, Volume 57, Supplement 1, pp S303–S306 | Cite as

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

  • J. Vial
  • K. Le Mapihan
  • A. Jardy
Short Communications Column Liquid Chromatography


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.

Key Words

Column liquid chromatography Statistical data processing Method validation Limits of detection and quantification 


  1. [1]
    Huber, L.LC-GC Int. 1998,11, 96–105.Google Scholar
  2. [2]
    Green, J.M.Anal. Chem. 1996,68, 305A-309A.Google Scholar
  3. [3]
    Jenke, D.R.J. Liq. Chromatogr. Related Technol. 1996,19, 719–736.Google Scholar
  4. [4]
    Jenke, D.R.J. Liq. Chromatogr. Related Technol. 1996,19, 737–757.Google Scholar
  5. [5]
    Feinberg, M.La validation des méthodes d'analyse, Masson, Paris,1996.Google Scholar
  6. [6]
    Hartmann, C.; Smeyers-Verbeke, J.; Massart, D.L.; McDowall, R.D.J. Pharm. Biomed. Anal. 1998,17, 193–218.CrossRefGoogle Scholar
  7. [7]
    Thompson, M.; Ellison, S.L.R.; Wood, R.Pure Appl. Chem. 2002,74, 835–855.Google Scholar
  8. [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. [9]
    Currie, L.A.Pure Appl. Chem. 1995,67, 1699–1723.Google Scholar
  10. [10]
    ICH4.Validation of Analytical Procedures: Methodology, Q2B, ICH Steering Committee London,1996.Google Scholar
  11. [11]
    EurachemAccreditation for Chemical Laboratories, Eurachem Secretariat, Teddington, UK,1993.Google Scholar
  12. [12]
    Jardy, A.; Vial, J.; Ménier, I.Analusis 1997,25, 106–111.Google Scholar
  13. [13]
    Vial, J.; Ménier, I.; Jardy, A.; Anger, P.; Brun, A.; Burbaud, L.J. Chromatogr. B 1998,708, 131–143.Google Scholar
  14. [14]
    Vial, J.; Jardy, A.; Anger, P.; Brun, A.; Menet, J.M.J. Chromatogr. A 1998,815, 173–182.CrossRefGoogle Scholar
  15. [15]
    Vial, J.; Jardy, A.Chromatographia 2001,53, S141-S148.CrossRefGoogle Scholar
  16. [16]
    Vial, J.; Hennion, M.C.; Fernandez-Alba, A.; Aguera, A.J. Chromatogr. A 2001,937, 21–29.CrossRefGoogle Scholar
  17. [17]
    Vial, J.; Jardy, A.Anal. Chem. 1999,71, 2672–2677.CrossRefGoogle Scholar
  18. [18]
    Geiß, S.; Einax, J.W.Fresenius J. Anal. Chem. 2001,370, 673–678.CrossRefGoogle Scholar
  19. [19]
    Rosset, R.; Caude, M.; Jardy, A. In:Chromatographies en phases liquide et supercritique, Masson, Paris,1991, pp. 135–137.Google Scholar
  20. [20]
    Boyer, K.W.; Horwitz, W.; Albert, R.Anal. Chem. 1985,57, 454–459.CrossRefGoogle Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 2003

Authors and Affiliations

  • J. Vial
    • 1
  • K. Le Mapihan
    • 1
  • A. Jardy
    • 1
  1. 1.Laboratoire Environnement et Chimie AnalytiqueCNRS-UMR 7121, Ecole Supérieure de Physique et Chimie Industrielles de la Ville de ParisParisFrance

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