Experimental Design in Analytical Chemistry—Part II: Applications

Ebrahimi‐Najafabadi, Heshmatollah; Leardi, Riccardo; Jalali‐Heravi, Mehdi

doi:10.5740/jaoacint.sgeebrahimi2

Cited by 21 publications

(8 citation statements)

References 28 publications

(28 reference statements)

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“…The experimental design (or design of experiments-DOE) is a mathematical modeling approach widely used in chemistry for the optimization of processes or procedures [53][54][55][56]. A response surface, in which both single and interaction effects of the variables of interest are taken into account, is generally built by means of a regression analysis.…”

Section: Statistic Data Analysismentioning

confidence: 99%

Optimization of a sequential extraction procedure for trace elements in Arctic PM10

et al. 2020

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In this work, a two-step sequential extraction scheme for the determination of trace elements in Arctic PM10 samples was optimized by using two certified reference materials (CRMs). By means of an experimental design for qualitative variables, the five most common extracting solutions for particulate matter (PM) sequential extraction (high purity water (HPW), 0.032 M HNO3, 0.022 M HCl, 0.11 M CH3COOH, and 0.012 M CH3COOH/CH3COONH4 buffer) and two different extraction methods (stirring and ultrasounds) were compared. The purpose of the study was the identification of the procedure which gives the best estimation of the anthropogenic portion of the elements present in PM10 samples. The use of ultrasounds instead of stirring induced a low but significant decrease of the extraction of all the elements and a decrease in the repeatability of the procedure. Diluted HNO3 was the extractant which allowed to maximize the extraction of anthropogenic elements (As, Cd, Pb, Zn) with respect to crustal ones (Al, Si, Ti). The optimized procedure proved successful in avoiding contaminations and, therefore, suitable to be applied to PM samples having extremely low concentrations, such as samples collected in polar or other remote areas. The chosen procedure was applied to ten Arctic PM10 samples, allowing for a better identification of their sources. Indeed, it was possible to hypothesize that even though the concentrations of As, Cd, K, Mg, Mn, and Ni in spring and summer were different, their mobility and, therefore, their chemical form in the analyzed PM10 samples were probably similar.

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Section: Statistic Data Analysismentioning

confidence: 99%

Optimization of a sequential extraction procedure for trace elements in Arctic PM10

et al. 2020

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“…It is beneficial to select the most important variables with minimum number of runs . The CCD was employed to investigate the effects of different operating factors on removal capacity and determine the optimum condition for Pb(II) determination. In this work, CCD was employed to investigate the significance of the effects of variables including pH value, mesoporous SBA‐15 dosage, contact time and initial Pb(II) concentration on the removal capacity and difference in absorption for solid optical sensor that designed by using the software package STATISTICA 10.0.…”

Section: Methodsmentioning

confidence: 99%

An easily organic–inorganic hybrid optical sensor based on dithizone impregnation on mesoporous SBA‐15 for simultaneous detection and removal of Pb(II) ions from water samples: Response‐surface methodology

Dashtian

Zare‐Dorabei

2017

Applied Organom Chemis

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In this study, a novel organic-inorganic hybrid adsorbent for single-step detection and removal of Pb(II) ions based on dithizone (DZ) anchored on mesoporous SBA-15 was fabricated. The designed solid optical sensor revealed rapid colorimetric responses and high selectivity. Central composite design (CCD) combined with desirability function (DF) was applied to evaluate the interactive effects and optimization of important variables such as pH value, mesoporous SBA-15 dosage, contact time and initial concentration of Pb(II) ions and optimum conditions for each of the factors were obtained 6.0, 25 mg, 30 min and 20 μg ml − 1 , respectively. This adsorbent or solid optical chemo sensor exhibited a linear range of 1.0 to 100.0 μg ml −1 of Pb(II) ion concentration with a detection limit of 0.07 μg ml −1 . This adsorbent was applied to determine and remove the Pb(II) in spiked samples. Various isotherm models such as Langmuir, Freundlich, Temkin and Dubinin-Radushkevich were studied for fitting the experimental equilibrium data. Langmuir model was chosen as an efficient model. Various kinetic models such as pseudo-first, second order intraparticle, diffusion models were studied for analysis of experimental adsorption data and the pseudo second order model was chosen as an efficient model. KEYWORDS central composite design, mesoporous SBA-15, organic-inorganic hybrid, Pb(II) ions, solid optical sensor

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“…These methods are considered to obtain the optimized response for an analytical performance or an extraction method and development of a formulation in pharmaceutical sciences. [30][31][32] Response surface methodology (RSM) is the common statistical approach based on the fit of a polynomial equation (in order to find the critical point) to the experimental data, which can be expressed by the following equation:…”

Section: Introductionmentioning

confidence: 99%

“…where, Y is the response function, xi and xj are the independent variables, β0 is the intercept and βi, βij and βii are the linear, interaction, and quadratic parameters of the model, respectively. [30][31][32] The objective of the study is to investigate the effect of different factors on the fluorescence of β-blockers by using experimental design methods and providing an analysis method based on the optimal conditions for the determination of ATE and CAR.…”

Section: Introductionmentioning

confidence: 99%

Spectrofluorimetric Determination of Atenolol and Carvedilol in Pharmaceutical Preparations after Optimization of Parameters using Response Surface Methodology

Tabrizi

Yousefzadeh

2019

Pharm Sci

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Background: The present work is aimed to study the effect of different parameters on the fluorescence intensity of atenolol (ATE) and carvedilol (CAR) and optimization by response surface methodology (RSM) to provide a simple analytical method for their quantification in pharmaceutical formulations. Methods: Various parameters affecting the fluorescence intensity, i.e., sodium dodecyl sulfate (SDS) concentration, pH, volume fraction of solvents were optimized using RSM. Then, the optimized parameters were applied to the validation of a method for fluorimetric determination of β-blockers in their pharmaceutical preparations. Results: It is obtained that under the optimum conditions for determination of ATE, the method provided a linear range between 130 to 750 ng/mL with a coefficient of correlation (r) of 0.9996. Also, the limit of detection and limit of quantification (LOD and LOQ) were 40 ng/mL and 130 ng/mL, respectively. Moreover, it is observed that, the linearity of method for determination of CAR was between 0.37 to 4.0 ng/mL and LOD and LOQ of method were 0.11 ng/mL and 0.37 ng/mL, respectively. Conclusion: An accurate, sensitive and reliable spectrofluorimetric method was developed anf successfully used to determine the (ATE) and carvedilol (CAR) in their pharmaceutical preparations.

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Experimental Design in Analytical Chemistry—Part II: Applications

Abstract: This paper reviews the applications of experimental design to optimize some analytical chemistry techniques such as extraction, chromatography separation, capillary electrophoresis, spectroscopy, and electroanalytical methods.

Cited by 21 publications

References 28 publications

Optimization of a sequential extraction procedure for trace elements in Arctic PM10

Optimization of a sequential extraction procedure for trace elements in Arctic PM10

An easily organic–inorganic hybrid optical sensor based on dithizone impregnation on mesoporous SBA‐15 for simultaneous detection and removal of Pb(II) ions from water samples: Response‐surface methodology

Spectrofluorimetric Determination of Atenolol and Carvedilol in Pharmaceutical Preparations after Optimization of Parameters using Response Surface Methodology

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