FT-NMR as an analytical tool for identification of inert materials in crop protection products

농약제품분석의 정성분석도구로서 FT-NMR

  • 최달순 (농업과학기술원 유해물질과) ;
  • 경석헌 (건국대학교 분자생명공학부) ;
  • 홍수명 (농업과학기술원 유해물질과) ;
  • 진용덕 (농업과학기술원 유해물질과) ;
  • 이해근 (농업과학기술원 유해물질과) ;
  • 김진화 (농업과학기술원 유해물질과) ;
  • 류갑희 (농업과학기술원 유해물질과)
  • Published : 2004.06.30

Abstract

In order to evaluate NMR spectrometer as the analytical tool for identification of individual adjuvant in crop protection products, the standard sample of individual adjuvant was analyzed by NMR spectrometer and then the formulation of crop protection products was also analyzed. Almost polymer system of surfactant was a co-polymer and there was an excess of ethylene. The most intense signal comes from long polyethylene blocks, 70.5 ppm. The carbonyl groups of ester group resonate at 173.5 ppm. Analytical sample was prepared in NMR tube without extraction, cleanup, concentration, or chromatographic separation. Identification of individual adjuvant in crop protection products was conducted by comparison of sample and reference spectra. NMR spectrometer was useful to analyze adjuvant in crop protection products without preparation process.

농약제품 중 개별부자재의 확인을 위한 분석도구로서 NMR 분광기를 사용하였고 부자재의 표준품 및 농약제품을 분석 비교하였다. 고분자물질인 계면활성제는 co-polymer였고 많은 ethylene 그룹으로 이루어졌다. 가장 두드러진 signal은 긴 체인의 polyoxyethylene 그룹으로 70.5 ppm에서 나타났고 Ester의 carbnyl 그룹은 173.5 ppm에서 자기공명 signal을 확인할 수 있었다. 분석 시료는 정제, 농축, 또는 크로마토그래피의 과정 없이 준비되었고 개별부자재의 확인은 분석된 시료와 표준품 스펙트럼과의 비교에 의하여 가능할 수 있었다. NMR 분광기는 전처리과정 없이 농약제품 중 개별부자재의 분석이 가능하였다.

Keywords

References

  1. Charles, J. S., D. G. Crosby, K. W. Moilanen, J. N. Seiber and J. E. Woodrow (1975) Occurrence of trifluralin and its photoproducts in air, J. Agric. Food Chem 23(2):304-309 https://doi.org/10.1021/jf60198a003
  2. Greenhalgh, R., B. A. Blackwell, C. M. Preston and W. J. Murray (1983) Phosphorus-31 nuclear magnetic resonance analysis of technical organophosphorus insecticides for toxic contaminants, J. Agric. Food Chem. 31:710-713
  3. Gunther, H. (1995) NMR Spectroscopy, second edition, John Wiley & Sons
  4. Mazzola, E. P., A. P. Borsetti, S. W. Page and D. W. Bristol (1984) Determination of pesticide residues in foods by fluorine-19 fourier transform nuclear magnetic resonance spectroscopy, J. Agric. Food Chem 32:1102-1103 https://doi.org/10.1021/jf00125a043
  5. Mortimer, R. D. and B. A. Dawson (1991) A study to determine the feasibility of using $^{31}P$ NMR for the analysis of organophosphorus insecticide residues in cole crops, J. Agric. Food Chem 39:911-91 https://doi.org/10.1021/jf00005a022
  6. Mortimer, R. D. and B. A. Dawson (1991) Using $^{19}F$ NMR for trace analysis of fluorinated pesticides in food products, J. Agric. Food Chem 39:1781-1785 https://doi.org/10.1021/jf00010a018
  7. Mortimer, R. D., D. B. Black and B. A. Dawson (1994) Pesticide residue analysis in foods by NMR. 3. Comparison of $^{19}F$ NMR and GC-ECD for analyzing trifluralin residues in Field-Grown Carrots, J. Agric. Food Chem 42: 1713~ 1716
  8. Scott, A. M. and G. C. Donald (1995) $^{19}F$ NMR as an analytical tool for fluorinated agrochemical research, J. gric. Food, Chem. 43:1845 -1848