Movatterモバイル変換

[0]ホーム
URL:

Skip to main content

Advertisement

Springer Nature Link
Log in

Automated coupling of capillary-HPLC to matrix-assisted laser desorption/ionization mass spectrometry for the analysis of small molecules utilizing a reactive matrix

  • Paper in Forefront
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract.

This study describes the application of a novel, reactive matrix for the mass spectral analysis of steroids by capillary-high performance liquid chromatography (capillary-HPLC) coupled to matrix-assisted laser desorption/ionization (MALDI). The mass spectral analysis of steroids was accomplished after fully automated peak deposition of chromatographic peaks onto MALDI targets. The seven corticosteroids used as test compounds were: triamcinolone, prednisone, cortisone, fludrocortisone, dexamethasone, deoxycorticosterone, and budesonide. They were separated using a PepMap C18 (3 μm particle size, 100 Å pore width) column at five different concentration levels of 25, 15, 7.5, 2.5 and 1 ng/μL, and the peaks were detected at a wavelength of 237 nm. The column effluent was mixed with 2,4-dinitrophenylhydrazine (DNPH) directly following the UV detector. The chromatographic peaks were then deposited onto the MALDI target with a robotic micro-fraction collector triggered by the UV detector signals. A special hydrophobic surface coating allowed the deposition of up to 4 μL (up to 90 % of the chromatographic peak volume) onto one sample spot. The compounds were then identified by MALDI mass spectrometry. Depending on the nature of the analyte, radical cations ([M]+.) and sodium adduct ions ([M+Na]+) of the steroids as well as protonated steroid-dinitrophenylhydrazone derivatives ([MD+H]+) were detected in positive ion mode. The detection limits were between 0.5 and 15 ng injected with capillary-HPLC-MALDI-TOF-MS and between 0.3 and 3 ng on target with MALDI-TOF when deposited manually.

This is a preview of subscription content,log in via an institution to check access.

Access this article

Log in via an institution

Subscribe and save

Springer+ Basic
¥17,985 /Month
  • Get 10 units per month
  • Download Article/Chapter or eBook
  • 1 Unit = 1 Article or 1 Chapter
  • Cancel anytime
Subscribe now

Buy Now

Price includes VAT (Japan)

Instant access to the full article PDF.

Fig. 1.
Fig. 2A, B
Fig. 3A, B
Fig. 4A, B

Similar content being viewed by others

Explore related subjects

Discover the latest articles and news from researchers in related subjects, suggested using machine learning.

References

  1. Karas M., Hillenkamp F. (1988) Anal Chem 60:2299–2301

    CAS PubMed  Google Scholar 

  2. Tanaka K., Waki H., Ido Y., Akita S., Yoshida Y., Yoshida T. (1988) Rapid Commun Mass Spectrom 2:151–153

    CAS  Google Scholar 

  3. Zenobi R., Knochenmuss R. (1998) Mass Spec Rev 17:337–366

    Article CAS  Google Scholar 

  4. Busch K. L. (1999) Spectroscopy 14:14–16

    Google Scholar 

  5. Cohen S. L., Chait B. T. (1996) Anal Chem 68:31–37

    Article CAS PubMed  Google Scholar 

  6. Önnerfjord P., Ekstrom S., Bergquist J., Nilsson J., Laurell T., Marko-Varga G. (1999) Rapid Commun Mass Spec 13:315–322

    Article  Google Scholar 

  7. Doroshenko V. M., Laiko V. V., Taranenko N. I., Berkout V. D., Lee H. S. (2002) Int J Mass Spec 221:39–58

    Article CAS  Google Scholar 

  8. Moyer S. C., Cotter R. J. (2002) Anal Chem 17:469A–476A

    Google Scholar 

  9. LeRiche, T., Osterodt J., Volmer D. A. (2001) Rapid Commun Mass Spectrom 15:608–614

    CAS PubMed  Google Scholar 

  10. Andalo C., Bocchini P., Pozzi R., Galletti G. C. (2001) Rapid Commun Mass Spectrom 15:

  11. Biot C., Caron S., Maciejewski L. A., Brocard J. S. (1998) J Labelled Compd Radiopharm 41:911–918

    Article CAS  Google Scholar 

  12. Cohen L. H., Gusev A. I. (2002) Anal Bioanal Chem 373:571–586

    Article CAS PubMed  Google Scholar 

  13. Nicola A. J., Gusev A. I., Proctor A., Jackson E. K., Hercules D. M. (1995) Rapid Commun Mass Spectrom 9:1164–1171

    CAS PubMed  Google Scholar 

  14. Zhu Y. F., Lee K. L., Tang K., Allman S. L., Taranenko N. I., Chen C. H. (1995) Rapid Commun Mass Spectrom 9:1315–1320

