Skip to main content
Log in

What is the best means of estimating the detection and quantification limits of a chromatographic method?

  • Short Communications
  • Column Liquid Chromatography
  • Published:
Chromatographia Aims and scope Submit manuscript

Summary

Limits of detection and quantification (LOD andLOQ) are two fundamental elements of method validation. Although strict statistical definitions exist, a variety of procedures based on different means of estimating the standard deviation of the blank can be used to evaluate these limits. An experiment set up to investigate their compatibility for an LC-UV method has proved they are not equivalent. We therefore recommend an alternative and absolute methodology:LOQ is obtained from the targetRSD chosen for the assay andLOD is taken as three tenths of theLOQ. To demonstrate the method is not restricted to LC-UV it has been applied to LC-MS and GC-FID.

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

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

References

  1. Huber, L.LC-GC Int. 1998,11, 96–105.

    Google Scholar 

  2. Green, J.M.Anal. Chem. 1996,68, 305A-309A.

    CAS  Google Scholar 

  3. Jenke, D.R.J. Liq. Chromatogr. Related Technol. 1996,19, 719–736.

    CAS  Google Scholar 

  4. Jenke, D.R.J. Liq. Chromatogr. Related Technol. 1996,19, 737–757.

    CAS  Google Scholar 

  5. Feinberg, M.La validation des méthodes d'analyse, Masson, Paris,1996.

    Google Scholar 

  6. Hartmann, C.; Smeyers-Verbeke, J.; Massart, D.L.; McDowall, R.D.J. Pharm. Biomed. Anal. 1998,17, 193–218.

    Article  CAS  Google Scholar 

  7. Thompson, M.; Ellison, S.L.R.; Wood, R.Pure Appl. Chem. 2002,74, 835–855.

    CAS  Google Scholar 

  8. Massart, D.L.; Vandeginste, B.G.M.; Buydens, L.M.C.; De Jong, S.; Lewi, P.J.; Smeyers-Verbeke, J. InHandbook of Chemometrics and Qualimetrics, Part A, Elsevier, Amsterdam,1997, pp. 422–435.

    Google Scholar 

  9. Currie, L.A.Pure Appl. Chem. 1995,67, 1699–1723.

    CAS  Google Scholar 

  10. ICH4.Validation of Analytical Procedures: Methodology, Q2B, ICH Steering Committee London,1996.

  11. EurachemAccreditation for Chemical Laboratories, Eurachem Secretariat, Teddington, UK,1993.

    Google Scholar 

  12. Jardy, A.; Vial, J.; Ménier, I.Analusis 1997,25, 106–111.

    CAS  Google Scholar 

  13. Vial, J.; Ménier, I.; Jardy, A.; Anger, P.; Brun, A.; Burbaud, L.J. Chromatogr. B 1998,708, 131–143.

    CAS  Google Scholar 

  14. Vial, J.; Jardy, A.; Anger, P.; Brun, A.; Menet, J.M.J. Chromatogr. A 1998,815, 173–182.

    Article  CAS  Google Scholar 

  15. Vial, J.; Jardy, A.Chromatographia 2001,53, S141-S148.

    Article  CAS  Google Scholar 

  16. Vial, J.; Hennion, M.C.; Fernandez-Alba, A.; Aguera, A.J. Chromatogr. A 2001,937, 21–29.

    Article  CAS  Google Scholar 

  17. Vial, J.; Jardy, A.Anal. Chem. 1999,71, 2672–2677.

    Article  CAS  Google Scholar 

  18. Geiß, S.; Einax, J.W.Fresenius J. Anal. Chem. 2001,370, 673–678.

    Article  Google Scholar 

  19. Rosset, R.; Caude, M.; Jardy, A. In:Chromatographies en phases liquide et supercritique, Masson, Paris,1991, pp. 135–137.

    Google Scholar 

  20. Boyer, K.W.; Horwitz, W.; Albert, R.Anal. Chem. 1985,57, 454–459.

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

Vial, J., Le Mapihan, K. & Jardy, A. What is the best means of estimating the detection and quantification limits of a chromatographic method?. Chromatographia 57 (Suppl 1), S303–S306 (2003). https://doi.org/10.1007/BF02492120

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Issue Date:

  • DOI: https://doi.org/10.1007/BF02492120

Key Words

Navigation