Fractional Factorial Experimental Design as a Teaching Tool for Quantitative Analysis

1998 ◽  
Vol 75 (3) ◽  
pp. 357 ◽  
Author(s):  
Philip J. Oles
2010 ◽  
Vol 22 (1-3) ◽  
pp. 22-29 ◽  
Author(s):  
Mehran Mohammadian Fazli ◽  
Ali Reza Mesdaghinia ◽  
Kazem Naddafi ◽  
Simin Nasseri ◽  
Masoud Yunesian ◽  
...  

Pharmacia ◽  
2021 ◽  
Vol 68 (1) ◽  
pp. 79-87
Author(s):  
Оlena Golembiovska ◽  
Oleksii Voskoboinik ◽  
Galina Berest ◽  
Sergiy Kovalenko ◽  
Liliya Logoyda

Aim. The aim of study was to develop and validate a simple, highly robust (quality by design (QbD) approach), precise and accurate method using high performance liquid chromatography for the simultaneous determination of original active pharmaceutical ingredient Quinabut and its impurities. Materials and methods. Experiments were performed on a Shimadzu LC-20 Prominence HPLC separation module, equipped with a quaternary gradient pump, temperature controlled column heater, sampler manager and diode array detector and LC-20 Chemstation for data analysis (Shimadzu Corporation, Japan). Same software was used for data acquisition and processing of results. X-Terra RP18 (4.6×150 mm, 5 μm) analytical chromatographic column provided by Waters Corporation (Milford, MA) was used for all optimization experiments. Mobile phase A: acetonitrile R. Mobile phase B: 0.025 M phosphate buffer solution. Samples were chromatographed in gradient mode. Flow rate of the mobile phase: 0.7 mL/min. Column temperature: 40 °С. Detection: at 233 nm wavelength. Injection volume: 50 μl. Results. Screening of the influence of four chromatographic factors on different chromatographic responses was performed as the initial step of analytical method optimization. A randomized fractional factorial experimental design (24–1) of resolution IV with central point was used. Buffer pH, amount of acetonitrile in mobile phase A, the amount of phosphate buffer solution in mobile phase B and column temperature were selected as factors of interest, and were used to generate the fractional factorial experimental design. Linearity was established in the range of LOQ level to 0.2% having regression coefficients 0.9977. Calibration curve – y = 0.0132 + 0.9902. Since Δt for the content of quinabut is less than max δ, the technique is stable over time. The possibility of contamination of the sample by decomposition products by keeping it under stressful conditions (irradiation of the substance solution with UV light (UV irradiation with mercury lamp light); acid hydrolysis with 0.1 M hydrochloric acid solution; oxidative decomposition) was investigated. As a result of the irradiation with UV light, the impurity peaks for about 8.74 min (impurity C) and 12.68 min (impurity B) are additionally revealed. Their content exceeds the limits of normalization and is 0.6% and 3.7%, respectively. Therefore, the powder of the substance and its solutions should be stored away from direct sunlight. The column temperature and the speed of the mobile phase within ± 10% did not significantly affect the test results. The results were found to be within the assay variability limits during the entire process. Conclusion. 1) The optimization of a new analytical method capable of simultaneous determination of quinabut assay and its impurities drug products was performed with a single fractional factorial experimental design. Only 11 experiments were needed for the optimization, while at least 16 experiments would be needed to cover the same analytical method operational region of the first optimization step with a traditional one factor at time (OFAT) approach. 2) HPLC method was developed and validated for the simultaneous detection and quantitation of quinabut and its impurities. 3) The final analytical method optimized with QbD approach was validated according to ICHQ2R1 guideline. The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating. 4) The method was successfully applied to the analysis of demonstrating acceptable precision and adequate sensitivity for the detection and quantitation of quinabut and its impurities. So it may be reasonable to claim that the method can be extended to the analysis of drug formulations and stability samples as well. This optimization reflects in saving of time and resources since one stability study includes hundreds of samples tested during the product’s shelf life.


2018 ◽  
Vol 11 (1) ◽  
Author(s):  
Camila A. Rezende ◽  
Beatriz W. Atta ◽  
Marcia C. Breitkreitz ◽  
Rachael Simister ◽  
Leonardo D. Gomez ◽  
...  

RSC Advances ◽  
2019 ◽  
Vol 9 (55) ◽  
pp. 32348-32356 ◽  
Author(s):  
Shahin Amani ◽  
Amir Bagheri Garmarudi ◽  
Niloofar Rahmani ◽  
Mohammadreza Khanmohammadi

Herein, the nanosized ZSM-5 zeolite was synthesized based on a fractional factorial experimental design by a hydrothermal method to study the optimum conditions for the synthesis and formation of the ZSM-5 zeolite by employing different conditions.


Buildings ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 214
Author(s):  
Athanasia Soultana ◽  
Michael Galetakis

This study aims to assess the production of cellular micro-concrete, consisting of quarry dust, calcareous fly ash, cement, and aluminum powder as aerating agent. The proposed mixture design methodology is based on a Box–Behnken fractional factorial experimental design. Testing of specimens included compressive and flexural strength, density, water absorption, and thermal conductivity measurements. Results indicate that density is a characteristic property which determines all the measured properties. Aerating agent to cement and fly ash ratio has the strongest effect on all the measured properties. The developed methodology is a valuable tool for the production of cellular micro-concrete with predetermined properties by utilizing large amounts of quarry dust.


1987 ◽  
Vol 22 (3) ◽  
pp. 377-384
Author(s):  
Evangelos Diamadopoulos ◽  
Donald R. Woods

Abstract The effect of five operating variables on the removal of fulvic acid from water by means of aluminum and polymers was studied. These variables were the pH, the calcium concentration in the water, and the polymer dosage, molar mass and degree of hydrolysis. The study followed a 25−1 resolution V fractional factorial experimental design. Based on a statistical analysis, the most significant effects were the pH, the calcium concentration, the polymer molar mass and the interaction of pH with calcium concentration. A calcium concentration of 40 mg/L, a pH of 7 and a polymer with a molar mass of 5 to 6 million were found to be most effective based on fulvic acid removal by filtration. The effect of calcium was larger at pH 8 than at pH 7. The type of polymer did not have any significant effect.


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