Robustness and System Suitability - Analytical Validation - page 99

optimizing the method, indicating whether or not further development or optimiza-
tion is necessary.
When performed early in the validation process, a robustness study can provide
feedback on what parameters can affect the method if not properly controlled, and
help in setting system suitability parameters for when the method is implemented.
reFerences
1. The United States Pharmacopeia 34/National Formulary 29 , The United States
Pharmacopeial Convention, Inc., Rockville, MD, 2011, Chapter <1225>.
2. International Conference on Harmonization, Harmonized tripartite guideline, validation of
analytical procedures, text and methodology, Q2 (R1), November 2005. See www.ICH.org.
3. ISO/IEC 17025, General Requirements for the Competence of Testing and Calibration
Laboratories, (2005), http://www.iso.org/iso/iso_catalogue/catalogue_tc/catalogue_
detail.htm?csnumber=39883.
4. Box, G. E. P., Hunter, W. G., and Hunter, J. S., Statistics for Experimenters , John Wiley
& Sons, New York, 1978.
5. Miller, J. C. and Miller, J. N., Statistics for Analytical Chemistry , Ellis Horwood
Publishers, Chichester, UK, 1986.
6. NIST/SEMATECH e-Handbook of Statistical Methods , http://www.itl.nist.gov/div898/
handbook.
7. Meier, P. C. and Zund, R. E., Statistical Methods in Analytical Chemistry , John Wiley &
Sons, New York, 1993.
8. Plackett, R. L. and Burman, J. P., The Design of Optimum Multifactorial Experiments.
Biometrika , 33, 305, 1946.
9. Ragonese, R., Mulholland, M., and Kalman, J., J. Chromatogr. A , 870, 45, 2000.
10. Nguyet, A. N. M., Tallieu, L., Plaizier-Vercammen, J., Massart, D. L., and Heyden,
Y. V., Validation of an HPLC method on short columns to assay ketoconazole and form-
aldehyde in shampoo. Correct reference to read volume 32. J. Pharm. Biomed. Analysis ,
21, 1-19, 2003.
11. Sun, S-W. and Su, H-T., Validated HPLC method for determination of sennosides A and
B in senna tablets. J. Pharm. Biomed. Analysis , 29, 881-894, 2002.
12. Heyden, Y. V., Nijhuis, A., Smeyers-Verbek, B. G. M., and Massart, D. L., Guidance
for robustness/ruggedness tests in method validation. J. Pharm. Biomed. Analysis , 24,
723-753, 2001.
13. Heyden, Y. V., Questier, F., and Massart, D. L., Ruggedness testing of chromatographic
methods: selection of factors and levels. J. Pharm. Biomed. Analysis , 18, 43-56, 1998.
14. Questier, F., Heyden, Y. V., and Massart, D. L., RTS, a computer program for the experi-
mental set-up and interpretation of ruggedness tests. J. Pharm. Biomed. Analysis , 18,
287-303, 1998.
15. Lukalay, P. and Morgado, J., Automation of the chromatographic analytical method vali-
dation process. LCGC , 24(2), 150-156, February 2006.
16. Empower 2 Software: Method Validation Manager, April 2007, 720001488EN LB-PC,
Waters Corporation, Milford, MA.
17. The United States Pharmacopeia 34/ National Formulary 29 , The United States
Pharmacopeial Convention, Inc., Rockville, MD, 2011, Chapter <621>.
18. Center for Drug Evaluation and Research (CDER), Reviewer Guidance: Validation of
Chromatographic Methods, US Government Printing Office, 1994, 615-023-1302/02757.
19. Furman, W. B., Dorsey, J. G., and Snyder, L. R., System Suitability Tests in Regulatory
Liquid and Gas Chromatographic Methods: Adjustments Versus Modifications. Pharm.
Technol . 22(6), 58-64, 1998.