Development and validation of a differential pulse polarographic method for quinolinic acid determination in human plasma and urine after solid-phase extraction: a chemometric approach

Furlanetto, Sandra; Pinzauti, S.; Porta, E. La; Chiarugi, Alberto; Mura, Paola; Orlandini, Serena

doi:10.1016/s0731-7085(98)00067-3

Cited by 26 publications

(16 citation statements)

References 18 publications

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“…-an optimisation procedure for simultaneous determination of diazepam and otilonium bromide by capillary electrophoresis [32] -development of a method for determination of quinolinic acid in human plasma and urine by use of differential pulse polarography [33]; -optimisation of method for determination of nimesulide by use of adsorptive stripping voltammetry [34], and -optimisation of a procedure for determination of rufloxacin hydrochloride in coated tablets [35].…”

Section: Introductionmentioning

confidence: 99%

Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction

2003

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This paper proposes a preconcentration procedure for determination of nickel in saline aqueous waste samples by flame atomic absorption spectrometry (FAAS). It is based on cloud-point extraction of nickel(II) ions as 2-(5-bromo-2-pyridylazo)-5-diethilaminophenol (Br-PADAP) complexes using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The optimisation step was performed using a four-variable Doehlert design, involving the factors centrifugation time (CT) of system after addition of surfactant, solution pH, methanol volume (MV) added at micellar phase, and buffer concentration (BC). The analytical response used was absorbance, after volume correction. Using the established experimental conditions in the optimisation step the procedure enables nickel determination with a detection limit (3 delta/ S) of 0.2 microg L(-1), quantification limit (10 delta/ S) of 0.7 microg L(-1), and precision, calculated as relative standard deviation ( RSD) of 4.7 ( n=8) and 3.5% ( n=8) for nickel concentration of 1 and 5 microg L(-1), respectively. The preconcentration factor, determined from the ratio of the slopes of the analytical curves with and without preconcentration, is 74. The recovery achieved for nickel determination in the presence of several cations demonstrated that this procedure could be applied for analysis of water samples. The robustness was checked by using saturated fractional factorial designs, centred on the established experimental conditions in the optimisation step. The results of these tests demonstrated that the variables centrifugation time and buffer concentration are robust for modification by 10% and that solution pH and methanol volume are robust for 5%. Accuracy was evaluated by using the certified material reference SLEW-3 estuarine water for trace metals. The procedure was used for determination of nickel in saline effluents from oil refinery samples. Recovery results (95-104%) indicate that the procedure has satisfactory accuracy for nickel determination in these samples.

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Section: Introductionmentioning

confidence: 99%

Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction

2003

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“…It should be noted that most of the cited works commonly deal with optimising resolution, rather than method selectivity. Meanwhile, when trying to maximise peak height or area, one acts also on limits of detection and quantification [21,22,33,43] Improvement of accuracy and repeatability of an AdSV method for nimesulide determination Accuracy is stated quantitatively in terms of "bias", with smaller absolute value of bias indicating greater accuracy. Precision is usually specified in terms of standard deviation or relative standard deviation [2].…”

Section: Resultsmentioning

confidence: 99%

“…However, few applications of this type have been published [21,25,26,32,33,34]. The factors that can be considered are those suspected to affect the intermediate precision such as day, analyst and equipment.…”

Section: Resultsmentioning

confidence: 99%

“…In addition, an RSD value can be calculated from all the experiments carried out during the experimental design approach and compared with the RSD value obtained from the repeatability study. This approach was successfully used for AdSV methods [32,33], for a differential pulse polarographic method [21] and HPLC methods [25,26].…”

Section: Resultsmentioning

confidence: 99%

“…As for the optimisation of method precision (repeatability), the Taguchi approach [12], the BoxMeyer approach [13], artificial neural networks [14] or experimental design methodology [15] are strategies that have been used. Further original applications of multivariate strategies to validation have dealt with evaluation of robustness [16,17,18,19,20,21,22,23,24,25,26,27,28,29,30,31] and intermediate precision [21,25,26,32,33,34].…”

Section: Introductionmentioning

confidence: 99%

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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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Application of Chemometrics in Capillary Electrophoresis Analysis of Herbal Medicines

Chen

Yang

2009

Chemometric Methods in Capillary Electrophoresis

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Development and validation of a differential pulse polarographic method for quinolinic acid determination in human plasma and urine after solid-phase extraction: a chemometric approach

Cited by 26 publications

References 18 publications

Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction

Doehlert matrix for optimisation of procedure for determination of nickel in saline oil-refinery effluents by use of flame atomic absorption spectrometry after preconcentration by cloud-point extraction

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

Application of Chemometrics in Capillary Electrophoresis Analysis of Herbal Medicines

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