Simultaneous analysis of glucocorticoids in bovine muscle and liver by LC-MS/MS

LC-MS/MS를 이용한 소의 근육과 간 중에 잔류하는 glucocorticoids 동시 분석

  • Received : 2010.02.16
  • Accepted : 2010.06.24
  • Published : 2010.08.25


A new method for the simultaneous determination of six glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, and flumethasone) in meats (bovine muscle, bovine liver) were established. Samples were effectively extracted using C18 cartridge with ethylacetate. Chromatographic separation was achieved using C18 column and negative electrospray ionization mass spectrometry was performed in the Multiple Reaction Monitoring mode for the effective quantitation and qualification of glucocorticoids. Acetonitrile and water (0.1% formic acid) were used as mobile phase and additive for effective electrospray ionization, and gave good chromatographic separation and mass spectrometric sensitivity. The limit of detection (LODs) and the limit of quantitation (LOQs) in spiked blank samples depending on types of matrix and pharmaceuticals were ranged from 0.2 to $1.0\;{\mu}g$/kg and 0.8 to $3.4\;{\mu}g$/kg, respectively. And the recoveries were between 89.5 to 119.6%. The established method showed good recoveries, accuracies, precisions and fast sample preparation and it will be applied to assay of glucocorticoids residues in meat.


Grant : 축산물중 항염증성 약물의 잔류분석법 개발 연구


  1. L. Istasse, V. De Haan, C. Van Eenaeme, B. Buts, P. Baldwin, M. Gielen, D. Demeyer and J.M. Bienfait, J. Anim. Physiol., Anim. Nutr. 62, 150(1984).
  2. M. L. J. Rijckaert and H. P. J. Vlemmix, The growth promoting effect of glucocorticoids, Department of Chemical Engineering, Eindhoven University of Technology, 1992.
  3. O. Van den hauwe, F. Dumoulin, J. P. Antignac, M. P. Bouche, C. Elliott and C. Van Peteghema, Anal. Chim. Acta., 473, 127-134(2002).
  4. M. J. O'Keeffe, S. Martin and L. Regan, Anal. Chim. Acta., 483, 341-350(2003).
  5. J.-P. Antignac, B. Le Bizec, F. Monteau, F. Poulain and F. Andre, J. Chromatogr. B, 757, 11-19(2001).
  6. V. Cirimele, P. Kintz, V. Dumestre, J. P. Goulle and B. Ludes, Forensic Sci. Int., 107, 381-388(2000).
  7. O. Van den Hauwe, M. Schneider, A. Sahin, C. H. Van Peteghem and H. Naegeli, J. Agric. Food Chem, 51, 326-330(2003).
  8. J.-P. Antignac, B. Le Bizec, F. Monteau and F. Andre. J. Mass Spectrom, 37, 69-75(2002).
  9. K. De Wasch, H. F. De Brabander, M. Van de Wiele, J. Vercammen and D. Courtheyn, J. Chromatogr. A, 926, 79-86(2001).
  10. R. Draisci, C. Marchiafava, L. Palleschi, P. Cammarata and S. Cavalli. J. Chromatogr. B, 753, 217-223(2001).
  11. O. Van den Hauwea, F. Dumoulina, C. Elliottb and C. Van Peteghema, J. Chromatogr. B, 817, 215-223(2005).
  12. J.-P. Antignac, B. Le Bizec, F. Monteau, F. Poulain and F. Andre, Rapid Commun. Mass Spectrom, 14, 33-39(2000).<33::AID-RCM829>3.0.CO;2-R
  13. Y. Xiong, K. P. Xiao and A. M. Rustum, J. Pharm. Biomed. Anal, 49, 646-654(2009).
  14. L. Cun, W. Yinliang, Y. Ting and Z. Yan, J. Chromatogr. A., 1217, 411-414(2010).
  15. A. Santos-Montes, AI Gasco-Lopez, and R. Izquierdo-Hornillos, Chromatographia, 39, 539(1994).
  16. J. P. Noben, B. Gielen, E. Royackers, M. Missotten, A. Jacobs and J. Raus, Rapid Commun. Mass Spectrom. 16, 1590-1594(2002).