pH조절 분배추출에 의한 식물체 중 Methoxyfenozide와 Bentazone의 HPLC 분석

DOI QR코드

DOI QR Code

노석초;황철환;유기용;한성수
Lo, Seog-Cho;Hwang, Cheol-Hwan;Yoo, Ki-Yong;Han, Seong-Soo

  • 발행 : 2007.09.30

초록

이 연구는 액액분배과정 중 pH 조절에 의한 diacylhyazine계의 곤충생장조정(IGR)계 살충제 methoxyfenozide와 benzothiadiazinone계의 제초제 bentazone의 분배효율을 향상시키기 위하여 수행하였다. 현미시료는 두 약제 모두 "추출$\rightarrow$응고법$\rightarrow$분배추출$\rightarrow$florisil column chromatography"의 동일한 과정을 거쳤다. 볏짚시료에 있어서 methoxyfenozide는 "추출$\rightarrow$1 M-NaOH 용액에 의한 알칼리화$\rightarrow$분배추출$\rightarrow$응고법$\rightarrow$florisil column chromatography"의 과정을 거친 후 용리액인 acetonitrile : 20 mM sodium acetate(75:25, v/v)로 정용, HPLC로 분석하였다. Bentazone의 경우는 "추출$\rightarrow$1 M-NaOH 용액 첨가에 의한 알칼리화$\rightarrow$유기용매 세척$\rightarrow$12 M-HCl 의한 산성화$\rightarrow$분배추출$\rightarrow$florisil column chromatography"의 과정을 거쳤으며, acetonitrile : 75 mM sodium acetate(pH 6.0) (40:60, v/v)로 정용, HPLC로 분석 하였다. Methoxyfenozide의 회수율은 현미 83.5-97.4%, 볏짚 86.4-97.3%였으며, 분석법의 검출한계는 현미 0.02 mg/kg 볏짚 0.04 mg/kg이었다. Bentazone의 회수율은 현미 86.8-101.9 %, 볏짚 88.3-94.5%였으며, 분석법의 검출한계는 현미 0.005 mg/kg, 볏짚 0.01 mg/kg이었다. 본 연구결과에서 얻은 위 방법은 재현성 있는 안정적 분석조건을 제공한다는 점에서 두 약제의 잔류분석에 유용하게 적용될 수 있을 것으로 생각된다.

