Skip to main content
SpringerLink
Log in

How experimental design can improve the validation process. Studies in pharmaceutical analysis

  • Special Issue Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

A critical discussion about the possibility of improving the method validation process by means of experimental design is presented. The reported multivariate strategies concern the evaluation of the performance parameters robustness and intermediate precision, and the optimisation of bias and repeatability. In particular, accuracy and precision improvement constitutes a special subset of experimental design in which the bias and the relative standard deviation of the assay are optimised. D-optimal design was used in order to plan experiments for this aim. The analytical methods considered were capillary electrophoresis, HPLC, adsorptive stripping voltammetry and differential pulse polarography. All methods were applied to real pharmaceutical analysis problems.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1a, b.
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

References

  1. Green JM (1996) Anal Chem 68:305A-309A

    CAS  Google Scholar 

  2. Thomposon M, Ellison S, Wood R (2002) Pure Appl Chem 74:835–855

    Google Scholar 

  3. ICH Harmonised tripartite guideline Q2B (1996) Validation of Analytical Procedures: Methodology. ICH, Geneva

    Google Scholar 

  4. The United States Pharmacopeia (2003) USP26, The United States Pharmacopeia, USA, pp. 2439–2443

  5. Swartz ME, Krull I (1997) Analytical method development and validation. Dekker, New York

  6. Lewis GA, Mathieu D, Phan-Tan-Luu R (1999) Pharmaceutical experimental design. Dekker, New York

  7. Montgomery DC (1997) Design and analysis of experiments. Wiley, New York

  8. Carlson R (1992) Design and optimization in organic synthesis. Elsevier, Amsterdam

  9. Pieniaszek HJ (1999) Short course on bioanalytical method development, validation and transfer. 10th International Symposium on Pharmaceutical and Biomedical Analysis, Washington, D.C., USA, May 9. Short course material

  10. Chen JG, Glancy K, Chen X, Alessandro M (2001) J Chromatogr A 917:63–73

    Article  CAS  PubMed  Google Scholar 

  11. Achilli M, Romele L (1997) J Chromatogr A 770:29–37

    Article  CAS  Google Scholar 

  12. Mathieu D, Phan-Tan-Luu R, Sergent M (1998) Méthodes modernes d'élaboration de matrices d'expériences optimales et qualité. LPRAI, Marseille

  13. Box G, Meyer D (1986) Technometrics 28:19–26

    Google Scholar 

  14. Polaskova P, Bocaz G, Li H, Havel J (2002) J Chromatogr A 979:59–67

    Article  CAS  PubMed  Google Scholar 

  15. Furlanetto S, Maestrelli F, Orlandini S, Pinzauti S, Mura P (2003) J Pharm Biomed Anal 32:159–165

    Article  CAS  PubMed  Google Scholar 

  16. Hund E, Vander Heyden Y, Haustein M, Massart DL, Smeyers-Verbeke J (2000) Anal Chim Acta 404:257–271

    Article  CAS  Google Scholar 

  17. Fabre H (1996) J Pharm Biomed Anal 14:1125–1132

    Article  CAS  PubMed  Google Scholar 

  18. Vander Heyden Y, Hartmann C, Massart DL, Michel L, Kiechle P, Erni F (1995) Anal Chim Acta 316:15–26

    Article  Google Scholar 

  19. Ragonese R, Mulholland M, Kalman J (2000) J Chromatogr A 870:45–51

    Article  CAS  PubMed  Google Scholar 

  20. Owens P, Wikstrom H, Nagard S, Karlsson L (2002) J Pharm Biomed Anal 27:587–598

    Article  CAS  PubMed  Google Scholar 

  21. Furlanetto S, Pinzauti S, La Porta E, Chiarugi A, Mura P, Orlandini S (1998) J Pharm Biomed Anal 17:1015–1028

    Article  CAS  PubMed  Google Scholar 

  22. Furlanetto S, Pinzauti S, Gratteri P, La Porta E, Calzeroni G (1997) J Pharm Biomed Anal 15:1585–1594

    Article  CAS  PubMed  Google Scholar 

  23. Furlanetto S, Orlandini S, La Porta E, Coran S, Pinzauti S (2002) J Pharm Biomed Anal 28:1161–1171

    Article  CAS  PubMed  Google Scholar 

  24. Gotti R, Furlanetto S, Andrisano V, Cavrini V, Pinzauti S (2000) J Chromatogr A 875:411–422

    Article  CAS  PubMed  Google Scholar 

  25. Ficarra R, Ficarra P, Tommasini S, Melardi S, Calabrò ML, Furlanetto S, Semreen M (2000) J Pharm Biomed Anal 23:169–174

    Article  CAS  PubMed  Google Scholar 

  26. Ficarra R, Calabrò M, Cutroneo P, Tommasini S, Melardi S, Semreen M, Furlanetto S, Ficarra P, Altavilla G (2002) J Pharm Biomed Anal 29:1097–1103

