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Development of pesticides and their metabolites certified reference materials using mass balance approach: Florylpicoxamid, X12485649, Spiropidion, and Spiropidion-enol

  • 이경진 (Kyungjin Lee, 아주대학교 일반대학원)

초록/요약

Despite their contribution to increasing agrifood production, concerns about the impacts of pesticides and their metabolites on environmental and human health have been persistently raised. Since the maximum residue levels of pesticides and their metabolites in agrifoods are legally regulated, development of certified reference materials (CRMs) is essential to ensure the reliability of residue analysis results. The aim of this study is to develop CRMs of florylpicoxamid, X12485649 (florylpicoxamid metabolite), spiropidion, and spiropidion-enol (spiropidion metabolite) following the ISO 33405:2024 guideline. Candidate CRMs were prepared in argon glove box by subdividing the target materials in vials and packaging with plastic bags. The characterization for the purity estimation was evaluated using a mass balance method by determination of impurities including organic impurities (HPLC-UV), inorganic impurities (residue on ignition), water (Karl Fischer coulometric titration), and residual solvents (GC-MS). Homogeneity, stability, and uncertainty estimation were assessed according to ISO 33405:2024. Expanded uncertainties were estimated by combining the uncertainties of characterization, homogeneity, and stability. Purities of candidate CRMs were estimated to be 97.737–99.665% (w/w), suggesting that target materials are high in purity and the major components in candidate CRMs. Homogeneity test results using ANOVA showed that all target materials are homogenous within and between the bottles. Short-term and long-term stability test at the stressed, accelerated, and storage conditions showed that all target materials are stable as assessed by linear regression and linear approximation analysis. In conclusion, purity ± expanded uncertainty of developed CRMs were florylpicoxamid (98.67 ± 0.82%), X12485649 (97.74 ± 0.07%), spiropidion (99.66 ± 0.20%), and spiropidion-enol (97.80 ± 0.66%). The established CRMs in this study can be used as references in pesticide residue analysis in foodstuffs of agricultural, dairy, and livestock products. They also contribute to ensuring food safety and promoting human health. Keywords Pesticide; Metabolite; Certified reference material; ISO 33405:2024; Mass balance method; Characterization; Homogeneity; Stability; Uncertainty

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목차

1. Introduction 1
1.1. Impact of pesticides on environment and human health 1
1.2. Development of CRM using mass balance method 3
1.3. Pesticide and its metabolite in this study 6
1.3.1. Florylpicoxamid and X12485649 6
1.3.2. Spiropidion and spiropidion-enol 7
1.4. Purpose of this study 8
2. Method 9
2.1. Chemicals 9
2.2. Instruments 9
2.3. Preparation of target pesticides or metabolites 10
2.4. Identification of target materials using LC-MS 10
2.5. The packaging process for the preparation of candidate CRMs 12
2.6. Mass balance method 13
2.6.1. Determination of organic impurity using HPLC-UV 13
2.6.2. Determination of inorganic impurity using residue on ignition 15
2.6.3. Determination of water using Karl-Fischer coulometric titration 16
2.6.4. Determination of residual solvent using GC-MS 17
2.6.5. Calculation of purity 20
2.7. Homogeneity 20
2.8. Stability 21
2.9. Uncertainty 24
2.9.1. Uncertainty of characterization 24
2.9.2. Uncertainty of homogeneity 27
2.9.3. Uncertainty of stability 28
2.9.4. Combined uncertainty 29
2.9.5. Expanded uncertainty 29
3. Results and discussion 30
3.1. Preparation of CRMs 30
3.1.1. Florylpicoxamid and X12485649 30
3.1.2. Spiropidion and spiropidion-enol 34
3.2. Characterization using the mass balance method 38
3.2.1. Organic impurity analysis using HPLC-UV 38
3.2.2. Solution stability of spiropidion 41
3.2.3. Residual solvents analysis using GC-MS 44
3.2.4. Determination of purity (%) 47
3.3. Homogeneity study 50
3.4. Stability study 55
3.5. Uncertainty 61
3.5.1. Uncertainty of characterization () 61
3.5.2. Uncertainty of homogeneity () 64
3.5.3. Uncertainty of stability () 64
3.5.4. Combined uncertainty () and expanded uncertainty () 64
3.6. Purity and expanded uncertainty of developed CRMs 66
4. Conclusion 68
Acknowledgements 69
References 70
국문 초록 73

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