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Establishment of Analytical Method for Pesticide Multiresidue in Soil and Water using HPLC-UVD/FLD

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dc.contributor.advisor김정한-
dc.contributor.author김병준-
dc.date.accessioned2017-07-14T06:42:59Z-
dc.date.available2017-07-14T06:42:59Z-
dc.date.issued2014-08-
dc.identifier.other000000021831-
dc.identifier.urihttps://hdl.handle.net/10371/125874-
dc.description학위논문 (석사)-- 서울대학교 대학원 : 농생명공학부, 2014. 8. 김정한.-
dc.description.abstractTo ensure safety of the soil and water directly related to food safety at large, 85 pesticides multiresidue analysis using HPLC-UVD/FLD for soil and water was established. Based on 73 pesticides (3 UVD-groups, 2 FLD-groups) on the list of the NAQS (National Agricultural Products Quality Management Service) for crops and vegetable, 12 pesticides were newly added considering the type of groups and retention time. UVD-group 3 and FLD-group 1, 2 sensitivity was enhanced by modifying detection wavelengths. Soil wetting (NH4Cl) and various extraction solvents (acetonitrile, dichloromethane, ethyl acetate) were attempted for the optimization of sample treatment of soil and water. Acetonitrile+saturated solution 30 mL (for soil) and acetonitrile+NaCl 20 g (for water) in general had the best recovery result. Established method was validated with linearity, selectivity, sensitivity, statistical LOD/LOQ, working range, method LOD/LOQ, trueness and precision, measurement uncertainty and ruggedness. Also system suitability test was performed by retention factor, separation factor, number of theoretical plate, resolution and symmetry.-
dc.description.tableofcontentsAbstract ⅰ
List of tables ⅵ
List of figures ⅶ
I. Introduction 1
1.1. Pesticides and environmental safety 1
1.2. Pesticide multiresidue analysis 3
1.3. System suitability test 6
1.4. Method validation 7
II. Material and Methods 17
1. Materials and reagents 17
1.1. Pesticides standard 17
1.2. Reagents and apparatus 17
2. Instruments and analytical condition 18
2.1. Instruments 18
2.2. Analytical condition 19
3. Standard solution mixture 19
4. Sampling for soil and water 20
5. Establishment of analytical condition of pesticide multiresidue analysisin soil and water 21
5.1 Analysis of 73 pesticides in the NAQSs pesticide multiresidue method 21
5.2. Optimization of UVD absorption wavelength 24
5.3. Optimization of FLD absorption wavelength 24
5.4. Addition of new pesticides 24
6. System suitability test 25
7. Establishment of sample treatment of pesticide multiresidue in soil and water 26
7.1. Confirmation of SPE cartridges efficiency 28
7.2. Comparing wetting condition in soil extraction 28
7.3. Comparing soil extraction condition 29
7.4. Comparing water extraction condition 30
8. Method validation on pesticide multiresidue analysis in soil and water followed by KOLAS-G-015 guideline 31
8.1. Linearity 32
8.2. Sensitivity 32
8.3. Statistic LOD/LOQ 33
8.4. Working range 33
8.5. Selectivity 34
8.6. Trueness and Precision 34
8.7. Method LOD/LOQ 35
8.8. Ruggedness 35
8.9. Measurement uncertainty 36
III. Results and Discussion 37
1. Establishment of analytical condition in HPLC-UVD/FLD 37
1.1. Addition of 1 pesticides in UVD and FLD groups 37
1.2. New analytical condition in HPLC-UVD/FLD 39
2. Establishment of sample treatment of pesticide multiresidue in soil and water analyzing by HPLC-UVD/FLD 49
2.1. Establishing SPE cartridges efficiency 51
2.2. Establishing wetting condition in soil extraction 54
2.3. Establishing soil extraction condition 56
2.4. Establishing water extraction condition 59
3. System suitability test 62
4. Method validation based on KOLAS-G-015 guideline 65
4.1. Linearity 65
4.2. Sensitivity 69
4.3. Statistic LOD/LOQ 71
4.4. Working range 73
4.5. Selectivity 75
4.6. Trueness and precision 77
4.7. Method LOD/LOQ 79
4.8. Ruggedness 81
4.9. Measurement uncertainty 83
IV. Conclusion 97
Reference 99
국문요약 103
감사의 글 105
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dc.formatapplication/pdf-
dc.format.extent3942081 bytes-
dc.format.mediumapplication/pdf-
dc.language.isoen-
dc.publisher서울대학교 대학원-
dc.subjectPesticide-
dc.subject.ddc630-
dc.titleEstablishment of Analytical Method for Pesticide Multiresidue in Soil and Water using HPLC-UVD/FLD-
dc.typeThesis-
dc.contributor.AlternativeAuthorByung Joon Kim-
dc.description.degreeMaster-
dc.citation.pagesvii, 106-
dc.contributor.affiliation농업생명과학대학 농생명공학부-
dc.date.awarded2014-08-
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