Utilisation des plans d'expériences pour évaluer la robustesse d'une méthode d'analyse quantitative par Chromatographie en
Phase Liquide

Vial, Jérôme; Jardy, Alain

doi:10.1051/analusis:1998104

Cited by 11 publications

(4 citation statements)

References 14 publications

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“…In addition, the HPLC method was fully validated and studied, and its dispersion characteristics were estimated rigorously through a collaborative study. − Briefly, this method used isocratic elution reversed-phase chromatography and UV detection. Resulting chromatograms were produced and processed by a Shimadzu Class-VP acquisition station.…”

Section: Methodsmentioning

confidence: 99%

Experimental Comparison of the Different Approaches To Estimate LOD and LOQ of an HPLC Method

1999

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Detection and quantification limits (LOD and LOQ) are two fundamental elements of method validation. Rigorous statistical definitions exist, but in HPLC they could not be implemented. Nevertheless there are several estimation methods for these limits. The most commonly used is the signal-to-noise ratio criterion. Others are based on the dispersion characteristics of the regression line, either simple or weighted. For LOQ, Eurachem proposed an alternate approach based on the use of a target value for the area RSD. Since official guidelines imposed no particular modus operandi, an experimental methodology was set up to investigate the compatibility of the different approaches and their respective reliabilities. Several samples prepared in a concentration range close to the limits were analyzed. It appeared that, both for values and their reliabilities, the different approaches were far from equivalent. In our opinion, the best way to handle the problem of detection and quantification limits was a methodology based on the use of the residual standard deviation of a weighted regression for LOD and on a Eurachem approach for LOQ. Values obtained by these means had the advantage of being reliable, i.e., with a small dispersion, and were still compatible with those obtained with the usual signal-to-noise ratio approach.

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Section: Methodsmentioning

confidence: 99%

Experimental Comparison of the Different Approaches To Estimate LOD and LOQ of an HPLC Method

1999

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“…Indeed, variations to the beach must satisfy two criteria that may be contradictory. On one hand, the range of change factors must be large enough that we observe significant changes in the response; on the other hand, it must be small enough to be able to simulate changes likely to occur in an uncontrolled manner during the performance of the method [17]. These considerations have led us to define the experimental fields as shown in Table 1.…”

Section: Experimental Datamentioning

confidence: 99%

Support vector machines for modelling phosphocalcic hydroxyapatite by precipitation from a calcium carbonate solution and phosphoric acid solution

Labjar¹,

Cherif

Digua³

et al. 2016

Journal of Taibah University for Science

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The aim of this work was to develop an effective quantitative relationship model using support vector machines for the synthesis of phosphocalcic hydroxyapatite by precipitation from a calcium carbonate solution and a phosphoric acid solution. The model was created using a set of factors consisting of the pH of the reaction solution, the Ca/P molar ratio of the reagents, the reaction time and the initial concentration of calcium. Previous studies modelled these relationships using different classification techniques. In this paper, a novel approach based on support vector machines (SVMs) is introduced. This latter approach yields the best result compared to polynomial regression (PR), linear regression (LR) and artificial neural networks (ANN). In addition, the contribution of each descriptor is evaluated. Thus, the proposed method can be successfully used to predict the Ca/P analysis directly from the considered factors.

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“…In addition, the HPLC method has been fully validated and studied [20], and its dispersion characteristics estimated rigorously through a collaborative study [21 -23]. Briefly, this method used isocratic elution reversed phase chromatography.…”

Section: Product and Hplc Methodsmentioning

confidence: 99%

Study of the Linear Range in HPLC Analyses with UV Detection: Methodology and Experimental Application to the Influence of the Analyte UV Spectrum

Vial

Jardy

1999

J. High Resol. Chromatogr.

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Determination of the linear range is one of the main concerns in validation of an HPLC analysis method. It is particularly important since single point calibration will be then used routinely. We proposed an iterative methodology to handle this problem. The idea was, at each step, to test statistically whether the following point belonged to the same regression line. The methodology was then used to evaluate quantitatively the effect on linear range of a shift in detection wavelength or of the detector bandwidth. Although experimental results were globally in accordance with spectroscopic theory, magnitudes observed were rather large. So the linear range could vary by a factor of over 2 with changes in conditions that remained within the range of current practical values. Changes in detection wavelength were limited to about fifteen nm around λmax and the detector used was considered to be representative of modern high‐performance UV detectors. The question of how to take consequences in method validation into account was raised. The solution proposed recommended that the validation was undertaken in conditions as close as possible to those where the method would be conducted routinely. This means with the same instrumentation and on the product of interest for analyses.

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Utilisation des plans d'expériences pour évaluer la robustesse d'une méthode d'analyse quantitative par Chromatographie en Phase Liquide

Cited by 11 publications

References 14 publications

Experimental Comparison of the Different Approaches To Estimate LOD and LOQ of an HPLC Method

Experimental Comparison of the Different Approaches To Estimate LOD and LOQ of an HPLC Method

Support vector machines for modelling phosphocalcic hydroxyapatite by precipitation from a calcium carbonate solution and phosphoric acid solution

Study of the Linear Range in HPLC Analyses with UV Detection: Methodology and Experimental Application to the Influence of the Analyte UV Spectrum

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