scholarly journals Application of Box–Behnken Design to Investigate the Effect of Process Parameters on the Microparticle Production of Ethenzamide through the Rapid Expansion of the Supercritical Solutions Process

Pharmaceutics ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 42 ◽  
Author(s):  
Yung-Tai Hsu ◽  
Chie-Shaan Su
Keyword(s):  
Thermal Behavior ◽  
Process Parameters ◽  
Crystal Form ◽  
Rapid Expansion ◽  
Crystal Habit ◽  
Extraction Temperature ◽  
Box Behnken Design ◽  
Mean Size ◽  
Supercritical Solutions ◽  
Expansion Temperature

In this study, the rapid expansion of the supercritical solutions (RESS) process was used to produce microparticles of a commonly used anti-inflammatory drug, ethenzamide. The effects of process parameters in RESS including the extraction temperature, pre-expansion temperature, and post-expansion temperature were investigated using the Box–Behnken design. According to the results of the analysis of variance (ANOVA), the effect of pre-expansion temperature is the most significant parameter on the mean size of RESS-produced ethenzamide. A higher pre-expansion temperature benefits the production of smaller crystals. In addition, a quadratic effect of the post-expansion temperature was also identified. Through RESS, ethenzamide microparticles with a mean size of 1.6 μm were successfully produced. The solid-state properties including the crystal habit, crystal form, thermal behavior, and spectrometric property were characterized by scanning electron microscopy (SEM), Fourier-transform infrared spectrometer (FTIR), differential scanning calorimeter (DSC), and powder X-ray diffraction (PXRD). These analytical results show that the rod-like crystals were generated through RESS, and the crystal form, thermal behavior, and spectrometric property of RESS-produced crystals are consistent with the unprocessed ethenzamide.

Trends on the Rapid Expansion of Supercritical Solutions Process Applied to Food and Non-food Industries

2019 ◽  
Vol 10 (2) ◽  
pp. 82-92 ◽  
Author(s):  
Maria T.M.S. Gomes ◽  
Ádina L. Santana ◽  
Diego T. Santos ◽  
Maria A.A. Meireles
Keyword(s):  
Process Parameters ◽  
Food Industry ◽  
Size Structure ◽  
Rapid Expansion ◽  
High Yield ◽  
Particle Engineering ◽  
Bioactive Constituents ◽  
Bioactive Substances ◽  
Food Industries ◽  
Supercritical Solutions

Background: The supercritical fluids applied to particle engineering over the last years have received growing interest from the food and non-food industries, in terms of processing, packaging, and preservation of several products. The rapid expansion of supercritical solutions (RESS) process has been recently reported as an efficient technique for the production of free-solvent particles with controlled morphology and size distribution. Objective: In this review, we report technological aspects of the application of the RESS process applied to the food and non-food industry, considering recent data and patent survey registered in literature. Methods: The effect of process parameters cosolvent addition, temperature, pressure, nozzle size among others, during RESS on the size, structure and morphology of the resulted particles, and the main differences about recent patented RESS processes are reviewed. Results: Most of the experimental works intend to optimize their processes through investigation of process parameters. Conclusion: RESS is a feasible alternative for the production of particles with a high yield of bioactive constituents of interest to the food industry. On the other hand, patents developed using this type of process for food products are very scarce, less attention being given to the potential of this technique to develop particles from plant extracts with bioactive substances.

Maximized Extraction of Flavonoid Luteolin from V.negundo L. Leaves: Optimization Using Box-Behnken Design

2019 ◽  
Vol 15 (3) ◽  
pp. 343-350 ◽  
Author(s):  
Lubna Abidin ◽  
Mohammad Mujeeb ◽  
Showkat R. Mir
Keyword(s):  
Process Parameters ◽  
High Performance ◽  
Optimization Technique ◽  
Optimization Method ◽  
Extraction Methods ◽  
Statistical Technique ◽  
Extraction Time ◽  
Extraction Temperature ◽  
Box Behnken Design ◽  
Extraction Field

