Guidance for robustness/ruggedness tests in method validation

ICH harmonised tripartite guideline prepared within the third international conference on harmonisation of technical requirements for the registration of pharmaceuticals for human use (ICH), Text on Validation of Analytical Procedures, 1994, (http:/www.ifpma.org/ich1.html).

Youden, E.H. Steiner, Statistical manual of the association of official analytical chemists, The Association of Official Analytical Chemists ed., Arlington, 1975, pp. 33–36,70–71,82–83.

Van Leeuwen, 1991, RES, an expert system for the set-up and interpretation of a ruggedness test in HPLC method validation. Part 1: the ruggedness test in HPLC method validation, Chemometrics and Intelligent Laboratory systems, 10, 337, 10.1016/0169-7439(91)80098-B

Mulholland, 1988, Ruggedness testing in analytical chemistry, TRAC, 7, 383

Vander Heyden, 1998, Ruggedness testing of chromatographic methods: selection of factors and levels, Journal of Pharmaceutical and Biomedical Analysis, 18, 43, 10.1016/S0731-7085(98)00174-5

van de Vaart, 1992, Validation in pharmaceutical and biopharmaceutical analysis, Het Pharmaceutisch Weekblad, 127, 1229

ICH harmonised tripartite guideline prepared within the third international conference on harmonisation of technical requirements for the registration of pharmaceuticals for human use (ICH), Validation of Analytical Procedures: Methodology, 1996, 1–8 (http:/www.ifpma.org/ich1.html).

Caporal-Gautier, 1992, Guide de validation analytique, rapport d'une commission SFSTP, STP Pharma Pratiques, 2, 205

The United States Pharmacopeia, 23rd edition, National Formulary 18, United States Pharmacopeial Convention, Rockville, USA, 1995.

Drugs Directorate Guidelines, Acceptable Methods, Health Protection Branch-Health and Welfare Canada, 1992, 20–22.

International organisation for standardisation (ISO), accuracy (trueness and precision) of measurement methods and results — part 2: basic method for the determination of repeatability and reproducibility of a standard measurement method, International Standard ISO (1994E), 5725–5722, First edition.

International organisation for standardisation (ISO), accuracy (trueness and precision) of measurement methods and results — part 3: intermediate measures of the precision of a standard measurement method, International Standard ISO 1994(E), 5725–3, First edition.

Massart, 1997

Mulholland, 1987, Development and evaluation of an automated procedure for the ruggedness testing of chromatographic conditions in high-performance liquid chromatography, Journal of Chromatography, 395, 539, 10.1016/S0021-9673(01)94142-1

Fabre, 1985, Validation d'une méthode de dosage par chromatography en phase liquide haute performance, Analusis, 13, 117

Miller, 1993, 53

Dadgar, 1995, Application issues in bioanalytical method validation, sample analysis and data reporting, Journal of Pharmaceutical and Biomedical Analysis, 13, 89, 10.1016/0731-7085(94)00106-C

Fabre, 1996, Robustness testing in liquid chromatography and capillary electrophoresis, Journal of Pharmaceutical and Biomedical Analysis, 14, 1125, 10.1016/S0731-7085(96)01770-0

Doornbos, 1990, Experimental design, response surface methodology and multicriteria decision making in the development of drug dosage forms, 85

European pharmacopoeia 1997, 3rd edition, European Department for the Quality of Medicines within the Council of Europe, Strasbourg, 1996.

Eurachem, A focus for analytical chemistry in Europe, Quantifying Uncertainty in Analytical Measurement, First Edition 1995.

Morgan, 1991, 118

Box, 1978, 306

Vander Heyden, 1996, Review of the use of robustness and ruggedness in analytical chemistry, 79

Plackett, 1946, The design of optimum multifactorial experiments, Biometrika, 33, 305, 10.1093/biomet/33.4.305

Vander Heyden, 1995, Ruggedness tests on the HPLC assay of the United States Pharmacopeia XXII for tetracycline hydrochloride. A comparison of experimental designs and statistical interpretations, Analytica Chimica Acta, 312, 245, 10.1016/0003-2670(95)00221-K

Vander Heyden, 1995, Ruggedness tests on an HPLC assay: comparison of tests at two and three levels by using two-level Plackett–Burman designs, Analytica Chimica Acta, 316, 15, 10.1016/0003-2670(95)00349-5

Vander Heyden, 1998, A ruggedness test strategy for procedure related factors : experimental set-up and interpretation, Journal of Pharmaceutical and Biomedical Analysis, 17, 153, 10.1016/S0731-7085(97)00196-9

J.L. Goupy, Methods for Experimental Design, Principles and Applications for Physicists and Chemists, Elsevier, Amsterdam, 1993, pp. 159–177,421–427.

Vander Heyden, 1997, Influence of the sequence of experiments in a ruggedness test when drift occurs, Analytica Chimica Acta, 347, 369, 10.1016/S0003-2670(97)81182-8

Nijhuis, 1999, Strategy for ruggedness tests in chromatographic method validation, Analytica Chimica Acta, 391, 187, 10.1016/S0003-2670(99)00113-0

Jones, 1986, Optimization of experimental data, International Laboratory, 16, 32

Vander Heyden, 1996, Ruggedness tests on the HPLC assay of the United States Pharmacopeia XXIII for tetracycline hydrochloride: comparison of different columns in an interlaboratory approach, Journal of Pharmaceutical and Biomedical Analysis, 14, 1313, 10.1016/S0731-7085(96)01754-2

Vander Heyden, 1996, Ruggedness testing of a size exclusion chromatographic assay for low molecular mass polymers, Journal of Chromatography A, 756, 89, 10.1016/S0021-9673(96)00633-4

Y. Vander Heyden, G.M.R. Vandenbossche, C. De Muynck, K. Strobbe, P. Van Aerde, J.P. Remon, D.L. Massart, Influence of process parameters on the viscosity of Carbopol® 974P dispersions, Ph.D. thesis, personal communication.

Dong, 1993, On the identification of active contrasts in unreplicated fractional factorials, Statistica Sinica, 3, 209

Daniel, 1959, Use of half-normal plots in interpreting factorial two-level experiment, Technometrics, 1, 311, 10.2307/1266715

Zahn, 1975, An empirical study of the half-normal plot, Technometrics, 17, 201, 10.2307/1268352

Lenth, 1989, Quick and easy analysis of unreplicated factorials, Technometrics, 31, 469, 10.2307/1269997

Haaland, 1995, Inference for effect-saturated fractional factorials, Technometrics, 37, 82, 10.2307/1269155

Sidak, 1967, Rectangular confidence regions for the means of multivariate normal distributions, Journal of the American Statistical Association, 62, 626, 10.2307/2283989

Vander Heyden, 1999, Determination of system suitability limits with a robustness test, Journal of Chromatography A, 845, 145, 10.1016/S0021-9673(99)00328-3