Establishment of certified reference material for pesticides using mass balance and differential scanning calorimetry: acynonapyr, flometoquin, bifenazate, and metabolite bifenazate diazene
Mass balance 및 differential scanning calorimetry를 사용한 농약 인증표준물질의 개발: acynonapyr, flometoquin, bifenazate 및 대사체 bifenazate diazene
- 주제(키워드) Pesticide , Certified reference material , Mass balance method , Differential scanning calorimetry , Characterization , Homogeneity , Stability , Uncertainty , Pooled uncertainty , Expanded uncertainty
- 주제(DDC) 651.1
- 발행기관 아주대학교
- 지도교수 백승훈
- 발행년도 2023
- 학위수여년월 2023. 8
- 학위명 석사
- 학과 및 전공 일반대학원 바이오헬스규제과학과
- 실제URI http://www.dcollection.net/handler/ajou/000000033076
- 본문언어 영어
- 저작권 아주대학교 논문은 저작권에 의해 보호받습니다.
초록/요약
Pesticides play a crucial role in modern agriculture as crop protectants for safeguarding crops and enhancing productivity. However, pesticide residues in food can be exposed to the human body and present a potential threat. Governments have implemented regulations on pesticide use and maximum residual levels in each agrifood to address this concern. In this study, certified reference materials (CRMs) of four candidate materials, namely acynonapyr, flometoquin, bifenazate, and bifenazate diazene were established by the interlaboratory collaboration with three institutions following ISO Guideline 35:2017. The CRMs were characterized using both mass balance (MB) and differential scanning calorimetry (DSC). Using both approaches can complement the limitations of a single method and result in highly accurate and reliable data. Homogeneity tests were conducted to evaluate the uniformity of the CRMs between bottles and within bottle. Furthermore, long- and short-term stability studies were performed at -20 ℃ for 12 months, and at 4 ℃, 25 ℃/60% relative humidity (RH), and 40 ℃/75% RH for 3 months. The test results confirmed that candidate CRMs are homogeneous and stable at the tested conditions and durations. Given the involving multiple laboratories, the pooled uncertainty was accounted for while estimating the expanded uncertainty. The accomplished CRMs offer the following purities and expanded uncertainties: acynonapyr 99.3% ± 0.6% (𝑘=2.262), flometoquin 98.9% ± 0.1% (𝑘=2.306), bifenazate 99.7% ± 1.2% (𝑘=4.303), bifenazate diazene 99.9% ± 0.7% (𝑘=2.776), respectively. The four CRMs were successfully established and can be reliable references for pesticide residue analysis in national testing agencies.
more목차
1. Introduction 1
1.1. Positive effects of pesticide 1
1.2. Side effects of pesticide 2
1.3. Importance of CRMs in the pesticide residue analysis 4
1.4. Candidate materials for CRM in this study 5
1.5. Aims of this study 6
2. Experimental 8
2.1. Chemicals and reagents 8
2.1.1. Candidate materials 8
2.1.2. Reagents 8
2.1.3. Packaging of the CRMs 9
2.2. Instrument and parameters 10
2.3. Mass balance (MB) method 11
2.3.1. HPLC for non-volatile organic impurity 11
2.3.2. GC for volatile organic impurity (residual solvent) 13
2.3.3. Karl-Fischer coulometric titration for moisture 16
2.3.4. Residue on ignition for inorganic impurity 17
2.4. Differential scanning calorimetry (DSC) method 18
2.5. Homogeneity test 19
2.6. Stability study 20
2.7. Statistical analysis 21
2.8. Value assignment 23
3. Results and discussion 24
3.1. Synthesis result of bifenazate diazene 24
3.2. Purity estimation by mass balance method 25
3.2.1. Non-volatile organic impurity assessment by HPLC-DAD 25
3.2.2. Volatile organic impurity assessment by GC 27
3.2.3. Overall purity by mass balance method 29
3.3. Purity estimation by DSC 30
3.4. Homogeneity test 32
3.5. Stability study 34
3.6. Uncertainty evaluation 39
3.6.1. Uncertainty of homogeneity test 39
3.6.2. Uncertainty of stability study 40
3.6.3. Uncertainty of mass balance and DSC 42
3.6.4. Purity and uncertainty of characterization 43
3.6.5. Uncertainty and expanded uncertainty of CRMs 44
3.7. Final assigned value of purity and uncertainty 46
4. Conclusion 47
Reference 49
국문요약 52
