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GC-ECD를 이용한 농산물 중 제초제 aclonifen의 공정분석법 확립

Development of an Official Analytical Method for Determination of Aclonifen in Agricultural Products Using GC-ECD

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초록

BACKGROUND: Aclonifen is used as a systemic andselective herbicide to control a wide spectrum broad-leafweeds by inhibition carotenoid biosynthesis, and then itsMRLs(Maximum Residue Limits) will be determined inonion and garlic. In this study, a new official method wasdeveloped for aclonifen determination in agriculturalproducts to routinely inspect the violation of MRL as wellas to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extractedfrom crop samples with acetone and the extract waspartitioned with dichloromethane and then purified bysilica solid phase extraction(SPE) cartridge. The purifiedsamples were detected GC using an ECD detector. Limits ofdetection(LOD) was 0.001 mg/kg and quantification(LOQ)was 0.005 mg/kg, respectively. For validation purposes,recovery studies were carried out at three differentconcentration levels (LOQ, 10×LOQ, 50×LOQ, n=5). Therecoveries were ranged from 74.3 to 95.0% with relativestandard deviations(RSDs) of less than 8%. All values wereconsistent with the criteria ranges requested in the Codexguidelines(CAC/GL 40). CONCLUSION: The proposed analytical method wasaccurate, effective and sensitive for aclonifen determinationand it will be used to as an official method in Korea.

Abstract

BACKGROUND: Aclonifen is used as a systemic andselective herbicide to control a wide spectrum broad-leafweeds by inhibition carotenoid biosynthesis, and then itsMRLs(Maximum Residue Limits) will be determined inonion and garlic. In this study, a new official method wasdeveloped for aclonifen determination in agriculturalproducts to routinely inspect the violation of MRL as wellas to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extractedfrom crop samples with acetone and the extract waspartitioned with dichloromethane and then purified bysilica solid phase extraction(SPE) cartridge. The purifiedsamples were detected GC using an ECD detector. Limits ofdetection(LOD) was 0.001 mg/kg and quantification(LOQ)was 0.005 mg/kg, respectively. For validation purposes,recovery studies were carried out at three differentconcentration levels (LOQ, 10×LOQ, 50×LOQ, n=5). Therecoveries were ranged from 74.3 to 95.0% with relativestandard deviations(RSDs) of less than 8%. All values wereconsistent with the criteria ranges requested in the Codexguidelines(CAC/GL 40). CONCLUSION: The proposed analytical method wasaccurate, effective and sensitive for aclonifen determinationand it will be used to as an official method in Korea.

참고문헌 (7)

  1. Kilinc, O., "The herbicide aclonifen: The complex theoretical bases of sunflower tolerance", Pestic. Biochem. Physiol, 100, pp.193~198 (2011)
  2. Lagana, A., "Determination of diphenyl-ether herbicides and metabolites in natural waters using high-performance liquid chromatography with diode array tandem mass spectrometric detection", Anal. Chim. Acta, 414, pp.79~94 (2000)
  3. Macbean, C., "The pesticide manual, sixteenth ed", BCPC, 16~17 (2012)
  4. Lee, Y.D., "Practical book of Korea Food Code pesticide residue analysis method", Mistry of Food & Drug Safety, 294~918 (2013)
  5. Ministry of Food and Drug Safety, "Analytical methods of pesticide residues in foods, fourth ed", NIFDS, 294~918 (2013)
  6. Reyes, R.C., "Single solid phase extraction method for the simultaneous analysis of polar and non-polar pesticides in urine samples by gas chromatography and ultra high pressure liquid chromatography couples to tandem mass spectrometry", Talanta, 85, pp.183~196 (2011)
  7. Sicbaldi, F., "Use of gas-liquid chromatography with electron-capture and thermionic-sensitive detection for the quantitation and identification of pesticide residues", J. Chromatography A, 765, pp.13~22 (1997)

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