A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • Published : 1998.06.20

Abstract

A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Keywords

References

  1. J. Am. Chem. Soc. v.102 Fukuyama, T.;Frank, R. K.;Jewell, C. F.
  2. J. C. S. Chem. Commun. v.702 Goiding, B. T.;Smith, A. J.
  3. Synthesis v.548 Ender, D.;Hassel, T.;Pieter, R.;Renger, B.;Seebach, D.
  4. J. Org. Chem. v.49 Handling, K. E.;Burks, S. R.
  5. J. Org. Chem. v.53 Shono, T.;Matsumura, Y.;Onomura, O.;Sato, M.
  6. Tetrahedron Lett. v.36 Oppplzer, W.;Boch, C. G.
  7. J. Org. Chem. v.62 Moody, C. J.;Lightfoot, A. P.;Gallagher, P. T.
  8. Tetrahedron Lett. v.37 Fry, D. F.;Brown, M.;Mcdonald, J. C.;Dieter, R. K.
  9. Liebigs Ann. Chem. v.1295 Hereis, C.;Held, W. A.;Schwabenlander, F.;Kirfel, A.
  10. Tertrahedron v.52 Herdeis, C.;Held, W. A.;Kirfel, A.;Shwabenlander, F.
  11. Synthesis v.1405 Herdeis, C.;Schfter, T.
  12. Synthesis v.232 Herdeis, C
  13. J. Org. Chem. v.44 Celerier, J.-P.;Deliisy, E.;Lhoment, G.;Maitte, P.
  14. J. Am. Chem. Soc. v.117 Crich, D.;Beckwith, A. L. J.;Chem, C.;Yao, A.;davison, I. G.;Longmore, R. W.;de Parrodi, C. A.;Quintero-cortes, L.;Sandoval-ramirez, J.
  15. J. Org. Chem. v.61 Sharma, R.;Lubell, W. D.
  16. J. Korean Chem. Soc. v.39 Chung, K.-H.;An, S.-O.
  17. Tetrahedron : Asymmetry v.1 Morley, C.;Knight, D. W.;Share, A. C.