Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Quantitative analysis of 3-MCPD in water using LC-MS

LC-MS를 이용한 수용액중의 3-MCPD 정량

  • Park, Gyo-Beom (Center for Chemical Analysis, Korea Research Institute of Chemical Technology) ;
  • Kim, Yong-Hwa (Toxicology Research Division, Korea Institute of Toxicology) ;
  • Kim, Jin-Sung (Toxicology Research Division, Korea Institute of Toxicology) ;
  • Jeong, Ja-Young (Department of Toxicologic Patholog, National Institute of Toxicological Research, Korea Food and Drug Administration) ;
  • Kim, Choong-Yong (Toxicology Research Division, Korea Institute of Toxicology) ;
  • Lee, Sueg-Geun (Center for Chemical Analysis, Korea Research Institute of Chemical Technology)
  • 박교범 (한국화학연구원 화학분석센터) ;
  • 김용화 (안전성평가연구소 독성연구부) ;
  • 김진성 (안전성평가연구소 독성연구부) ;
  • 정자영 (식품의약품안전청 국립독성연구원 독성병리과) ;
  • 김충용 (안전성평가연구소 독성연구부) ;
  • 이석근 (한국화학연구원 화학분석센터)
  • Received : 2007.04.02
  • Accepted : 2007.04.23
  • Published : 2007.06.28
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Abstract

The analysis method of 3-Monochloropropane-1,2-diol (3-MCPD) compound in water was developed using liquid chromatography with mass spectrometric detection. Aqueous solution was controlled in strong basic condition with sodium hydroxide, and then $25{\mu}L$ of benzoyl chloride was added to the solution for the derivatization of 3-MCPD. The derivative was extracted using pentane and analyzed by the selected ion monitoring (SIM) method of LC-MS. The results of analyses showed that the calibration curves was in the range of 1.0 to $100{\mu}g/mL$ with a good linearity (correlation coefficient of $r^2=0.992$) and limit of detection was below $0.01{\mu}g/mL$. The recoveries of this analysis method by LC-MS were 92.3-98.0 %.

수용액상에 존재하는 3-monochloropropane-1,2-diol (3-MCPD)의 LC-MS를 이용한 분석방법을 개발하였다. 수용액 시료에 수산화나트륨 용액을 첨가하여 강알칼리 상태를 유지시킨 후, 3-MCPD의 유도체화를 위하여 benzoyl chloride $25{\mu}L$을 넣어 직접 반응시켰다. 반응 후 유도체를 pentane으로 추출하여 LC-MS의 selected ion monitoring (SIM) 법으로 정량하였다. 분석결과 검량선은 $1.0-100{\mu}g/mL$ 농도범위에서 $r^2=0.992$의 상관관계 계수를 갖는 좋은 직선성을 나타내었으며, 검출한계는 $0.01{\mu}g/mL$ 이하였다. LC-MS에 의한 분석방법의 회수율은 92.3-98.0%이었다.

Keywords

References

  1. J. B. Conant and O. R. Quayle, Organic Syntheses Collective, I, 294-296 (1941)
  2. J. Velisek, J. Davidek, V. Kubelka, G. Janicek, Z. Svobodova, Z. Simicova, J. Agric. Food Chem. 28, 1142- 1144 (1980) https://doi.org/10.1021/jf60232a022
  3. P. D. Collier, D. D. O. Cromine, A. P. Davies, J. Am. Oil Chem. Soc. 68, 785-790 (1991) https://doi.org/10.1007/BF02662173
  4. C. A. Van Bergen, P. D. Collier, D. D. O. Cromine, R. A. Rucas, H. D. Preston, and D. J. Sissons, J. Chromatogr. 589, 109-119 (1992) https://doi.org/10.1016/0021-9673(92)80011-I
  5. K. T. Kirton, R. J. Ericsson, J. A. Ray, A. D. Forbes, J. Reprod. Fert. 21, 275 (1970)
  6. E. K. Weisburger, B. M. Uliand, J. Nam, J. J. Gart, J.H. Weisburger, J. Natl. Cancer 67, 75-88 (1981)
  7. L. Silhankova, F. Smid, M. Cerna, J. Davidek, J. Velisek, Mutat. Res. 103, 77-81 (1982) https://doi.org/10.1016/0165-7992(82)90090-2
  8. Position Paper on Chloropropanols for the Thirty-third Session of the Code Commit-tee on Food Additives and Contaminants, Joint FAO/WHO Food Standard program, 2001
  9. E. Kissa, J. Chromatogr. 605, 134-138 (1992) https://doi.org/10.1016/0021-9673(92)85038-U
  10. L. E. Rodman, R. D. Ross, J. Chromatogr. 369, 97-103 (1986) https://doi.org/10.1016/S0021-9673(00)90101-8
  11. W. J. Plantinga, W. G. van Toorn, G. H. D. van der Stegen, J. Chromatogr. 555, 311-314 (1991) https://doi.org/10.1016/S0021-9673(01)87196-X
  12. R. L. Pesselman, M. J. Feit, J. Chromatogr. 439, 448- 452 (1988) https://doi.org/10.1016/S0021-9673(01)83859-0
  13. W.-C. Chung, K.-Y. Hui, S.-C. Cheng, J. Chromatogr. A 952. 185-192 (2002) https://doi.org/10.1016/S0021-9673(02)00062-6
  14. C. A. van Bergen, P. D. Collier, D. D. O. Cromie, R. A. Lucas, H. D. Preston, D. J. Sissons, J. Chromatogr. 589, 104-109 (1992)
  15. C.G. Hamlet, P.G. Sutton, Rapid Commun. Mass Spectrum., 11, 1417(1997) https://doi.org/10.1002/(SICI)1097-0231(19970615)11:9<997::AID-RCM942>3.0.CO;2-2
  16. C.G. Hamlet, Food Addit. Contam. 15, 451(1998)
  17. D.C. Meierhans, J. Bruehlmann, J. Meili, C. Taeschler, J. Chromatogr. A 802, 325-333(1998) https://doi.org/10.1016/S0021-9673(97)01188-6
  18. M. Holcapek, H. Virelizire, J. Chamot-Rooke, P. Jandera, and C. Moulin, Anal. Chem, 71, 2288-2293 (1999) https://doi.org/10.1021/ac981087y
  19. 박교범, 이석근, 한국분석과학회지, 17(6), 527-531 (2004)