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LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증

Determination and Validation of an Analytical Method for Dichlobentiazox in Agricultural Products with LC-MS/MS

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주제분류농학

초록

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.

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.

참고문헌 (15)

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  3. Anastassiades M, "Fast and Easy multiresidue method employing acetonitrile extraction", partitioning and"dispersive solid phase extraction"for the determination of pesticide residues in produce, 2003, pp.86, 412~431
  4. Rahman MM, "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), pp.2079~2086 (2016)[DOI]
  5. Harischandra NR, "Simultaneous determination of 79 pesticides in pigeonpea grains using GC-MS", MS and LC-MS, Food Chemistry, pp.2021, 347[DOI]
  6. Naik RH, "Determination of 72 chemical pesticides and estimation of measurement of uncertainty in rice using LC-MS", MS and GC-MS, Food Analytical Methods, pp.2021[DOI]
  7. Zheng W, "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, 2018, pp.1072, 60~69
  8. Melo MG, "Modified QuEChERS Extraction and HPLCMS", MS for Simultaneous Determination of 155 Pesticide Residues in Rice (Oryza sativa L.), 2020, pp.9(1), 18~
  9. Huang Y, "Determination of multi-pesticide residues in green tea with a modified QuEChERS protocol coupled to HPLC-MS", MS, 2019, pp.275, 255~264
  10. Hu M, "Method development and validation of indaziflam and its five metabolites in soil, water, and fruits by modified QuEChERS and UHPLC-MS", MS, 2018, pp.66(39), 10300~10308
  11. Lehotay SJ, "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), pp.615~629 (2005)[DOI]
  12. Lehotay SJ, "Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables", Journal of Chromatography A, 1217(16), pp.2548~2560 (2010)[DOI]
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  15. Mallet CR, "A study of ion suppression effects in electrospray ionization from mobile phase additives and solid-phase extracts", Rapid Communications in Mass Spectrometry, 18(1), pp.49~58 (2004)[DOI]

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