Korean Journal of Environmental Agriculture (한국환경농학회지)

The Korean Society of Environmental Agriculture (한국환경농학회)
권호 표지
DOI QR코드

DOI QR Code

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

LC-MS/MS를 이용한 농산물 중 Spiropidion 및 대사산물 Spiropidion-enol (SYN547305) 시험법 개발 및 검증

  • Gu, Sun Young (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Su Jung (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Shin, Hye-Sun (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kang, Sung Eun (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chung, Yun Mi (Hazardous Substances Analysis Division, Gwangju Regional Food and Drug Administration) ;
  • Lee, Jung Mi (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Jung, Yong-hyun (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Moon, Guiim (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 구선영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이수정 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 신혜선 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강성은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정윤미 (식품의약품안전처 광주지방식품의약품안전청 유해물질분석과) ;
  • 이정미 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정용현 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 문귀임 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2022.04.15
  • Accepted : 2022.05.27
  • Published : 2022.06.30
Download PDF
⟨ Previous Next ⟩

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.

Keywords

Acknowledgement

This study was supported by the Ministry of Food and Drug Safety (MFDS), Republic of Korea under the paradigm of a study on risk assessment and establishment of new analytical method for safety management of pesticide residues in food (21161MFDS 364).

References

  1. Umetsu N, Shirai Y (2020) Development of novel pesticides in the 21st century. Journal of Pesticide Science, 45(2), 55-74. https://doi.org/10.1584/jpestics.D20-201.
  2. Brownsey RW, Boone AN, Elliott JE, Kulpa JE, Lee WM (2006) Regulation of acetyl-CoA carboxylase. Biochemical Society Transactions, 34(2), 223-227. https://doi.org/10.1042/BST0340223.
  3. Anastassiades M, Lehotay SJ, Stajnbaher D, chenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce. Journal of AOAC International, 86(2), 412-431. https://doi.org/10.1093/jaoac/86.2.412.
  4. Yang Y, Lin G, Liu L, Lin T (2022) Rapid determination of multi-antibiotic residues in honey based on modified QuEChERS method coupled with UPLC-MS/MS. Food Chemistry, 374, 131733. https://doi.org/10.1016/j.foodchem.2021.131733.
  5. Wu Y, An Q, Li D, Kang L, Zhou C, Zhang J, Pan C (2022) Multi-residue analytical method development and risk assessment of 56 pesticides and their metabolites in tea by chromatography tandem mass spectroscopy. Food Chemistry, 375, 131819. https://doi.org/10.1016/j.foodchem.2021.131819.
  6. Harischandra NR, Pallavi MS, Bheemanna M, PavanKumar K, Reddy VCS, Udaykumar NR, Paramasivam M, Yadav S (2021) Simultaneous determination of 79 pesticides in pigeonpea grains using GC-MS/MS and LC-MS/MS. Food Chemistry, 347, 128986. https://doi.org/10.1016/j.foodchem.2020.128986.
  7. Harischandra Naik R, Pallavi MS, Pavan Kumar K, Vanitha BK, Chandra Sekhara Reddy V, Shwetha A, Nandini S, Naveenkumar P, Udaykumar Nidoni R et al. (2021) Determination of 72 chemical pesticides and estimation of measurement of uncertainty in rice using LC-MS/MS and GC-MS/MS. Food Analytical Methods, 14(9), 1788-1805. https://doi.org/10.1007/s12161-021-02000-9.
  8. Melo MG, Carqueijo A, Freitas A, Barbosa J, Silva AS (2020) Modified QuEChERS Extraction and HPLC-MS/MS for Simultaneous Determination of 155 Pesticide Residues in Rice (Oryza sativa L.). Foods, 9(1), 18. https://doi.org/10.3390/foods9010018.
  9. Hu M, Qiu J, Zhang H, Fan X, Liu K, Zeng D, Tan H (2018) Method development and validation of indaziflam and its five metabolites in soil, water, and fruits by modified QuEChERS and UHPLC-MS/MS. Journal of Agricultural and Food Chemistry, 66(39), 10300-10308. https://doi.org/10.1021/acs.jafc.8b04186.
  10. Guo Q, Zhao S, Zhang J, Qi K, Du Z, Shao B (2018). Determination of fipronil and its metabolites in chicken egg, muscle and cake by a modified QuEChERS method coupled with LC-MS/MS. Food Additives & Contaminants: Part A, 35(8), 1543-1552. https://doi.org/10.1080/19440049.2018.1472395.
  11. Rahman MM, Kim SW, Na TW, Abd El-Aty AM, Lee YJ, Park JS, Ramadan A, Lee HS, Chung HS et al. (2016) QuEChERS method for the simultaneous quantification of phorate and its metabolites in porcine and chicken muscle and table eggs using ultra-high performance liquid chromatography with tandem mass spectrometry. Journal of Separation Science, 39(11), 2079-2086. https://doi.org/10.1002/jssc.201600151.
  12. Rejczak T, Tuzimski T (2015) A review of recent developments and trends in the QuEChERS sample preparation approach. Open Chemistry, 13(1), 980-1010. https://doi.org/10.1515/chem-2015-0109.
  13. Lehotay SJ, Son KA, Kwon H, Koesukwiwat U, Fu W, Mastovska K, Hoh E, Leepipatpiboon N (2010) Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. Journal of Chromatography A, 1217 (16), 2548-2560. https://doi.org/10.1016/j.chroma.2010.01.044.
  14. Lehotay SJ, Mastovska K, Lightfield AR (2005) Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. Journal of AOAC International, 88(2), 615-629. https://doi.org/10.1093/jaoac/88.2.615.
  15. Wilkowska A, Biziuk M (2011) Determination of pesticide residues in food matrices using the QuEChERS methodology. Food Chemistry, 125, 803-812. https://doi.org/10.1016/j.foodchem.2010.09.094.