Experimental design methodology and data analysis technique applied to optimise an organic synthesis

Guervenou, J.; Giamarchi, Philippe; Coulouarn, C; Guerda, M; Lez, C Le; Oboyet, T

doi:10.1016/s0169-7439(02)00038-2

Cited by 16 publications

(5 citation statements)

References 6 publications

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“…Fitting experimental data to generate response surface model, regression modeling techniques and optimization methods are usually combined into RSM. The statistical method of experimental design has the advantage of optimization of several processes [23][24][25][26][27] and of being less expensive and time-consuming than the classical method.…”

Section: Introductionmentioning

confidence: 99%

Using the Response Surface Methodology to Optimize the Extraction of Silica and Alumina from Coal Fly Ash for the Synthesis of Zeolite Na-A

et al. 2011

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Response surface methodology and inductively coupled plasma-optical emission spectroscopy were used to analyze the silicon (Si) and aluminum (Al) ion concentrations extracted from microwave-assisted hydrothermal fusion reactions between coal fly ash (CFA) and sodium hydroxide solution. The extracts containing Si and Al ions were successfully converted to zeolites by hydrothermal treatment at 95 • C for 72 h. Fifteen experimental conditions for the extraction process were obtained using Box-Behnken design through the manipulation of three independent variables. These variables include NaOH concentration (2, 4 and 6 M), power level of microwave irradiation (10, 50 and 100 W)+++ and exposure time (1, 3.5 and 6 min). The statistical analysis result indicated a significant interaction effect with a p value of 0.001. Increasing the values of all the three variables led to an increase in the concentration of Si and Al ions in the CFA extract. The optimized combinations of the three variables within the experimental range for Si and Al extraction were 5.6 M for NaOH concentration, 5.5 min time of exposure to microwave irradiation and 100 W of microwave power level. Based on the extracted concentration values of Si and Al, three products were isolated; zeolite Na-A, sodalite octahydrate and gibbsite which were characterized by their XRD images. Plots of percent yield of the final products versus [Si 4+ ] and [Al 3+ ] revealed a trend of the types of product for various ranges of concentrations of the ions in the extracts prior to hydrothermal treatment at 95 • C.

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Section: Introductionmentioning

confidence: 99%

Using the Response Surface Methodology to Optimize the Extraction of Silica and Alumina from Coal Fly Ash for the Synthesis of Zeolite Na-A

et al. 2011

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“…According to this diagram, the temperature of the reaction medium is the most important effect, followed by the effect of the amount of anhydride and then the effect of the amount of kaolin and the volume of solvent; On the contrary, the interactions between Qc* T and Qc*Qa showed significant effects. However, the other interactions (Qc* V , Qa* V , Qa* T and T * V ) had weaker effects as they did not exceed the reference line (2.36) and had small effects that were not statistically significant 31 …”

Section: Resultsmentioning

confidence: 89%

A chemometric approach based on a full factorial design to optimize terpene acylation using natural kaolin as eco‐friendly catalyst

Boukachabia

Bendjeffal

Merabet‐Khelassi

et al. 2023

Flavour & Fragrance J

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A statistical approach was successfully applied to optimize the acylation of l‐menthol 1 in the presence of natural kaolin as an eco‐compatible catalyst. The influence of the main variation of the operating parameters, namely solvent volume, amount of the acyl donor, temperature and the catalytic rate of kaolin, was studied. A full factorial design (FFD) was used to search for the optimum of each parameter affecting the evolution of l‐menthol 1 acylation. A quadratic polynomial regression model was applied to analyse the experimental data with a p‐confidence level <.05 (95%). Statistical analysis of the data confirmed that temperature (T), acyl donor/acceptor ratio (Qa), kaolin mass (Qc) and solvent volume (V) were the significant factors affecting the l‐menthol catalytic acylation process. The determination coefficient of the adopted model was in the order of 98%. A set of optimal reaction conditions was established, and experimental tests were performed to validate the optimal conditions; the threshold of 100% was reached. Monitoring the kinetic profile of the reaction by gas chromatography (GC) showed complete conversion after 30 min of reaction. An upgrade of this developed environmentally benign process was applied to some monoterpenic alcohols, and the corresponding acetates were yielding at 45%–90%.

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“…Although DoE has been widely used in analytical chemistry, its utility in synthetic chemistry remains largely unknown, especially in the academic field [ 36 ]. A few previous studies report significant applications of DoE in synthetic chemistry, leading to improved yields of high purity products in the shortest time and with minimum amounts of reagents [ 37 , 38 , 39 ].…”

Section: Introductionmentioning

confidence: 99%

Chemometrically Assisted Optimization of Pregabalin Fluorescent Derivatization Reaction with a Novel Xanthone Analogue and Validation of the Method for the Determination of Pregabalin in Bulk via a Plate Reader

et al. 2022

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Quantitation of chromophore-free analytes is always a challenge. To this purpose, derivatization of the analyte constitutes a common strategy, leading to a product with a strong signal. In the current study, a novel xanthone analogue was utilized for the first time for the derivatization of pregabalin, a model analyte with a primary amine moiety that lacks a chromophore. The fact that only the xanthene-based derivative, formed after the derivatization reaction fluoresces, enables avoiding its chromatographic separation from the reagent and thus reducing the analysis time of a series of samples in 1–2 min via a plate reader. The reaction conditions were optimized via a central composite design (CCD), with fluorescence signal as the measure of the yield. The following factors that affect the derivatization reaction were chosen: (a) temperature, (b) reaction time, and (c) triethylamine solution volume used to drive the reaction to completion. After the identification of the optimal conditions, the method was validated according to ICH guidelines, using a fluorescence plate reader for signal measurement (λex = 540, λem = 615 nm). Finally, the newly developed high-throughput method was applied to the determination of drug content in pregabalin bulk.

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Experimental design methodology and data analysis technique applied to optimise an organic synthesis

Cited by 16 publications

References 6 publications

Using the Response Surface Methodology to Optimize the Extraction of Silica and Alumina from Coal Fly Ash for the Synthesis of Zeolite Na-A

Using the Response Surface Methodology to Optimize the Extraction of Silica and Alumina from Coal Fly Ash for the Synthesis of Zeolite Na-A

A chemometric approach based on a full factorial design to optimize terpene acylation using natural kaolin as eco‐friendly catalyst

Chemometrically Assisted Optimization of Pregabalin Fluorescent Derivatization Reaction with a Novel Xanthone Analogue and Validation of the Method for the Determination of Pregabalin in Bulk via a Plate Reader

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