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 Dichlobentiazox in Agricultural Products with LC-MS/MS

LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 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, Han Sol (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Park, Ji-Su (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) ;
  • Choi, Ha Na (Hazardous Substances Analysis Division, Gwangju Regional Food and Drug Administration) ;
  • Yoon, Sang Soon (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, Young-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) ;
  • Yoon, Hae 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)
  • 구선영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이한솔 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 박지수 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이수정 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 신혜선 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강성은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정윤미 (식품의약품안전처 광주지방식품의약품안전청 유해물질분석과) ;
  • 최하나 (식품의약품안전처 광주지방식품의약품안전청 유해물질분석과) ;
  • 윤상순 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정용현 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 윤혜정 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2021.03.29
  • Accepted : 2021.06.22
  • Published : 2021.06.30
Download PDF
⟨ Previous Next ⟩

Abstract

BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C18 showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides 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 (20161MFDS606).

References

  1. Umetsu N, Shirai Y (2020) Development of novel pesticides in the 21st century. The Korean Journal of Pesticide Science, 45(2), 55-74. https://doi.org/10.1584/jpestics.D20-201.
  2. Food Safety Commission of Japan (FSCJ) (2020) Dichlobentiazox (Pesticides). Food Safety, 8(1), 6-7. https://doi.org/10.14252/foodsafetyfscj.D-20-00002.
  3. Anastassiades M, Lehotay SJ, Tajnbaher D, Schenck 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, 412-431. https://doi.org/10.1093/jaoac/86.2.412.
  4. Rahman MM, Kim SW, Na TW, Abd El-Aty AM, Lee YJ, Park JS, Shim JH 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.
  5. 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.
  6. Naik RH, Pallavi MS, Kumar KP, Vanitha BK, Reddy VCS, Shwetha A, Bheemanna M et al. (2021). Deter-mination of 72 chemical pesticides and estimation of measurement of uncertainty in rice using LC-MS/MS and GC-MS/MS. Food Analytical Methods, 1-18. https://doi.org/10.1007/s12161-021-02000-9.
  7. Zheng W, Park JA, Abd El-Aty AM, Kim SK, Cho SH, Choi JM, Shin HC et al. (2018). Development and validation of modified QuEChERS method coupled with LC-MS/MS for simultaneous determination of cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its metabolite in various types of honey and royal jelly. Journal of Chromatography B, 1072, 60-69. https://doi.org/10.1016/j.jchromb.2017.11.011.
  8. Melo MG, Carqueijo A, Freitas A, Barbosa J, Silva AS (2020). Modified QuEChERS Extraction and HPLCMS/MS for Simultaneous Determination of 155 Pesticide Residues in Rice (Oryza sativa L.). Foods, 9(1), 18. https://doi.org/10.3390/foods9010018.
  9. Huang Y, Shi T, Luo X, Xiong H, Min F, Chen Y, Xie M et al. (2019). Determination of multi-pesticide residues in green tea with a modified QuEChERS protocol coupled to HPLC-MS/MS. Food Chemistry, 275, 255-264. https://doi.org/10.1016/j.foodchem.2018.09.094.
  10. 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.
  11. 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.
  12. Lehotay SJ, Son KA, Kwon H, Koesukwiwat U, Fu W, Mastovska K, Leepipatpiboon N et al. (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.
  13. Rejczak T, Tuzimski T (2015). A review of recent developments and trends in the QuEChERS sample preparation approach. Open Chemistry, 1(open-issue). https://doi.org/10.1515/chem-2015-0109.
  14. 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.
  15. Mallet CR, Lu Z, Mazzeo JR (2004) A study of ion suppression effects in electrospray ionization from mobile phase additives and solid-phase extracts. Rapid Communications in Mass Spectrometry, 18(1), 49-58. https://doi.org/10.1002/rcm.1276.