Chromatographia

, Volume 50, Issue 7–8, pp 399–406 | Cite as

Enhanced sensitivity by laser-induced fluorescence for the determination of calcitriol and other vitamin D3 metabolites in plasma

  • F. Ortiz Boyer
  • J. M. Fernández Romero
  • M. D. Luque de Castro
  • J. M. Quesada
Originals
Received:
Accepted:

Summary

A sensitive method for the determination of hydroxymetabolites of vitamin D3, parficularly calcitriol (1,25-(OH)2-D3), in human plasma is reported. The method is based on the use of laser-induced fluorescence detection as an alternative to conventional fluorimetry in an integrated cleanup/preconcentration, HPLC separation and post-column derivatization system. The derivatization step is based on a dehydration reaction which takes place in secosteroid structures at high temperature in a strong-acid medium. A LOD of 0.01 pg mL−1 (SNR=3) was obtained for each analyte with a linear dynamic range over 4 order of magnitude with excellent regression coefficients (≥0.9922) in all cases. The precision was studied at two concentration levels and the RSDs values (for n=5) were acceptable (between 2.6 and 4.7%). The method was also checked by applying it to human plasma spiked with the target analytes and excellent recoveries were obtained. This is the first time that these species have been determined at the sub-pg mL−1 level.

Key Words

Column liquid chromatography Continuous cleanup/preconcentration Post-column derivatization Vitamin D3 hydroxymetabolites Plasma samples 
This is a preview of subscription content, log in to check access.

