Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS

LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석

  • 장미애 (경기대학교 자연과학대학 화학과) ;
  • 명승운 (경기대학교 자연과학대학 화학과)
  • Received : 2009.03.07
  • Accepted : 2009.07.01
  • Published : 2009.08.25

Abstract

A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

Keywords

Glucocorticoids;LC/MS/MS;egg

Acknowledgement

Grant : 축산물 중 항염증성 약물의 잔류분석법 개발 연구

Supported by : 국립수의과학검역원

References

  1. M. Michael, M. D. Wolfe, R. David, M. D. Lichtenstein and Gurkirpal Singh, M. D., N ENGL J Med., 340, 1888-1899(1999) https://doi.org/10.1056/NEJM199906173402407
  2. K. DeWasch, H. de Brabender, I. Vandereyt, P. Batjoens, K. Vanoosthuyze and C. Van Peteghem, Analyst, 119, 2557-2564(1994) https://doi.org/10.1039/an9941902557
  3. M. J. O'Keeffe, S. Martin and L. Regan, Anal. Chim. Acta, 483, 341-350(2003) https://doi.org/10.1016/S0003-2670(03)00059-X
  4. F. Guan, C. E. Uboh, L. R. Soma, Y. Luo, J. Rudy and T. Tobin, J. Chromatogr. B, 829, 56-68(2005) https://doi.org/10.1016/j.jchromb.2005.09.045
  5. X. Cui, B. Shao, R. Zhao, Y. Yang, J. Hu, and X. Tu, Rapid Commun. Mass Spectrom., 20, 2355-2364 (2006) https://doi.org/10.1002/rcm.2544
  6. M. L. J. Rijckaert and H. P. J. Vlemmix, The growth promoting effect of glucocorticoids, Department of Chemical Engineering, Eindhoven University of Technology, 1992
  7. 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, 150-158(1984) https://doi.org/10.1111/j.1439-0396.1989.tb00829.x
  8. M. McDonald, K. Granelli and P. sjoberg, Anal. Chim. Acta, 588, 20-25(2007) https://doi.org/10.1016/j.aca.2007.01.075
  9. O. Van den Hauwe, F. Dumoulin, C. Elliott and C. Van Peteghem, J. Chromatogr. B, 817, 215-223(2005) https://doi.org/10.1016/j.jchromb.2004.12.006
  10. A. Santos-Montes, A. I. Gasco-Lopez and R. Izquierdo- Hornillos, Chromatographia, 39, 539-542(1994) https://doi.org/10.1007/BF02268276
  11. K. De Wasch, H. De Brabander, D. Courtheyn and C. Van Peteghem, Analyst, 123, 2415-2422(1998) https://doi.org/10.1039/a804932g
  12. Y. R. Nii and P. O. Edlund, J. Pharm. Biomed. Anal., 37, 341-350(2005) https://doi.org/10.1016/j.jpba.2004.10.044
  13. D. Courtheyn, J. Vercammen, H. De Brabander, I. Vanderreyt, P. Batjoens, K. Vanoosthuyze and C. Van Peterghem, Analyst, 119, 2557-2564(1994) https://doi.org/10.1039/an9941902557
  14. O. H. Hidalgo, M. J. L'opez, E.A. Carazo, M. San Andr´es Larrea and B. A. Thea, Reuvers, J. Chromatogr. B, 788, 137-146(2003) https://doi.org/10.1016/S1570-0232(02)01039-5
  15. J.-P. Antignac, F. Monteau, J. Negriolli, F. Andre, B. LeBizec, Chromatographia, (1/2), 59(2004)
  16. G. N. W. Leung, E. W. Chung, E. M. Ho, W. H. Kwok, D. K. K. Leung, F. P. W. Tang, T. S. M. Wan and N. H. Yu, J. Chromatogr. B, 825, 47-56(2005) https://doi.org/10.1016/j.jchromb.2004.12.039