Determination of Amisulbrom Residues in Agricultural Commodities Using HPLC-UVD/MS

HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석

  • Received : 2014.12.02
  • Accepted : 2014.12.20
  • Published : 2014.12.31


This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.




  1. AOAC (2000) 'Pesticide and industrial chemical residues, In Official method of analysis', 17th ed., pp. 1-88, AOAC International, Arlington, VA, USA.
  2. Ardrey, R, E. (2003) Liquid Chromatography-Mass Spectrometry, pp. 98-122, Wiley, West Sussex, UK.
  3. Codex Alimentarius Commission (2003) Guidelines on Good Laboratory Practice in Residue Analysis, CAC/GL 40-1993, Rev.1-2003, Rome, Italy.
  4. Fong, W. G., H. A. Moye, J. N. Seiber and J. P. Toth (1999) Pesticide Residues in Food: Methods, Technologies, and Regulations, Wiley Interscience. pp. 3-4, 40-44, Canada.
  5. Hwang, K. W., T. W. Kim, J. H. Yoo, B. S. Park and J. K. Moon (2012) Dissipation pattern of amisulbrom in cucumber under greenhouse condition for establishing pre-harvest residue limit, Korean J. Pestic. Sci. 16(4):288-293.
  6. Korea Crop Protection Association (2014) Using guideline of crop protection agents, pp. 154-156.
  7. Korea food and drug administration (2012) Korea Food Code, pp. 10-4-340-10-4-342.
  8. Kwon, C. H., M. I. Chang, M. H. Im, H. Choi, D. I. Jung, S. C. Lee, J. Y. Yu, Y. D. Lee, J. O. Lee and M. K. Hong (2008) Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry. Analytical Sci. & Technoligy, 21(6):518-525.
  9. Lee, J. H., Y. Keum . Park, C. Kwon, Y. Lee and J. Kim (2008) Dissipation pattern of boscalid in cucumber under green house condition. Korean Journal of Pesticide Science, 12:67-73.
  10. Lee, Y. D. (2012) Pesticide Analytical Residues Manual in Food Code, pp. 3, 78-80, NiFDS, Korea.
  11. McLafferty, F. W. and Turecek, F. (1993) Interpretation of Mass Spectra, 4th ed., pp. 19-50, University Science Books, Sausalito, CA, USA.
  12. Miller, J. M. (2005) Chromatography : Concepts and Contrasts (2nd), Wiley Intersciense, p. 286-287, USA, Standardization Administration of the People's Republic.
  13. Ministry of Food and Drug Safety (2014) MRLs for Pesticides in Foods, pp. 150-151.
  14. US EPA (2011) Pesticide Fact Sheet for Amisulbrom. Washington D.C., 20460.
  15. US FDA (1999) Pesticide Analytical Manual, Vol 1: Multiresidue Methods (3rd ed.), US Food and Drug Administration, USA.

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