Multi‐objective optimization strategy based on desirability functions used for electrophoratic separation and quantification of rosiglitazone and glimepiride in plasma and formulations

Abstract

Multiple response simultaneous optimization employing Derringer's desirability function was used for the development of a capillary electrophoresis method for the simultaneous determination of rosiglitazone (RSG) and glimepiride (GLM) in plasma and formulations. Twenty experiments, taking the two resolutions, the analysis time, and the capillary current as the responses with three important factors--buffer morality, volte and column temperature--were used to design mathematical models. The experimental responses were fitted into a second order polynomial and the six responses were simultaneously optimized to predict the optimum conditions for the effective separation of the studied compounds. The separation was carried out by using capillary zone electrophoresis (CZE) with a silica capillary column and diode array detector at 210 nm. The optimum assay conditions were 52 mmol l⁻¹ phosphate buffer, pH 7, and voltage of 22 kV at 29 °C. The method showed good agreement between the experimental data and predictive value throughout the studied parameter space. The assay limit of detection was 0.02 µg ml⁻¹ and the effective working range at relative standard deviation (RSD) of ≤ 5% was 0.05-16 µg ml⁻¹ (r = 0.999) for both drugs. Analytical recoveries of the studied drugs from spiked plasma were 97.2-101.9 ± 0.31-3.0%. The precision of the assay was satisfactory; RSD was 1.07 and 1.14 for intra- and inter-assay precision, respectively. The proposed method has a great value in routine analysis of RSG and GLM for its therapeutic monitoring and pharmacokinetic studies.

A systematic and critical review on bioanalytical method validation using the example of simultaneous quantitation of antidiabetic agents in blood

“…The methods included in this systematic review were validated according to the criteria established by the "Guidance for Industry - Bioanalytical Method Validation" by US FDA [3] (16 records) [9,12,15,[20][21][22][23]27,29,30,[32][33][34][38][39][40], "Harmonized Tripartite Guideline" by ICH [73] (four records) [16,17,36,38], "RDC 27/2012 -Minimum Requirements for Validation of Bioanalytical Methods" by ANVISA [5] (one record) [37], "The Fitness for Purpose of Analytical Methods" by Eurachem [98] (one record) [7], "Requirements for Initial Assay Validation and Publication in Journal of Chromatography B" by Wolfgang Lindner and Irving W. Wainer [99] (one record) [26], "Requirements for the Validation of Analytical Methods" by the Society of Toxicological and Forensic Chemistry [100] (one record) [18]; "Validation of New Methods" by Peters, Drummer and Musshoff, 2007 [101] (two records) [13,18] and "MS Identification Guidelines in Forensic Toxicology" by Australian/New Zealand Specialist Advisory Group in Toxicology [102] (one record) [13]. Although the EMA has a specific guideline for bioanalytical method validation, none of the records declared to have used it as guidance.…”

“…None of the main guidelines describes how to evaluate LOD, nor do they require the assessment of this parameter. Despite this, 19 articles determined the LOD, considering it to be three times the blank plasma signal [7,[9][10][11]13,[16][17][18][19][24][25][26]29,31,32,35,[38][39][40], as suggested in the ICH guideline (for analytical method validation) [73]. Although not mandatory, the determination of LOD is interesting and must be considered when the qualitative identification of the drug is important information.…”

“…Only 15 records followed the instructions regarding the number of curves [7,9,13,14,[16][17][18]20,21,23,27,29,37,39,40], while 19 did not report how many curves were prepared [8,[10][11][12]15,19,22,[24][25][26]28,[30][31][32][33][34][35][36]38]. Regarding the calibration levels, 24 records included six or more levels [7,9,[11][12][13][14][15][16][17][18][19][20][21][22][23]25,[27]…”

“…This specification should be met by at least 75% of the analyzed points [3][4][5]. However, only ten records followed this recommendation regarding curve specifications [15,17,21,[27][28][29]33,37,39,40]. The other articles did not report whether these criteria were evaluated and considered the curve acceptable through the correlation coefficient (r).…”

“…Of the 34 articles included in this review, 25 assessed precision according to the recommendations and obtained values within those established in the guidelines [7][8][9][12][13][14][15][16][17][19][20][21][22][23][27][28][29][31][32][33][34][37][38][39][40]. The other nine did not follow the guidelines or the values are out of the acceptable deviation [10,11,18,[24][25][26]30,35,36].…”