환경중잔류의약물질대사체분석방법확립에 관한연구 (Ⅱ) - 테트라사이클린계항생제 - 환경건강연구부화학물질연구과,,,,,, Ⅱ 2010

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11-1480523-000702-01 환경중잔류의약물질대사체분석방법확립에 관한연구

1 환경중잔류의약물질대사체분석방법확립에 관한연구 (Ⅱ) - 테트라사이클린계항생제 - 환경건강연구부화학물질연구과,,,,,, Ⅱ 2010

2 목차 ⅰ ⅱ ⅲ Abstract ⅳ Ⅰ Ⅱ i

3 목차 Ⅲ Ⅳ i

4 목차 ii

5 목차 iii

6 Abstract α β α β iv

7 Ⅰ. 서론 Ⅰ 1

8 Ⅱ. 연구내용및방법 Ⅱ. 2

9 Ⅱ. 연구내용및방법 <Table 1> Consumption of veterinary antibiotics in Republic of Korea(2009) Antibiotics Consumption(kg) Antibiotics Consumption(kg) Source : Safe Food 2010, Vol. 5, No. 1,

10 Ⅱ. 연구내용및방법 <Fig. 1> Chemical structure of tetracyclines. 4

11 Ⅱ. 연구내용및방법 <Table 2> Metabolites of tetracycline, chlortetracycline and oxytetracycline Tetracyclines Metabolites CAS No. M.W. αα ββ Source : Arch. Environ. Contam. Toxicol. 2002, 42, Source : Arch. Environ. Contam. Toxicol. 2002, 42, <Fig. 2> Biological activity of tetracycline metabolites. 5

12 Ⅱ. 연구내용및방법. <Table 3> Tetracyclines in dung slurry of cow, pig and chicken in China Tetracyclines Animal Detection (%) Min (mg/kg) Max (mg/kg) Mean (mg/kg) Source : Science of the Total Environment 2010, 408,

13 Ⅱ. 연구내용및방법 7

14 Ⅱ. 연구내용및방법 <Table 4> Previously reported analytical methods for tetracycline and their transformation products Sample Extraction Cleanup Analysis MDL Ref. 8

15 Ⅱ. 연구내용및방법 9

16 Ⅱ. 연구내용및방법 α β. ( 가 ) 시약 ( 나 ) 초자 10

17 Ⅱ. 연구내용및방법 ( 가 ) 질량분석기 ( 나 ) 액체크로마토그래피 ( 가 ) 시료의준비 11

18 Ⅱ. 연구내용및방법 ( 나 ) 고체상추출법 12

19 Ⅱ. 연구내용및방법. 13

20 Ⅱ. 연구내용및방법 <Fig. 3> Environmental samples(wastewater and surface water). 14

21 Ⅲ. 연구결과및고찰 Ⅲ. LC/MS/MS α β α β α β 15

22 Ⅲ. 연구결과및고찰 <Table 5> Precursor ions and product ions of tetracyclines and their metabolites Compounds α α β β Precursor ion Tube lens Product ion Collision energy 16

23 Ⅲ. 연구결과및고찰 <Table 6> Analytical condition of LC/MS/MS LC/MS/MS Analytical parameters μ μ 17

24 Ⅲ. 연구결과및고찰 <Fig. 4> LC/MS/MS chromatogram of tetracyclines and their metabolites. 18

25 Ⅲ. 연구결과및고찰 <Fig. 5> Calibration curve of tetracycline and metabolites(x=ng, Y=Peak). 19

26 Ⅲ. 연구결과및고찰 <Fig. 6> Calibration curve of chlortetracycline and metabolites(x=ng, Y=Peak). <Fig. 7> Calibration curve of oxytetracycline and metabolites(x=ng, Y=Peak). 20

27 Ⅲ. 연구결과및고찰. SPE α β 21

28 Ⅲ. 연구결과및고찰 <Fig. 8> Pretreatment of tetracyclines and their metabolites using HLB cartridge. < F ig. 9 > P re tre a tm e n t o f te tra cyclin e s a n d th e ir m e ta b o lite s u sin g M A X α β 22

29 Ⅲ. 연구결과및고찰 <Table 7> Precision and accuracy of SPE-LC/MS/MS analysis No. Compounds Extraction Recovery (%) RSD (%) Recovery (%) Clean up RSD (%) α β 23

30 Ⅲ. 연구결과및고찰 <Table 8> Method detection limit of tetracyclines and their metabolites No. Compounds MDL(ng) n=10, t=2.821 Recovery (%) RSD (%) α β 24

31 Ⅲ. 연구결과및고찰.. β α 25

32 Ⅲ. 연구결과및고찰 <Fig. 10> Detected level of tetracycline and their metabolites in wastewater and surface water samples. 26

33 Ⅳ. 결론 Ⅳ α β α β α β α β β 27

34 Ⅳ. 결론 α 28

35 참고문헌 29

36 참고문헌 30

37 부 록 31

38 부 록 < 부록 Fig. 1> Mass spectrum of tetracycline. < 부록 Fig. 2> Mass spectrum of 4-Epitetracycline. 32

39 부 록 < 부록 Fig. 3> Mass spectrum of tetracycline of anhydrotetracycline. < 부록 Fig. 4> Mass spectrum of 4-Epianhydrotetracycline. 33

40 부 록 < 부록 Fig. 5> Mass spectrum of chlortetracycline. < 부록 Fig. 6> Mass spectrum of 4-Epichlortetracycline. 34

41 부 록 < 부록 Fig. 7> Mass spectrum of 4-Epianhydrochlortetracycline. < 부록 Fig. 8> Mass spectrum of oxytetracycline. 35

42 부 록 < 부록 Fig. 9> Mass spectrum of 4-Epioxytetracycline. < 부록 Fig. 10> Mass spectrum of α-apo-oxytetracycline. 36

43 부 록 < 부록 Fig. 11> Mass spectrum of β-apo-oxytetracycline. 37

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