Multivariate optimisation of a cyclodextrin-assisted-capillary zone electrophoretic method for the separation of torasemide and its metabolites

Akesolo, Urtzi; González, Lino; Jiménez, Roberto; Alonso, Rosa M.

doi:10.1016/s0021-9673(03)00055-4

Cited by 13 publications

(11 citation statements)

References 25 publications

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“…In fact, a method can become specific/selective thanks to the optimisation of the experimental conditions. This is a simple example where optimisation and validation are linked together and several experimental design applications for this purpose can be found in the literature [24,36,37,38,39,40,41,42]. It should be noted that most of the cited works commonly deal with optimising resolution, rather than method selectivity.…”

Section: Resultsmentioning

confidence: 99%

How experimental design can improve the validation process. Studies in pharmaceutical analysis

Furlanetto

Orlandini

Mura

et al. 2003

Analytical and Bioanalytical Chemistry

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A critical discussion about the possibility of improving the method validation process by means of experimental design is presented. The reported multivariate strategies concern the evaluation of the performance parameters robustness and intermediate precision, and the optimisation of bias and repeatability. In particular, accuracy and precision improvement constitutes a special subset of experimental design in which the bias and the relative standard deviation of the assay are optimised. D-optimal design was used in order to plan experiments for this aim. The analytical methods considered were capillary electrophoresis, HPLC, adsorptive stripping voltammetry and differential pulse polarography. All methods were applied to real pharmaceutical analysis problems.

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Section: Resultsmentioning

confidence: 99%

How experimental design can improve the validation process. Studies in pharmaceutical analysis

Furlanetto

Orlandini

Mura

et al. 2003

Analytical and Bioanalytical Chemistry

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“…[17,29] After the individual desirabilities were calculated for each response, they were combined to provide a measure of the composite desirability of the multi-response system. This measure is the weighted geometric average of the individual desirability or the responses.…”

Section: Capillary Electrophoretic Enantioresolution Of Tamsulosin 225mentioning

confidence: 99%

“…The most popular methodology applied to multiple response optimization is the desirability function approach. [28,29] The measured properties of each response Y i , I ¼ 1, 2, are transformed to a dimensionless desirability scale (d i ), defined as partial desirability function. This make it possible to combine results obtained for properties measured on different scales.…”

Section: Capillary Electrophoretic Enantioresolution Of Tamsulosin 225mentioning

confidence: 99%

“…The shortest t 2 (3.0 min) and the highest R value (2.5) in all experiments were given the value 1 (maximum), while the longest t 2 (6.0 min) and the lowest R 2 values (the unwanted one, 1.0) were given the value 0 (minimum). Linear interpolation allowed us to calculate the normalized values for the remaining t 2 and R, normalized values were called d 1 , and d 2 , which could be calculated according to the following equations: [28,29] …”

Section: Capillary Electrophoretic Enantioresolution Of Tamsulosin 227mentioning

confidence: 99%

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Design of Experiments for Capillary Electrophoretic Enantioresolution of Tamsulosin using Sulfated‐β‐Cyclodextrin as Chiral Selector

Zhang

Gong

et al. 2007

Journal of Liquid Chromatography & Related Technologies

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A method of quickly determining tamsulosin enantiomers by capillary zone electrophoresis with a photodiode array detector was developed. Response surface methodologies based on three-level, three-variable designs such as Box-Behnken design, central composite face-centered, and central composite circumscribed design, were comparatively used for the optimization with respect to selector concentration, applied voltage, and column temperature. Statistical interpretation of the variables on different responses, such as resolution and migration time of the last isomer were performed. The optimum conditions of these variables were predicted by using a second-order polynomial model, fitted to the results obtained by applying three designs. The response surface plots using three experimental designs revealed a separation optimum with 100 mM tris (hydroxymethyl) aminomethane buffered with phosphoric acid to pH ¼ 2.5, concentration of sulfated-b-cyclodextrin, 0.15% (W/V), column temperature 258C, and applied voltage of 25 kV. The significance of the statistical designs was confirmed by the generally good agreement obtained between predicted responses and actual experimental data. We have concluded that experimental designs offer a rapid means of optimizing several variables, and provide an efficient test for the robustness of the analytical method.

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“…In that process, different weight factors are to be assigned for each of the responses. Larger and smaller weight factors can be given to more important responses and less important responses, respectively [7] . .…”

Section: Experimental Design For Hplc Separationmentioning

confidence: 99%

Optimization strategies for separation of sulfadiazines using Box-Behnken design by liquid chromatography and capillary electrophoresis

Gong

Zhang

Yi-jun

et al. 2007

J Cent. South Univ. Technol.

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Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H 2 O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35 ℃ and 1.0 mL/min, respectively. Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.

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Multivariate optimisation of a cyclodextrin-assisted-capillary zone electrophoretic method for the separation of torasemide and its metabolites

Cited by 13 publications

References 25 publications

How experimental design can improve the validation process. Studies in pharmaceutical analysis

How experimental design can improve the validation process. Studies in pharmaceutical analysis

Design of Experiments for Capillary Electrophoretic Enantioresolution of Tamsulosin using Sulfated‐β‐Cyclodextrin as Chiral Selector

Optimization strategies for separation of sulfadiazines using Box-Behnken design by liquid chromatography and capillary electrophoresis

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