국
언어	한국어
발행년월	2013-12
과제시작연도	2013
주관부처	식품의약품안전청 Korea Food & Drug Administration
등록번호	TRKO201400011696
과제고유번호	1475007303
사업명	농림수산검역검사기술개발
DB 구축일자	2014-07-26
키워드	시험법 개선.페니실린계열.아미노글리코사이드계열.모니터링.Aminoglycosides.Method development.Monitoring.Penicillins.Veterinary drugs.
DOI	https://doi.org/10.23000/TRKO201400011696

초록 ▼

연구결과
필요성 및 목표
○ 식품안전관리 일원화에 따라, 축산물위생관리법과 식품위생법에서 각각 관리되고 있던 부분을 통일하고자 「식품공전」과 「축수산물 유해물질 분석법 편람」에서 시험법이 서로 다른 동물용의약품을 비교·검토하고 개선하여 일선검사기관에서 표준시험법 사용의 혼란을 없애고자 함
○ 개선된 표준시험법으로 축산물의 동물용의약품 잔류실태조사를 실시하고 위해평가하여 축산물의 안전성 확보에 기여하고자 함
방법 및 결과
○ 축산물 관리체계 개선을 위한 분석법 비교 연구
- 시험법 개선
∙페니실린 계열 8종: 암피실린, 아목시실린, 클록사실린, 디클록사실린, 나프실린, 옥사실린, 페니실린G, 페니실린V
∙아미노글리코사이드 계열 10종: 스펙티노마이신, 겐타마이신, 카나마이신, 하이그로마이신B, 아프라마이신, 스트렙토마이신, 디하이드로스트렙토마이신, 아미카신, 네오마이신, 파로모마이신
- 시험법 검증: 국제식품규격위원회(CODEX) 기준에 따라 특이성, 직선성, 정량한계, 정확성, 정밀성, 회수율 확인
○ 축산물 중 잔류동물용의약품의 잔류실태 파악으로 안전관리를 위한 기초자료 확보
- 대상시료 : 소고기, 돼지고기, 닭고기, 우유
- 대상동물용의약품 : 페니실린 계열 8종 및 아미노글리코사이드 계열 10종
- 총 검체수 : 208건 (목표 건수 : 200건)
기대성과
○ 축산물 중 동물용의약품 관리체계 개선(안) 기초자료 마련
○ 축산물에 대한 잔류물질의 안전성 확보

Abstract ▼

Ministry of Food and Drug Safety (MFDS) has established analytical methods of veterinary drug residues in 'Food Code (FC)'. On the other hand, Animal, Plant and Fisheries Quarantine and Inspection Agency (QIA) that was in charge of method improvement on residues of veterinary drugs in livestock products has provided 'Manual of hazardous substances analysis in livestock and fishery products (MHSA)' for inspection agencies. After governmental reorganizationon on March 2013, food safety management in Korea is unified under MFDS.
Therefore, It was necessary to unify two kinds of analytical methods of residues in veterinary drugs.
In this study, the analytical methods were developed for 8 penicillin antibiotics (amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G, and penicillin V) and 10 aminoglycoside antibiotics (spectinomycin, paromomycin, gentamicin, streptomycin, amikacin, hygromycin B, dihydrostreptomycin, kanamycin, apramycin, and neomycin) that were found in livestock products and have major differences in analytical methods between FC and MHSA.
The results of the methods for penicillins in FC, recoveries were 78.9～112.1%, and limits of quantification (LOQ) were 0.01～0.05 mg/kg. In the case of the methods in MHSA, recoveries were 95.9～118.2%, and LOQ were 0.01～0.03 mg/kg. The results for aminoglycoside antibiotics, recoveries of method in FC were 69.0∼124.9%, and LOQs were 0.01-0.05 mg/kg. Recoveries and LOQs of analysis method in MHSA were 36.3∼75.5% and 0.01-0.06 mg/kg, respectively.
Therefore, the method of penicillin antibiotics was developed base on MHSA, and the method of aminoglycoside antibiotics was developed according to FC. The developed methods were validated by the parameters such as linearity, specificity, limit of quantification, precision, and accuracy based on CODEX validation guideline.
Survey of residual veterinary drugs was performed for 208 samples of livestock and fishery products. A penicillin antibiotic (cloxacillin) was found in a sample of beef with the concentration below the MRLs.

목차 Contents

표지 ... 1
자체연구개발과제 최종보고서 ... 2
국문 요약문 ... 3
Summary ... 4
목차 ... 5
연구개발과제 연구결과 ... 6
제1장 연구개발과제의 개요 ... 6
제1절 연구개발과제의 목표 ... 6
제2절 연구개발과제의 필요성 ... 7
제2장 연구개발과제의 국내·외 연구개발 현황 ... 9
제1절 국내ㆍ외 시험법 개발 현황 ... 9
제2절 국내ㆍ외 잔류실태조사 현황 ... 12
제3장 연구개발과제의 연구수행 내용 및 결과 ... 17
제1절 시험법 비교 ... 17
제2절 시험법 개선 및 검증 ... 49
제3절 잔류실태조사 ... 105
제4장 연구개발과제의 연구결과 고찰 및 결론 ... 107
제1절 시험법 비교 ... 107
제2절 시험법 검증 ... 107
제3절 잔류실태조사 ... 111
제5장 연구개발과제의 목표달성도 및 관련분야에의 기여도 ... 112
제6장 연구개발과제의 연구개발결과 활용계획 ... 113
제7장 참고문헌 ... 115
제8장 첨부서류 ... 117
끝페이지 ... 119