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. [1]
    A. Brown, A. Dusso, E. Slatopolsky, Vitamin D. In D. W. Seldin, and G. Giebisch, Eds., The kidney: physiology and physiopathology, 2nd ed. New York; Raven Press, 1992.Google Scholar
  2. [2]
    N. H. Bell, P. H. Stern, E. Panther, T. K. Sinha, H. F. DeLuca, J. Clin. Invest.64, 218 (1979).CrossRefGoogle Scholar
  3. [3]
    E. Abe, C. Miyaura, H. Sakagami, M. Takeda, K Konno, T. Yamazaki, S. Yoshiki, T. Suda, Proc. Acad. Sci.78, 4990 (1981).CrossRefGoogle Scholar
  4. [4]
    T Suda, T. Shinki, N. Takahashi, Annu. Rev. Nutr.10, 195 (1990).CrossRefGoogle Scholar
  5. [5]
    Y. J. Zhou, A. W. Norman, M. Lübbert, E. D. Collimns, M. R. Uskokovic, H. P. Koeffler, Blood,74, 82 (1989),Google Scholar
  6. [6]
    G. Jones, D. H. J. Trafford, H. L. J. Makin, B. W Hollis, Vitamin D: Cholecalciferol, Ergocalciferol and hydroxylated metabolites. In A. P. Delleheer, w. E. Lambert and H. J. Nelis Eds., Modern Chromatographic Analysis of Vitamins; Chromatographic Science Series. Marcel Dekker. Vol.60, 1992Google Scholar
  7. [7]
    K Shimada, N. Kobayashi, Trends Anal, Chem.10 (3), 103 (1991)CrossRefGoogle Scholar
  8. [8]
    H. Koyama, J. M. Prahl, A. Uhland, M. Nanjo, M. Inaba, Y. Nishizawa, Y. Morii, Y. Nishii, H. F. DeLuca, Anal. Biochem,205 (2), 213 (1992)CrossRefGoogle Scholar
  9. [9]
    M. L. Traba, M. Babe, C. De-la-Piedra, A. Marin, Clin. Chim. Acta.29 (10), 1806 (1983)Google Scholar
  10. [10]
    F. H. Johannsen, Landwirtsch. Forsch.40 (1), 32 (1987)Google Scholar
  11. [11]
    M. A. Haughton, R. S. Mason, Clin. Chem.38 (9), 179 (1992).Google Scholar
  12. [12]
    E. Stary, A. M. C. Cruz, C. A. Donomai, J. L. Mondardinl. J. High Resolut. Chromatogr,12 (6), 421 (1989).CrossRefGoogle Scholar
  13. [13]
    E. C. Bligh, W. J. A. Dyer, Can. J. Biochem. Physiol.37, 911, (1959)Google Scholar
  14. [14]
    G. Jones, Clin. Chem.24, (2), 287 (1978).Google Scholar
  15. [15]
    M. Shimizu, Y. Gao, T. Aso, K. Nakatsu, S. Yamada, Anal. Biochem.204 (2), 258 (1992).CrossRefGoogle Scholar
  16. [16]
    R. D. Coldwell, D. J. H. Trafford, H. L. J. Makin, Clin Chem.31 (11), 1919 (1985).Google Scholar
  17. [17]
    R. D. Coldwell, D. J. H. Trafford, M. J. Varley, D. N. Kirk, H. L. J. Makin, Clin. Chim. Acta180 (2), 157 (1989).CrossRefGoogle Scholar
  18. [18]
    F. Ortiz-Boyer, J. M. Fernández-Romero, M. D. Luque de Castro J. M. Quesada, J. Chromatogr. B.693, 43 (1997).Google Scholar
  19. [19]
    R. D. Coldwell, D. J. H. Trafford, H. L. J. Makin, M. J. Varley, D. N. Kirk, J. Chromatogr. Biomed. Appl.39, 2891 (1985).Google Scholar
  20. [20]
    E. B. Mawer, J. T. Hann, J. Chromatogr. Biomed. Appl.59, 305 (1987).Google Scholar
  21. [21]
    R. L. G. Norris, M. J. Thomas, P. W. Craswell, Chromatogr. Biomed. Appl.54 (1), 53 (1986).CrossRefGoogle Scholar
  22. [22]
    S. Shimada, K. Mitamura, N. Kitama, Biomed. Chromatogr.9 (5), 229 (1995).CrossRefGoogle Scholar
  23. [23]
    A. Benmoussa, J. L. Lacout, P. R. Loiseau, M. Mikou, Chromatographia42 (3–4), 177 (1996).CrossRefGoogle Scholar
  24. [24]
    A. Benmoussa, G. Dlaurent, J. L. Lacout, P. R. Loiseau, M. Mikou, J. Chromatogr.731 (1–2), 153 (1996).CrossRefGoogle Scholar
  25. [25]
    J. M. Halket, I. Ganschow, B. P. Lisboa, J. Chromatogr.192 (2), 434 (1980).Google Scholar
  26. [26]
    S. Komuro, I. Nakatsuka, A. Yoshizake, K. Iba, Biol. Mass. Spectrom.23 (1), 33 (1994).CrossRefGoogle Scholar
