Experimental design strategies in the optimization and robustness testing of adsorptive stripping voltammetric conditions for kynurenic acid determination

Furlanetto, Sandra; Pinzauti, S.; Gratteri, Paola; Porta, E. La; Calzeroni, G.

doi:10.1016/s0731-7085(96)02029-8

Cited by 26 publications

(11 citation statements)

References 14 publications

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“…The analysis of the variance (ANOVA) indicated that the regression models assumed were significant [20,28]. The null hypothesis H o, i.e., the hypothesis that all coefficients 13i are equal to zero, was disproved, for the three models, and the alternative hypothesis, that one or more of the coefficients is not equal to zero, was considered adequate [34].…”

Section: Resultsmentioning

confidence: 99%

“…The null hypothesis H o, i.e., the hypothesis that all coefficients 13i are equal to zero, was disproved, for the three models, and the alternative hypothesis, that one or more of the coefficients is not equal to zero, was considered adequate [34]. The statistic analysis of coefficients showed that all main effects were significant for the three responses [28]. The considered interactions were found significant for the three responses, except for the interaction pH-voltage that was found not significant for the response R, meaning that the effect of change of one variable on the overall separation and analysis time, is not immediately obvious.…”

Section: Resultsmentioning

confidence: 99%

“…The experimental design strategy involved a fractional factorial design and a central composite design, because a linear model did not give a good fit with the data. From the response surfaces, it was possible to point out that the method was robust with regard to the change in the response with a small change in the factor level [21,28,29]. A desirability function D, that makes it possible to combine results obtained for properties measured on different scales, was used to simultaneously optimize the responses, resolution, and migration times of the two enantiomers [301.…”

Section: Introductionmentioning

confidence: 99%

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Experimental design methodologies to optimize the CE separation of epinephrine enantiomers

Fanali¹,

Furlanetto

Aturki³

et al. 1998

Chromatographia

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SummaryA capillary electrophoretic method using a chiral selector was optimized by experimental design for the enantioresolution of epinephrine enantiomers. Two 13-cyclodextrins derivatives, namely heptakis-2,6-di-O-methy|-13-cyclodextrin and carboxy-methyl-13-cyclodextrin, respectively neutral and charged, were used as chiral selectors employing an uncoated capillary. By using a statistical experimental design in which all factors are varied at the same time, it was possible to optimize the method with regard to the resolution between peaks and the two migration times. A fractional factorial design and a central composite design were used. A compromise between conflicting goals, such as maximization of resolution and minimization of analysis time, was found by means of a desirability function D. Balancing these goals against each other, the most acceptable solution to the problem was found and the optimized method gave a fast separation with complete resolution between the adrenaline enantiomers. The response surfaces obtained confirmed the robustness of the method.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Experimental design methodologies to optimize the CE separation of epinephrine enantiomers

Fanali¹,

Furlanetto

Aturki³

et al. 1998

Chromatographia

Self Cite

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show abstract

“…Then a systematic procedure should be used to implement to method under slightly different experimental parameters [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][65][66][67][68][69][70][71][72]. The usual way of performing robustness testing is first to define the parameters with reasonable maximum variation.…”

Section: Robustnessmentioning

confidence: 99%

The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques

Gümüştaş¹,

Özkan²

2014

TOACJ

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Electroanalytical methods are chosen for the sensitive analysis of pharmaceutically active compounds in their dosage forms and biological samples. Electroanalytical method validation is the process used to confirm that the determination procedure employed for a specific test is suitable for its intended use like other analytical methods. Results from electroanalytical method validation can be used to judge the quality, applicability, accuracy, reliability and consistency of analytical results; it is an integral part of any analytical procedure. Also in electroanalytical drug analysis, important decisions are taken which are based on data obtained from real samples. Validation parameters help assure that the electroanalytical methods ensure the correct identity, strength, quality, accurate, precise, selective, robust and sensitive. A well-defined and well-documented validation process provides regulatory agencies with evidence that the system and method suitable for its intended use. Method validation is an essential component of the measures that a laboratory should implement to permit it to produce reliable electroanalytical data.

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“…Table II). Several criteria can be used to define the optimality of a design; the D-optimal design, in particular, maximizes the determinant D of the product of the matrix of effects (Z) and its transpose (X'), i. e. ]]X'X[] [291, which enables minimization of the variance of the estimates of the effects [30]. The JMP software was used to construct this algorithmic design; this is the best compromise between the quality of information desired and the number of experiments to be performed.…”

Section: Screening Testmentioning

confidence: 99%

Liquid chromatographic analysis of local anesthetics in human plasma after sample preparation by on-line dialysis. Optimization by use of experimental design

et al. 2001

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SummaryA fully automated method involving dialysis, clean-up and enrichment of the diaJysate on a pre-column packed with a strong cation-exchange phase, and subsequent liquid chromatographic (LC) analysis with UV detection at 220 nm has been developed for the determination of local anesthetics (prilocaine, mepivacaine, and bupivacaine) in human plasma.All samplehandling operations were executed automatically by means of an Asted XL system.To identify the most important conditions affecting analyte recovery from the dialysis and trace-enrichment processes, a seven-factor D-optimal design with 16 experimental points was elaborated as a screening test. A four-factor D-optimal design with 24 experimental points was then used to predict and optimize analyte recovery. Derringer's desirabilif,/function was also used to deduce optimum conditions for analyte recovery and dialysis time within the experimental domain.Finally; the method developed was validated. Mean recoveries were approximately 72% for bupivacaine and approximately 67% for mepivacaine and prilocaine. The limits of quantification were 28 ng mL 1 for bupivacaine and 25 ng mL 1 for mepivacaine and prilocaine.

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Experimental design strategies in the optimization and robustness testing of adsorptive stripping voltammetric conditions for kynurenic acid determination

Cited by 26 publications

References 14 publications

Experimental design methodologies to optimize the CE separation of epinephrine enantiomers

Experimental design methodologies to optimize the CE separation of epinephrine enantiomers

The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques

Liquid chromatographic analysis of local anesthetics in human plasma after sample preparation by on-line dialysis. Optimization by use of experimental design

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