표/그림 (80)

표 Fig. 1. Molecular structures of penicillins
표 Fig. 1. Molecular structures of penicillins
표 Fig. 2. Procedure of the method of penicillins on 'Food Code'.
표 Fig. 3. LC-MS/MS chromatograms of penicillins (concentration of 0.5 MRL) on 'Food Code'
표 Fig. 4. Procedure of the method on ‘Manual of hazardous substances analysis in livestock and fishery products’.
표 Fig. 5. LC-MS/MS chromatograms of penicillins (concentration of 0.5 MRL) on ‘Manual of hazardous substances analysis in livestock and fishery products’.
표 Fig. 6. Molecular structures of aminoglycosides
표 Fig. 6. Molecular structures of aminoglycosides
표 Fig. 7. Procedure of the method for aminoglycoside on ‘Food code'.
표 Fig. 8. LC-MS/MS chromatograms of aminoglycoside (concentration of 0.5 MRL) on ‘Food code'.
표 Fig. 9. Procedure of the method on ‘Manual of hazardous substances analysis in livestock and fishery products’.
표 Fig. 10. LC-MS/MS chromatograms of aminoglycosides (concentration of 0.5 MRL) on ‘Manual of hazardous substances analysis in livestock and fishery products’.
표 Fig. 11. Chromatogram of penicillin G at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 12. Chromatogram of ampicillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 13. Chromatogram of penicillin V at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 14. Chromatogram of amoxicillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 15. Chromatogram of oxacillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 16. Chromatogram of nafcillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 17. Chromatogram of cloxacillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 18. Chromatogram of dicloxacillin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 19. Chromatogram of piperacillin (I.S) at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 20. Linearity of calibration curve for standard penicillins.
표 Fig. 21. Chromatogram of penicillin G at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 22. Chromatogram of ampicillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 23. Chromatogram of penicillin V at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 24. Chromatogram of amoxicillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 25. Chromatogram of oxacillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 26. Chromatogram of nafcillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 27. Chromatogram of cloxacillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 28. Chromatogram of dicloxacillin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 29. Chromatogram of piperacillin (I.S) at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 30. Linearity of calibration curve for standard penicillins
표 Fig. 31. Chromatogram of penicillin G at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 33. Chromatogram of penicillin V at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 32. Chromatogram of ampicillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 35. Chromatogram of oxacillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 34. Chromatogram of amoxicillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 34. Chromatogram of nafcillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 37. Chromatogram of cloxacillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 39. Chromatogram of piperacillin(IS) at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 38. Chromatogram of dicloxacillin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 40. Linearity of calibration curve for standard penicillins.
표 Fig. 41. Chromatogram of spectinomycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 42. Chromatogram of tobramycin (I.S) at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 43. Chromatogram of gentamicin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 44. Chromatogram of kanamycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 46. Chromatogram of apramycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 45. Chromatogram of hygromycin B at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 47. Chromatogram of streptomycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 48. Chromatogram of dihydrostreptomycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 49. Chromatogram of amikacin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 50. Chromatogram of neomycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 51. Chromatogram of paromomycin at blank (A), standard solution (B) and spiked sample of beef (C).
표 Fig. 52. Linearity of calibration curve for standard aminoglycosides
표 Fig. 53. Chromatogram of spectinomycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 54. Chromatogram of tobramycin (I.S) at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 55. Chromatogram of gentamicin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 56. Chromatogram of kanamycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 57. Chromatogram of hygromycin B at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 58. Chromatogram of apramycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 59. Chromatogram of streptomycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 60. Chromatogram of dihydrostreptomycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 61. Chromatogram of amikacin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 62. Chromatogram of neomycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 63. Chromatogram of paromomycin at blank (A), standard solution (B) and spiked sample of pork (C).
표 Fig. 64. Linearity of calibration curve for standard aminoglycosides
표 Fig. 64. Linearity of calibration curve for standard aminoglycosides
표 Fig. 65. Chromatogram of spectinomycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 66. Chromatogram of tobramycin (I.S) at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 67. Chromatogram of gentamicin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 68. Chromatogram of kanamycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 69. Chromatogram of hygromycin B at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 71. Chromatogram of streptomycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 70. Chromatogram of apramycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 72. Chromatogram of dihydrostreptomycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 73. Chromatogram of amikacin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 75. Chromatogram of paromomycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 74. Chromatogram of neomycin at blank (A), standard solution (B) and spiked sample of chicken (C).
표 Fig. 76. Linearity of calibration curve for standard aminoglycosides.
표 Fig. 76. Linearity of calibration curve for standard aminoglycosides.

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연합인증

축·수산물 내 유해물질의 기기분석법 비교·개선 및 위해평가를 위한 잔류실태조사 (2013년)
Method improvement and monitoring on residues of veterinary drugs in foods (2013) 원문보기