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GC/ECD를 이용한 농산물 중 생장조정제 dichlorprop 잔류 분석법 확립

Establishment of Analytical Method for Dichlorprop Residues, a Plant Growth Regulator in Agricultural Commodities Using GC/ECD

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참고문헌

키워드

주제분류농학

초록

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP;2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient (r 2) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %)was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity,repeatability and reproducibility.

Abstract

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP;2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient (r 2) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %)was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity,repeatability and reproducibility.

참고문헌 (13)

  1. Agust´ı, M., "Effect of the synthetic auxin 2,4-DP on fruit development of loquat", Plant Growth Regul, 41, pp.129~132 (2003)
  2. AOAC, "Pesticide and industrial chemical residues, In official method of analysis", pp.1~88 (2000), AOAC International
  3. 장희라, "식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-", 한국환경농학회지, 31(2), pp.157~163 (2012), 한국환경농학회
  4. 도정아, "LC-MS", MS를 이용한 농산물 중 pyrimisulfan 잔류량 분석법 개발 및 확인, 2013, pp.26(2), 154~163[DOI]
  5. 도정아, "HPLC-UVD를 이용한 농산물 중 살충제 sulfoxaflor의 시험법 개발 및 검증", 한국식품과학회지, 45(2), pp.148~155 (2013), 한국식품과학회[DOI]
  6. Inoue, K., "Use of chiral derivatization for the determination of dichlorprop in tea samples by ultra performance LC with fluorescence detection", J. Sep. Sci, 36, pp.1356~1361 (2013)
  7. 김미옥, "LC", MS, 한국식품과학회지, pp.2010, 42(6)[DOI]
  8. Lee, C. S., "Effects of dichlorprop and GA3 on storability of ‘Tsugaru’ apple fruits", Hort. Environ. Biotechnol, 41, pp.56~60 (2000)
  9. Ma, Y., "Enantioselective separation and degradation of the herbicide dichlorprop methyl in sediment", Chirality, 21, pp.480~483 (2009)
  10. Park, J. E., "Fact-finding survey on plant growth regulators use at farmer's level", Korean J. Weed Sci, 20, pp.309~314 (2000)
  11. Raina, R., "Liquid chromatography with post-column reagent addition of ammonia in methanol coupled negative ion electrospray ionization tandem mass spectrometry for determination of phenoxyacid herbicides and their degradation products in surface water", Anal. Chem. Insights, 5, pp.1~14 (2010)
  12. Thorstensen, C. W., "Development of a solid-phase extraction method for phenoxy acids and bentazone in water and comparison to liquid-liquid extraction method", J. Agric. Food Chem, 48, pp.5829~5833 (2000)
  13. West, A., "Comparison of HPLC and CE for the analysis of dichlorprop in a case of intoxication", Int. J. Legal Med, 110, pp.251~253 (1997)

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