    Article  CAS  PubMed  Google Scholar 

  27. Furlanetto S, Orlandini S, Massolini G, Faucci M, La Porta E, Pinzauti S (2001) Analyst 126:1700–1706

    Article  CAS  PubMed  Google Scholar 

  28. Altria K, Bryant S, Hadgett T (1997) J Pharm Biomed Anal 15:1091–1101

    Article  CAS  PubMed  Google Scholar 

  29. Altria K (1996) J Chromatogr A 735:43–56

    Article  CAS  PubMed  Google Scholar 

  30. Altria K, Clark B, Filbey S, Kelly M, Rudd D (1995) Electrophoresis 16:2143–2148

    CAS  PubMed  Google Scholar 

  31. Altria K, Filbey S (1994) Chromatographia 39:306–310

    CAS  Google Scholar 

  32. Furlanetto S, Tognini C, Carpenedo R, La Porta E, Pinzauti S (1998) J Pharm Biomed Anal 18:67–73

    Article  CAS  PubMed  Google Scholar 

  33. Furlanetto S, Orlandini S, Aldini G, Gotti R, Dreassi E, Pinzauti S (2000) Anal Chim Acta 413:229–239

    Article  CAS  Google Scholar 

  34. Ye C, Liu J, Ren F, Okafo N (2000) J Pharm Biomed Anal 23:581–589

    Article  CAS  PubMed  Google Scholar 

  35. Mathieu D, Nony J, Phan-Tan-Luu R (2000) NEMROD-W. LPRAI, Marseille

  36. Kaale E, Van Schepdael A, Roets E, Hoogmartens J (2001) J Chromatogr A 924:451–458

    Article  CAS  PubMed  Google Scholar 

  37. Marchesini A, Williner M, Mantovani V, Robles J, Goicoechea H (2003) J Pharm Biomed Anal 31:39–46

    Article  CAS  PubMed  Google Scholar 

  38. Stalberg O, Sander K, Sanger-van de Griend C (2002) J Chromatogr A 977:265–275

    Article  CAS  PubMed  Google Scholar 

  39. Ficarra R, Cutroneo P, Aturki Z, Tommasini S, Calabrò M, Phan-Tan-Luu R, Fanali S, Ficarra P (2002) J Pharm Biomed Anal 29:989–997

    Article  CAS  PubMed  Google Scholar 

  40. Ragonese R, Macka M, Hughes J, Petocz P (2002) J Pharm Biomed Anal 27:995–1007

    Article  CAS  PubMed  Google Scholar 

  41. Saavedra L, Barbas C (2002) J Chromatogr B 766:235–242

    Article  CAS  Google Scholar 

  42. Akesolo U, Gonzalez L, Jimenez R, Alonso R (2003) J Chromatogr A 990:271–279

    Article  CAS  PubMed  Google Scholar 

  43. Furlanetto S, Gratteri P, Pinzauti S, Leardi R, Dreassi E, Santoni G (1995) J Pharm Biomed Anal 13:431–438

    Article  CAS  PubMed  Google Scholar 

  44. European Community (2002) Official Journal of the European Communities L 221, 17.8.2002, p. 8–36

  45. Meier P, Zünd R (1993) Statistical methods in analytical chemistry. Wiley, New York

  46. Frank IE, Todeschini R (1994) The data analysis handbook. Elsevier, Amsterdam

  47. de Aguiar PF, Bourguignon B, Khots MS, Massart DL, Phan-Tan-Luu R (1995) Chemom Intell Lab Sys 30:199–210

    Article  Google Scholar 

  48. Mathieu D, Phan-Tan-Luu R, Sergent M (1996) Criblage et étude des facteurs. LPRAI, Marseille

  49. Lenth RV (1989) Technometrics 3:469–473

    Google Scholar 

  50. Vander Heyden Y, Massart DL (1996) Review of the use of robustness and ruggedness in analytical chemistry. In: Smilde A, de Boer J, Hendricks M (eds) Robustness of analytical methods and pharmaceutical technological products. Elsevier, Amsterdam pp 79–147

  51. Vander Heyden Y, Nijhuis A, Smeyers-Verbeke J, Vandeginste BGM, Massart DL (2001) J Pharm Biomed Anal 24:723-753

    Article  PubMed  Google Scholar 

  52. van Leeuwen JA, Buydens LMC, Vandeginste BGM, Kateman G, Schoenmakers PJ, Mulholland M (1991) Chemom Intell Lab Sys 10:337–347

    Article  Google Scholar 

  53. Plackett RL, Burman JP (1946) Biometrika 33:305

    Google Scholar 

  54. Fanali S, Furlanetto S, Aturki Z, Pinzauti S (1998) Chromatographia 48:395–401

    CAS  Google Scholar 

Download references

Acknowledgements

This work was supported in part by a grant from MIUR.

Author information

Authors and Affiliations

  1. Department of Pharmaceutical Sciences, University of Florence, Via G. Capponi 9, 50121, Florence, Italy

    S. Furlanetto, S. Orlandini, P. Mura & S. Pinzauti

  2. Laboratory of Experimental Research Methodologies, University of Aix-Marseille III, Av. Escadrille Normandie-Niemen, 13397 Marseille Cedex 20, Marseille , France

    M. Sergent

Authors
  1. S. Furlanetto
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. S. Orlandini
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. P. Mura
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. M. Sergent
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. S. Pinzauti
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to S. Furlanetto.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Furlanetto, S., Orlandini, S., Mura, P. et al. How experimental design can improve the validation process. Studies in pharmaceutical analysis. Anal Bioanal Chem 377, 937–944 (2003). https://doi.org/10.1007/s00216-003-2189-2

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-003-2189-2

Keywords

Search

Navigation