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Method development and validation for optimised separation of salicylic, acetyl salicylic and ascorbic acid in pharmaceutical formulations by hydrophilic interaction chromatography and response surface methodology

Citation

Hatambeygi, N and Abedi, G and Talebi, M, Method development and validation for optimised separation of salicylic, acetyl salicylic and ascorbic acid in pharmaceutical formulations by hydrophilic interaction chromatography and response surface methodology, Journal of Chromatography A, 1218, (35) pp. 5995-6003. ISSN 0021-9673 (2011) [Refereed Article]

Copyright Statement

Copyright 2011 Elsevier B.V.

DOI: doi:10.1016/j.chroma.2011.06.009

Abstract

This paper introduces a design of experiments (DOE) approach for method optimisation in hydrophilic interaction chromatography (HILIC). An optimisation strategy for the separation of acetylsalicylic acid, its major impurity salicylic acid and ascorbic acid in pharmaceutical formulations by HILIC is presented, with the aid of response surface methodology (RSM) and Derringer’s desirability function. A Box-Behnken experimental design was used to build the mathematical models and then to choose the significant parameters for the optimisation by simultaneously taking both resolution and retention time as the responses. The refined model had a satisfactory coefficient (R2 > 0.92, n = 27). The four independent variables studied simultaneously were: acetonitrile content of the mobile phase, pH and concentration of buffer and column temperature each at three levels. Of these, the concentration of buffer and its crossproduct with pH had a significant, positive influence on all studied responses. For the test compounds, the best separation conditions were: acetonitrile/22 mM ammonium acetate, pH 4.4 (82:18, v/v) as the mobile phase and column temperature of 28 °C. The methodology also captured the interaction between variables which enabled exploration of the retention mechanism involved. It would be inferred that the retention is governed by a compromise between hydrophilic partitioning and ionic interaction. The optimised method was further validated according to the ICH guidelines with respect to linearity and range, precision, accuracy, specificity and sensitivity. The robustness of the method was also determined and confirmed by overlying counter plots of responses which were derived from the experimental design utilised for method optimisation.

Item Details

Item Type:Refereed Article
Keywords:hydrophilic interaction chromatography (HILIC), response surface methodology (RSM), Derringer's desirability function, Box-Behnken, optimisation, ICH guidelines
Research Division:Chemical Sciences
Research Group:Analytical Chemistry
Research Field:Separation Science
Objective Division:Expanding Knowledge
Objective Group:Expanding Knowledge
Objective Field:Expanding Knowledge in the Chemical Sciences
Author:Talebi, M (Dr Mohammad Talebi)
ID Code:78356
Year Published:2011
Web of Science® Times Cited:41
Deposited By:Austn Centre for Research in Separation Science
Deposited On:2012-06-22
Last Modified:2012-09-10
Downloads:0

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