Optimising reversed-phase liquid chromatographic separation of an acidic mixture on a monolithic stationary phase with the aid of response surface methodology and experimental design

• Published in: Journal of Chromatography A Vol. 1105; no. 1; pp. 199 - 207
• Main Authors: Wang, Y., Harrison, M., Clark, B.J.
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Amsterdam Elsevier B.V 10-02-2006; Elsevier
• Subjects: Acids - isolation & purification; Analysis; Analytical chemistry; Biological and medical sciences; Carboxylic Acids - isolation & purification; Central composite design; Chemistry; Chemometrics; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Evaluation of column; Exact sciences and technology; General pharmacology; Hydrogen-Ion Concentration; Medical sciences; Models, Chemical; Multivariate Analysis; Orthogonal array design; Other chromatographic methods; Pharmaceutical Preparations - isolation & purification; Pharmacology. Drug treatments; Response surface fitting; Software; Sulfonylurea Compounds - isolation & purification; Orthogonal array design; Central composite design; Response surface fitting; Evaluation of column; Chemometrics; Chemical analysis; Phenolic acid; Multicomponent mixture; Monolithic column; Tolbutamide; HPLC chromatography; Indoprofen; Optimization; Non steroidal antiinflammatory agent; Reversed phase chromatography; Hypoglycemic agent; Carboxylic acid; Experimental design; Sulfonylureas; Chlorpropamide; Arylpropionic acid derivatives; Response surface; Stationary phase
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2005.11.101

An optimization strategy for the separation of an acidic mixture by employing a monolithic stationary phase is presented, with the aid of experimental design and response surface methodology (RSM).
An orthogonal array design (OAD) OA
16 (2
15) was used to choose the significant parameters for the optimization. The significant factors were optimized by using a central composite design (CCD) and the quadratic models between the dependent and the independent parameters were built. The mathematical models were tested on a number of simulated data set and had a coefficient of
R
2
>
0.97 (
n
=
16). On applying the optimization strategy, the factor effects were visualized as three-dimensional (3D) response surfaces and contour plots. The optimal condition was achieved in less than 40
min by using the monolithic packing with the mobile phase of methanol/20
mM phosphate buffer pH 2.7 (25.5/74.5, v/v). The method showed good agreement between the experimental data and predictive value throughout the studied parameter space and were suitable for optimization studies on the monolithic stationary phase for acidic compounds.