A TEST OF ROBUSTNESS IN IIR-RP-HPLC SEPARATION OF NINE PRIORITY POLLUTANT PHENOLS

This study presents an example of method validation, applied to an IIR-RP-HPLC method, developed for the separation of nine PPPs (Priority Pollutant Phenols). The parameters of both primary validation (accuracy, precision, response linearity, detection. and quantitation limits,) and of secondary validation (method ruggedness) are evaluated. The glossary used in literature for ruggedness and robustness is discussed. The robustness test is carried out with respect to five chromatographic conditions, both depending on analyst accuracy (concentration of the ion-interaction reagent, concentration of the organic modifier, and pH of the mobile phase) and on instrumentation (column temperature and flow-rate). The effect of the experimental factors is studied by a fractional factorial design and mathematical models are built, that correlate the chromatographic retention to the experimental factors and to their interactions. The cross-validated models can usefully be employed to evaluate for each studied variable the region of acceptable ruggedness for any given confidence level.

[1]  Awwa,et al.  Standard Methods for the examination of water and wastewater , 1999 .

[2]  H. Fabre,et al.  Robustness testing in liquid chromatography and capillary electrophoresis. , 1996, Journal of pharmaceutical and biomedical analysis.

[3]  T. S. West.  Analytical Chemistry , 1969, Nature.

[4]  M. C. Gennaro,et al.  Neural network and experimental design to investigate the effect of five factors in ion-interaction high-performance liquid chromatography , 1998 .

[5]  M. Mulholland,et al.  Development and evaluation of an automated procedure for the ruggedness testing of chromatographic conditions in high-performance liquid chromatography , 1987 .

[6]  Dennis R. Jenke.  Chromatographic Method Validation: A Review of Current Practices and Procedures. I. General Concepts and Guidelines , 1996 .

[7]  Johanna Smeyers-Verbeke,et al.  Handbook of Chemometrics and Qualimetrics: Part A , 1997 .

[8]  D. Massart,et al.  Detection of bias in method comparison by regression analysis , 1997 .

[9]  M. Gennaro,et al.  Experimental design and partial least squares for optimization of reversed-phase ion-interaction liquid chromatographic separation of nitrite, nitrate, and phenylenediamine isomers , 1992 .

[10]  Dennis Jenke,et al.  Chromatographic Method Validation: A Review of Current Practices and Procedures. III. Ruggedness, Re-Validation and System Suitability , 1996 .

[11]  Gregory A. Mack,et al.  Chemometrics: A Textbook , 1990 .

[12]  T. Whitehead,et al.  A rapid and simple chemiluminescent assay for water quality monitoring , 1994 .

[13]  Gerrit Kateman,et al.  Expert system for precision testing in validation of liquid chromatographic methods , 1990 .

[14]  G. Kateman,et al.  An expert system for the choice of factors for a ruggedness test in liquid chromatography , 1990 .

[15]  D L Massart,et al.  An analysis of the Washington Conference Report on bioanalytical method validation. , 1994, Journal of pharmaceutical and biomedical analysis.

[16]  M. Mulholland,et al.  Investigation of the limitations of saturated fractional factorial experimental designs, with confounding effects for an HPLC ruggedness test , 1988 .

[17]  K. Altria,et al.  The application of experimental design to the robustness testing of a method for the determination of drug-related impurities by capillary electrophoresis , 1994 .

[18]  J. Crabbe.  Robustness of Analytical Methods and Pharmaceutical Technological Products , 1997 .

[19]  Desire L. Massart,et al.  Ruggedness testing of a size-exclusion chromatographic assay for low-molecular-mass polymers , 1996 .

[20]  Age K. Smilde,et al.  Robustness of analytical chemical methods and pharmaceutical technological products. , 1996 .

[21]  Luis Cuadros Rodríguez,et al.  A new approach to a complete robustness test of experimental nominal conditions of chemical testing procedures for internal analytical quality assessment , 1998 .

[22]  M. Mulholland,et al.  Ruggedness testing in analytical chemistry , 1988 .

[23]  D. Jenke.  Chromatographic Method Validation: A Review of Current Practices and Procedures. II. Guidelines for Primary Validation Parameters. , 1996 .

[24]  Lutgarde M. C. Buydens,et al.  RES, AN EXPERT SYSTEM FOR THE SET-UP AND INTERPRETATION OF A RUGGEDNESS TEST IN HPLC METHOD VALIDATION .1. THE RUGGEDNESS TEST IN HPLC METHOD VALIDATION , 1991 .

[25]  W. J Youden,et al.  Statistical Manual of the Association of Official Analytical Chemists , 1984 .

[26]  M. Gennaro,et al.  An ion-interaction RP-HPLC method for the determination of the eleven EPA priority pollutant phenols , 1997 .

[27]  J. Wahlich,et al.  A practical approach to method validation in pharmaceutical analysis. , 1990, Journal of pharmaceutical and biomedical analysis.

[28]  M. Gennaro,et al.  Investigation by experimental design and regression models of the effect of five experimental factors on ion-interaction high-performance liquid chromatographic retention , 1996 .

[29]  D. Wiggins.  System Suitability in an Optimized HPLC System , 1991 .

[30]  A. E. Greenberg,et al.  Standard Methods for the Examination of Water and Wastewater seventh edition , 2013 .

[31]  M. Gennaro,et al.  Chemometric Optimization of Azide Sensitivity in Reversed-Phase Ion-Interaction HPLC , 1994 .

[32]  D. L. Massart,et al.  Ruggedness tests for a high-performance liquid Chromatographic assay: Comparison of an evaluation at two and three levels by using two-level Plackett-Burman designs , 1995 .

[33]  Desire L. Massart,et al.  Influence of the sequence of experiments in a ruggedness test when drift occurs , 1997 .