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Analysis of Multiple Pesticide Residues in Apples and Pears Using Gas-Liquid Chromatography

Gas-Liquid Chromatography를 이용한 사과 및 배 중의 농약 다성분 잔류분석법

  • Park, Ju-Hwang (Department of Agricultural Chemistry, Kyungpook National University) ;
  • Kim, Taek-Kyum (Department of Agricultural Chemistry, Kyungpook National University) ;
  • Oh, Chang-Hwan (Lab Frontier Inc.) ;
  • Kim, Jeong-Han (School of Agricultural Biotechnology, Seoul National University) ;
  • Lee, Young-Deuk (Division of Life and Environmental Science, Daegu University) ;
  • Kim, Jang-Eok (Department of Agricultural Chemistry, Kyungpook National University)
  • Published : 2004.09.30

Abstract

A rapid analytical method was developed to determine multiple pesticide residues in apples and pears using gas-liquid chromatography (GLC). The samples were extracted with water-miscible solvents and purified by cleanup procedures serially comprising liquid-liquid partition and solid-phase extraction (SPE). Each analyte was separated and determined by a high-resolution GLC equipped with electron-capture detector (ECD) and nitrogen-phosphorous detector (NPD). A total of 196 pesticides, which were previously classified into 5 groups each for ECD and NPD based on their retention behaviors on the capillary column and responses to the detector, were subjected to the recovery experiment. In compliance with the analytical criteria, 70 to 120% of recovery and less than 20% relative standard deviation the proposed method could be successfully applied to analyze 136 and 133 pesticide residues in apples and pears, respectively, which enabled not only rapid screening but quantitation of the residues. Even though less reliability was resulted from unacceptable recovery range, rest of pesticides including 43 and 45 analyzes in apples and pears, could be also detected for their identity. The proposed method fliled to cover 17 and 18 pesticides for apples and pears, which mostly showed high polarity or heat-lability but could be suitable far fast surveilance or monitoring of fruit harvests.

사과 및 배 시표에서 농약 다성분의 gas chromatography를 이용한 잔류분석법 확립을 위하여 199가지의 농약을 선정하여 retention time 및 검출기에 따라 ECD 5 그룹 및 NPD 5 그룹의 10개 그룹으로 분류하였다. 시료의 종류에 따른 분석조건을 확립하기 위한 회수율 시험은 농약들의 log $P_{ow}$ 값과 화학적 분류에 따라 총 18개 (ECD 11개, NPD 7개)의 농약을 선정하였다. 예비 실험 후 확립된 분석방법에 따라 10개 그룹의 혼합 표준용액으로 사과 및 배에 대한 회수율시험을 행하였다. 그 결과, 총 196가지의 농약의 70%에 해당하는 사과에서 136개, 배에서 133개의 농약들에서 회수율 70에서 120%의 양호한 결과를 나타내었다. 그러나 사과에서 43개, 배에서 45개의 농약들이 70% 미만의 회수율을 보였고, fenvalerate는 120% 이상의 회수율을 나타내었으며, 사과에서 17개 및 배에서 18개의 농약들은 검출이 되지 않았다. 그러나 확립된 분석법은 SOP에 의한 신속하고 수월한 수행으로 농산물 중의 잔류농약을 검출 및 모니터링하는 목적에 적합하다고 사료된다.