키워드

methoxyfenozide;bentazone;residue analysis;pH;HPLC

참고문헌

  1. Tomlin, C. D. S. (2000) The pesticide manual 12th edition, The British Crop Protection Council, Farnham, United Kingdom, p. 624
  2. Korea Crop Protection Council (2005) Pesticides application manual, Seoul, Korea, pp. 366-670
  3. Tomlin, C. D. S. (2000) The pesticide manual 12th edition, The British Crop Protection Council, Farnham, United Kingdom p. 80
  4. Kim, K. U. (1998) Principles of weed science, Kyungpook university press, Korea, p. 221
  5. Choi, B. K., Hercules, D. M and Gusev, A. I. (2001) Effect of liquid chromatography separation of complex matrices on liquid chromatography-tandem mass spectrometry signal suppression, J. Chromato. A. 907, 337-342 https://doi.org/10.1016/S0021-9673(00)01052-9
  6. Kim, S. 5., Lee, S. M., Koo, M. Y., Park, D. S. and Hur, J. H. (2003) Residual analysis and safety uses of methoxyfenozide and etofenprox in pastures, J. Agri. Sci. 14, 59-66
  7. Wu, S., Stein, R., Desai, T. B., Hofmann, C. K. and Burnett, T. F. (1998) Rohm and Haas Technical Report No. 34-98-71; Residue analytical method for parent RH-2485 in soil, Philadelphia, USA, p. 1-17
  8. Research group for pesticide residue analysis method (1995) Recent pesticide analysis method, Chuohoki publishers, Tokyo, Japan, p. 68-70
  9. Balinova, A. (1996) Ion-pairing mechanism in the solid-phase extraction and reversed-phase highperformance liquid chromatographic determination of acidic herbicides in water, J. Chromato. A. 728, 319-324 https://doi.org/10.1016/0021-9673(95)01139-0
  10. Fontanals, N., Calia, M, Marce, R. M. and Borrull, F. (2004) Solid-phase extraction of polar compounds with a hydrophilic copolymeric sorbent, J. Chromato. A. 1030, 63-68 https://doi.org/10.1016/j.chroma.2003.10.076
  11. Lee, P. W, Aizawa, H, Barefoot, A C. and Murphy, J. J. (2003) Handbook of residue analytical methods for agrochemicals, Wiley, Delaware, USA, p.773
  12. Hogendoorn, E. A, Westhuis, K, Dijkman, E., Heusinkveld, H. A. G., den Boer, A c, Evers, E. A.I.M. and Baumann, R. A (1999) Semi-permeable surface analytical reversed-phase column for the improved trace analysis of acidic pesticides in water with coupled-column reversed-phase liquid chromatography with UV detection determination of bromoxynil and bentazone in surface water, J. Chromato. A. 858, 45-54 https://doi.org/10.1016/S0021-9673(99)00799-2
  13. Choi, J. C, Lee, Y. J., Kim, S. H, Choi, S. Y., Choi, H J., Jeong, S. W, Park, H J. and Kim W S. (2005) Multiresidue analytical method of pesticides in rice by HPLC, J. Environ. Sci. 14 (4), 445-449 https://doi.org/10.5322/JES.2005.14.4.445
  14. Dollan, J. W. (2002) Mobile-phase buffers, Part II-buffers selection and capacity, LCGC NORTH AMERICA. 20 (12), 1114-1118
  15. Dollan, J. W. (2003) Mobile-phase buffers, Part III-preparation of buffers, LCGC NORTH AMERICA. 21(1), 28-32
  16. Tekel, J., Hudecova, T. and Pecnikova, K. (2001) Isolation and purification techniques for pesticide residue analyses in samples of plant or animal origin, Eur. Food Res. Technol. 213, 350-258
  17. Neue, U. D. (2002) HPLC troubleshooting guide. Waters. USA p. 20
  18. Horwitz, W. (2000) Official methods of analysis of AOAC international 17th edition. AOAC international, Gaithersburg, USA, p. 43-44
  19. Choi, D. M, Jeong, J. Y, Chang, M. I., Im, M. H, Park, K S. and Hong M. K (2005) Determination of tetracycline antibiotics in food, Anal. Sci & Tech. 18(3) : 250-256
  20. Pest management regulatory agency (2004) Regulatory note; REG2004-08, Canada, pp. 1-8
  21. Rural development administration & Korea crop protection association (2003) Text book for pesticide registration experiment, Korea, pp. 173-176
  22. Hall, G. L., Engebretson, J., Hengel, M. J. and Shibamoto, T. (2004) Analysis of methoxyfenozide residues in fruits, vegetables, and mint by liquid chromatography-tandem mass spectrometry(LCMS/MS), J. Agric. Food Chem. 52, 672-676 https://doi.org/10.1021/jf030591n
  23. Vink, M and van der Poll, J. M (1996) Gas chromatographic determination of acid herbicides in surface water samples with electron-capture detection and mass spectrometric confirmation, J. Chromato. A. 733, 361-366 https://doi.org/10.1016/0021-9673(95)00997-3
  24. Aguilar, c., Ferrer,I., Borrull, F., Marce, R. M. and Barcelo, D. (1999) Monitering of pesticides in river water based on samples previously stored in polymeric cartridges followed by on-line solidphase extraction-liquid chromatography-diode array detection and confirmation by atmospheric pressure chemical ionization mass spectrometry, Analytica Chimica Acta. 386, 237-248 https://doi.org/10.1016/S0003-2670(99)00033-1
  25. Smagghe, G., Carton, B., Wesemael, W., Ishaaya, I. and Tirry, L. (1999) Ecdysone agonists -Mechanism of action and application on spodoptera species, Pesti. Sci. 55, 386-389 https://doi.org/10.1002/(SICI)1096-9063(199903)55:3<386::AID-PS922>3.0.CO;2-5