Background: Luteolin is a flavonoid unveiling various therapeutic activities, found in Vitex negundo L. Thus, there is a need to present process parameters at which maximum amount of luteolin can be extracted from V. negundo L. leaves in “one-run”. Objective: Response surface methodology (RSM) was employed for optimizing the process parameters for the extraction of luteolin from V. negundo L. leaves. The study also compared the efficacy of various traditional and modern extraction methods for luteolin extraction. Methods: Extraction conditions (solvent to drug ratio, extraction temperature and extraction time) were optimized by RSM, Box-Behnken Design (BBD). Quantification of luteolin in various extracts was done through High Performance Liquid Chromatography (HPLC). Results: Hot solvent extraction by reflux technique stood out to be the best technique and methanol was found to be the most effective solvent for luteolin extraction.Through the use of BBD, the optimal conditions for luteolin extraction were established as: solvent to drug ratio- 17.7 mL/g, extraction temperature- 55.5°C and extraction time-2.04 hours. Under such conditions 7.32 %w/w of luteolin was yielded which was close to predicted value of 7.29 %w/w. Conclusion: Reflux technique stood out to be the best among all the studied modes of extraction and methanol proved to be the most effective solvent. Moreover, all the three variables significantly affected the luteolin extraction. Our study shows the applicability of a statistical technique, RSM in phytocompound extraction field. This makes the optimization technique cheap and less laborious than the traditional optimization method.

scholarly journals Recrystallization and Micronization of p-Toluenesulfonamide Using the Rapid Expansion of Supercritical Solution (RESS) Process

Crystals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 449 ◽  
Author(s):  
Tsung-Mao Yang ◽  
Chie-Shaan Su ◽  
Jin-Shuh Li ◽  
Kai-Tai Lu ◽  
Tsao-Fa Yeh
Keyword(s):  
Operating Conditions ◽  
Rapid Expansion ◽  
Optimum Operating ◽  
Control Factor ◽  
Process Conditions ◽  
Extraction Temperature ◽  
Control Factors ◽  
Supercritical Solution ◽  
Average Size ◽  
Expansion Temperature

This study is focused on the micronization of p-toluenesulfonamide (p-TSA) using the rapid expansion of supercritical solution (RESS) process. Taguchi’s experimental design method was applied to determine the optimum operating conditions. L9(34) orthogonal array with four control factors and three levels of each control factor was used to design nine experimental conditions. Four control factors were selected, including extraction temperature, extraction pressure, pre-expansion temperature, and post-expansion temperature. The particle size and morphology of the prepared samples were observed by scanning electron microscopy (SEM). In addition, Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC) were employed to compare the differences between the raw and micronized p-TSA particles. The experimental and analytical results indicated that the extraction temperature was the most significant factor for the micronization of p-TSA in the RESS process, and the optimal operating conditions were at an extraction temperature of 50 °C, an extraction pressure of 220 MPa, a pre-expansion temperature of 220 °C, and a post-expansion temperature of 30 °C. The p-TSA particles were micronized from the original average size of 294.8 μm to the smallest average size of 1.1 μm at the optimal RESS process conditions. Furthermore, the physicochemical characteristics of p-TSA did not differ significantly before and after recrystallization.

On the interaction of azithromycin monohydrate with metallic containers

2006 ◽  
Vol 39 (6) ◽  
pp. 826-830 ◽  
Author(s):  
J. Montejo-Bernardo ◽  
S. García-Granda ◽  
M. Bayod-Jasanada ◽  
I. Llorente ◽  
L. Llavona
Keyword(s):  
Crystal Form ◽  
Crystal Habit ◽  
Metallic Surfaces ◽  
Crystal Face ◽  
Great Propensity ◽  
Erythromycin A ◽  
Semisynthetic Derivative

The monohydrate form of azithromycin (an antibiotic semisynthetic derivative of erythromycin A) is difficult to manipulate due to its great propensity to stick to metallic surfaces (during crystallization, drying, grinding,etc.). In this paper, this behaviour is explained on the basis of the conformation and packing of the azithromycin molecules in this crystal form. In particular, the crystal habit favours interaction between the N and O atoms with the metal through one particular crystal face.

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