Keywords

References

  1. 식품의약품안전청 (1999) 식품공전 P.37-106
  2. 식품의약품안전청 (1999) 식품공전 별책 제 7. 일반시험법,P.110-256
  3. 殘留農藥基準便覽 (1994) 日本食品衛生協會 173pp
  4. C, Patricia (1995) Official metthods of analysis AOAC international, Pesticide and industrial chemical residues, 16th ed., Chapter 10, USA
  5. Mcmahon, B. M. (1994) Pesticide Analytical Manual Volume I : Multiresidue Methods, 3rd ed., FDA. USA
  6. Pang, G. F., Cao, Y. J. and Fan, C. L. (1995) Modification of AOAC multiresidue method for determining synthetic pyrethroid residues in fruits, vegetables and grains, Part I : Acetonitrile extraction system and optimization of Florisil cleanup and chromatography, J.AOAC International 78(6), 1481-1488
  7. Zoonen, P. V. and Rijksinstituut, V. (1996) Analytical methods for pesticide residues in foodstuffs, 6th ed., Ministryof Public Health, Welfare and Sport, Netherlands
  8. Kim, T. J., Eo, Y. W. and Kim, Y. S. (1987) A Study on the Separation and Determination of Organochlorine Pesticides by Capillary Column Gas-liquid Chromatography, J. Korean Chem. Soc. 31(5), 425-433
  9. 김택제, 어연우(1990) 다성분 잔류농약 동시 분석법에 관한 연구(3차), KIAT 연구보고서
  10. Kim, W. S., Lee, B. H. and Park, H, J. (1996) Study on the Development of Simultaneous Analytical Method for the Residual Organic Chloride Pesticides by Gas Chromatography, J. Korean Environ Sci. 5(5), 561-567
  11. Niessner, G, Buchberger, W. and Eckerstorfer, R. (1999)Multiresidue screening methods for fhe determination ofpesticides in plant materials, J. Chromatogr. A 846, 341-348 https://doi.org/10.1016/S0021-9673(99)00198-3
  12. Serrano, R, Lopez, F. J. and Hemandez, F. (1999) Multiresidue determination of persistent organochlorine and organophosphorus compounds in whale tissues using automated liquid chromatographic clean up and gas chromatographic-mass spectrometric detection, J. Chromatogr. A 855, 633-643 https://doi.org/10.1016/S0021-9673(99)00706-2
  13. Colume, A., Cardenas, S., Gallego, M. and Valcairel, M.(2001) Semiautomatic multiresidue gas chromatographic method for the screening of vegetables for 25 organochlorine and pyrethroid pesticides, Anal. Chem. Acta 436,153-162 https://doi.org/10.1016/S0003-2670(01)00901-1
  14. Castro,J., Sanchez-Brunete, C. and Tadeo, J. L. (2001) Multiresidue analysis of insecticides in soil by gas chromatography with electron-capture detection and confirmation by gas chromatography-mass spectrometry, J.Chromatogr. A 918, 371-380 https://doi.org/10.1016/S0021-9673(01)00751-8
  15. Ho, W. H. and Hsieh, S. J. (2001) Solid phase microextraction associated with microwave assited extraction of organochlorine pesticides in medicinal plants, Anatytica Chimica Acta 428, 111-120 https://doi.org/10.1016/S0003-2670(00)01219-8
  16. Ahmed, F. E. (2001) Analyses of pesticides and their metabolites in foods and drinks, Trends in anal. chem.20(11), 649-661 https://doi.org/10.1016/S0165-9936(01)00121-2
  17. Valverde, A., Aguilera, A., Rodriguez, M. and Boulaid, M. (2001) What are we determining using gas chromatographic multiresidue methods: tralomethrin or deltamethrin?, J. Chromatogr. A 943, 101-111 https://doi.org/10.1016/S0021-9673(01)01414-5
  18. Lacassie, E., Marquet, P, Gaulier, J. M., Dreyfuss, M. F.and Lachahre, G. (2001) Sensitive and specific multiresidue methods for the determination of pesticides ofvarious classes in clinical and forensic toxicology, Forensic Sci. Int'l 121, 116-125 https://doi.org/10.1016/S0379-0738(01)00461-3
  19. Lehotay, S. J. (1997) SupercnticaI fluid extraction ot pesticide in foods, J. Chromatogr. A 785, 289-312 https://doi.org/10.1016/S0021-9673(97)00461-5
  20. Sabic, H., Jeannot, R., Roudeau, B. (2000) Muldresidue methods using solid-phase extraction techniques for monitoring priority pesticides, including triazines and degradation products, in ground and surface waters, J. Chromatogr. A 885, 217-236 https://doi.org/10.1016/S0021-9673(99)01084-5

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