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Korean Journal of Environmental Agriculture

Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS

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@article{HGNHB8_2022_v41n2_82,
author={Sun Young. Gu and Su Jung. Lee and Hye-Sun. Shin and Sung Eun. Kang and Yun Mi. Chung and Jung Mi. Lee and Yong-hyun. Jung and Guiim. Moon},
title={Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS},
journal={Korean Journal of Environmental Agriculture},
issn={1225-3537},
year={2022},
volume={41},
number={2},
pages={82-94},
doi={10.5338/KJEA.2022.41.2.11},
url={https://doi.org/10.5338/KJEA.2022.41.2.11}

TY - JOUR
AU - Gu, Sun Young.
AU - Lee, Su Jung.
AU - Shin, Hye-Sun.
AU - Kang, Sung Eun.
AU - Chung, Yun Mi.
AU - Lee, Jung Mi.
AU - Jung, Yong-hyun.
AU - Moon, Guiim.
TI - Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS
T2 - Korean Journal of Environmental Agriculture
PY - 2022
VL - 41
IS - 2
PB - The Korean Society of Environmental Agriculture
SP - 82-94
SN - 1225-3537
AB - nullBACKGROUND:Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products.METHODS AND RESULTS:Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively.CONCLUSION(S):Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.
KW - Agricultural product
KW - Analytical method
KW - Insecticide
KW - LC-MS/MS
KW - Spiropidion
DO - 10.5338/KJEA.2022.41.2.11
UR - https://doi.org/10.5338/KJEA.2022.41.2.11
ER -

Gu, S. Y., Lee, S. J., Shin, H. S., Kang, S. E., Chung, Y. M., Lee, J. M., Jung, Y. H., & Moon, G. (2022). Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS. Korean Journal of Environmental Agriculture, 41(2), 82-94.

Gu, SY, Lee, SJ, Shin, HS, Kang, SE, et al. 2022, “Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS”, Korean Journal of Environmental Agriculture, vol. 41, no. 2, pp. 82-94. Available from: doi:10.5338/KJEA.2022.41.2.11

Gu, Sun Young et al. “Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS.” Korean Journal of Environmental Agriculture 41.2 (2022): 82-94.

1. Gu SY, Lee SJ, Shin HS, Kang SE, Chung YM, Lee JM, Jung YH, Moon G. Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS. Korean Journal of Environmental Agriculture [Internet]. 2022;41(2): 82-94. Available from: doi:10.5338/KJEA.2022.41.2.11.

Gu, Sun Young, Su Jung Lee, Hye-Sun Shin, Sung Eun Kang, Yun Mi Chung, Jung Mi Lee, Yong-hyun Jung and Guiim Moon. “Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS.” Korean Journal of Environmental Agriculture 41, no.2 (2022): 82-94. doi: 10.5338/KJEA.2022.41.2.11.

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Korean Journal of Environmental Agriculture

p-ISSN 1225-3537
e-ISSN 2233-4173

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Article History

Received2022-04-15
Revised2022-05-12
Accepted2022-05-27

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Citation

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Korean Journal of Environmental Agriculture

2022. Vol.41. n2. pp.82-94

DOI : https://doi.org/10.5338/KJEA.2022.41.2.11

Number of citation : 0
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Abstract

BACKGROUND:

Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products.

METHODS AND RESULTS:

Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively.

CONCLUSION(S):

Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

Keyword

Agricultural product,Analytical method,Insecticide,LC-MS/MS,Spiropidion