  27. [27]
    R. D. Coldwell, D. J. L. Trafford, H. L. J. Makin, J. Mass. Spec.30, 348 (1995).CrossRefGoogle Scholar
  28. [28]
    P. P. Nair, C. Bucana, D. DeLeón, D. A. Turner, Anal. Chem.37, 631 (1965).CrossRefGoogle Scholar
  29. [29]
    I. Bjorkhem, I. Holmberg, T. Kristiansen, J. I. Pedersen, Clin. Chem.25 (4), 584 (1979).Google Scholar
  30. [30]
    P. M. K. Poon, I. T. Mak, C. P. Pang, Clin. Biochem.26 (6), 461 (1993).CrossRefGoogle Scholar
  31. [31]
    K. Shimada, K. Mitamura, M. Mukoujamaj, T. Okura, K. Sagaya, J. Chromatogr. Sci.32 (2), 82 (1995).Google Scholar
  32. [32]
    D. A. Seamark, D. J. H. Trafford, P. G. Hiscocks, H. L. J. Makin, J. Chromatogr.197 (2), 271 (1980).CrossRefGoogle Scholar
  33. [33]
    T. Iwata, M. Yamaguchi, H. Hanazono, Y. Imeto M. Nakamura, Y. Ohkura, Anal. Sci.6 (3), 361 (1990).Google Scholar
  34. [34]
    K. Shimada, I. Nakatani, K. Saito, K. Mitamura, Biol. Pharm. Bull.19 (4), 491 (1996).Google Scholar
  35. [35]
    P. H. Jordan, G. Read, T. Hargreaves, Analyst.116 (12), 1347 (1991).CrossRefGoogle Scholar
  36. [36]
    B. Yeung, P. Vouros, G. S. Reddy, J. Chromatogr.645 (1), 115 (1993).CrossRefGoogle Scholar
  37. [37]
    R. J. Vreeken, M. Honing, B. L. M. Van-Baar, R. T. Ghijsen, G. J. DeJong, U. A. T. Brinkman, Biol. Mass-Spectrom.22 (11), 621 (1993).CrossRefGoogle Scholar
  38. [38]
    D. J. H. Trafford, D. A. Seamark, H. Turnbull, H. L. J. Makin, J. Chromatogr. Biomed. Appl.15, 351 (1981).Google Scholar
  39. [39]
    M. Shimizu, Y. Iwasaki, H. Ishida, S. Yamada, J. Chromatogr.672, 63 (1995).Google Scholar
  40. [40]
    T. Iwata, M. Yamaguchi, H. Hanazono, Y. Imazato, M. Nakamura, Y. Ohkura, Anal. Sci.6 (3), 361 (1990).Google Scholar
  41. [41]
    M. Shimizu, S. Kamachi, Y. Nishii, S. Yamada, Anal. Biochem.194, 77 (1991).CrossRefGoogle Scholar
  42. [42]
    A. Sánchez-Pérez, M. J. Gallego-Matilla, J. S. Hernández-Méndez, Anal. Lett.26 (4), 721 (1993).Google Scholar
  43. [43]
    S. A. Solpe, S. M. Lunte, T. Kuwana, Anal. Sci.5, 23 (1989).Google Scholar
  44. [44]
    R. J. Van de Nesse, G. P. Hoornwegm, C. Gooijer, U. A. T. Brinkman, N. H. Velthorst, Anal. Chim. Acta.227, 173 (1989).CrossRefGoogle Scholar
  45. [45]
    S. V. Rahavendran, H. T. Karnes, Anal. Chem.69 (15), 3022 (1997).CrossRefGoogle Scholar
  46. [46]
    D. L. Stokes, M. J. Sepaniak, T. Vo-Dinh, Biomed. Chromatogr11 (4), 187 (1997).CrossRefGoogle Scholar
  47. [47]
    E. Gonzalez, J. J. Laserna, Quim. Anal.16, 3–15 (1997).Google Scholar
  48. [48]
    H. Li, H. Shang, C. Liu, Shenyang-Yaoxueyuan-Xuebao8 (4), 248 (1991).Google Scholar
  49. [49]
    F. Ortiz-Boyer, J. M. Fernández-Romero, M. D. Luque de Castro, J. M. Quesada, Clin. Chim. Acta.274, 139 (1998).CrossRefGoogle Scholar
  50. [50]
    F. Ortiz-Boyer, J. M. Fernández-Romero, M. D. Luque de Castro, J. M. Quesada, Talanta. (in press, 1998).Google Scholar
  51. [51]
    F. Ortiz-Boyer, J. M. Fernández-Romero, M. D. Luque de Castro, J. M. Quesada, J. Liq. Chrom. & Rel. Technol.21 (4), 503 (1998).Google Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 1999

Authors and Affiliations

  • F. Ortiz Boyer
    • 1
  • J. M. Fernández Romero
    • 1
  • M. D. Luque de Castro
    • 1
  • J. M. Quesada
    • 2
  1. 1.Analytical Chemistry Division, Faculty of SciencesUniversity of CórdobaSpain
  2. 2.Mineral Metabolism Unit, Hospital Reina SofiaUniversity of CórdobaCórdobaSpain

Personalised recommendations