    CAS PubMed  Google Scholar 

  15. Harvey D. J. (1999) Mass Spectrom Rev 18:349–451

    CAS  Google Scholar 

  16. Harvey D. J. (1993) Rapid Commun Mass Spectrom 7:614–619

    CAS PubMed  Google Scholar 

  17. Keil O., LeRiche T., Deppe H., Volmer D. A. (2002) Rapid Commun Mass Spectrom 16:814–820

    Article CAS PubMed  Google Scholar 

  18. Vogel M., Büldt A., Karst U. (2000) Fresenius J Anal Chem 366:781–791

    CAS PubMed  Google Scholar 

  19. Camel V., Caude M. (1995) J Chromatogr A 710:3–19

    CAS  Google Scholar 

  20. Grosjean D., Grosjean E. (1995) Int J Environ Anal Chem 61:343–360

    CAS  Google Scholar 

  21. Tholey A., Wittmann C., Kang M.-J., Bungert D., Hollemeyer K., Heinzle E. (2002) J Mass Spectrom 37:963–973

    Article CAS PubMed  Google Scholar 

  22. Zhang L.-K., Gross M. L. (2002) J Am Soc Mass Spectrom 13:1418–1426

    Article CAS PubMed  Google Scholar 

  23. Volmer D. A., Hui J. P. M. (1997) Rapid Commun Mass Spectrom 11:1926–1934

    CAS PubMed  Google Scholar 

  24. Carey F. A. Sundberg R. J. (1990) Advanced Organic Chemistry. Plenum Press, New York 3:802

  25. Allwood D. A., Dreyfus R. W., Perera I. K., Dyer P. E. (1996) Rapid Commun Mass Spectrom 10:1575–1578

    Article CAS  Google Scholar 

  26. Allwood D. A., Dreyfus R. W., Perera I. K., Dyer P. E. (1997) Appl Surf Sci 109/110:154–157

    Google Scholar 

  27. Owen S. J., Brombacher S., Volmer D. A. (2003) In preparation

  28. Kölliker S., Oehme M. (1998) Anal Chem 70:1979–1985

    Article  Google Scholar 

  29. Brombacher S., Oehme M., Beukes J. A. (2001) J Environ Monit 3:311–316

    CAS PubMed  Google Scholar 

  30. Gobom J., Mueller M., Egelhofer V., Theiss D., Lehrach H., Nordhoff E. (2002) Anal Chem 74:3915–3923

    Article CAS PubMed  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Institute for Marine Biosciences, National Research Council, 1411 Oxford Street, Halifax, Nova Scotia, B3H 3Z1, Canada

    Stephan Brombacher, Stacey J. Owen & Dietrich A. Volmer

Authors
  1. Stephan Brombacher

    You can also search for this author inPubMed Google Scholar

  2. Stacey J. Owen

    You can also search for this author inPubMed Google Scholar

  3. Dietrich A. Volmer

    You can also search for this author inPubMed Google Scholar

Corresponding author

Correspondence toDietrich A. Volmer.

Rights and permissions

About this article

Cite this article

Brombacher, S., Owen, S.J. & Volmer, D.A. Automated coupling of capillary-HPLC to matrix-assisted laser desorption/ionization mass spectrometry for the analysis of small molecules utilizing a reactive matrix.Anal Bioanal Chem376, 773–779 (2003). https://doi.org/10.1007/s00216-003-2024-9

Download citation

Keywords

Access this article

Subscribe and save

Springer+ Basic
¥17,985 /Month
  • Get 10 units per month
  • Download Article/Chapter or eBook
  • 1 Unit = 1 Article or 1 Chapter
  • Cancel anytime
Subscribe now

Buy Now

Price includes VAT (Japan)

Instant access to the full article PDF.

Advertisement

[8]ページ先頭
©2009-2025 Movatter.jp