• Title/Summary/Keyword: antisolvent

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Experimental Investigation on Finasteride Microparticles Formation via Gas Antisolvent Process

  • Najafi, Mohammad;Esfandiari, Nadia;Honarvar, Bizhan;Aboosadi, Zahra Arab
    • Korean Chemical Engineering Research
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    • v.59 no.3
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    • pp.455-466
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    • 2021
  • Micro and nanoparticles of Finasteride were prepared by gas-antisolvent method. The influence of process parameters such as pressure (100, 130 and 160 bar), temperature (308, 318 and 328 K) and solute concentrations (10, 25 and 40 mg/ml) on mean particle size was studied by Box-Behnken design. As ANOVA results indicated, the highest influence in production of smaller particles was attributed to the pressure. Optimum condition leading to the smallest particle size was as follows: initial solute concentration, 10 mg/ml; temperature, 308 K and pressure, 160 bar. The particles were evaluated with FTIR, SEM, DLS, XRD as well as DSC. The analyses revealed a size decrease in the precipitated Finasteride particles (232.4 nm, on mean) via gas-antisolvent method, as compared to the original particles (55.6 ㎛).

Solubility of Nifedipine in Mixed Solvents and Antisolvent Crystallization (혼합용매에 대한 니페디핀의 용해도와 반용매 결정화)

  • Kang, Mi-Young;Yeo, Sang-Do
    • Korean Chemical Engineering Research
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    • v.58 no.1
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    • pp.92-97
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    • 2020
  • In this study, the solubilities of a pharmaceutical compound, nifedipine, in three mixed solvents were determined. In addition, the nifedipine, that was dissolved in solvents (acetone, DMF, methylene chloride), was recrystallized using antisolvents (water, hexane, carbon dioxide) The external shape, size, and melting point of the crystallized nifedipine were measured. As the mixed solvents, acetone+water, DMF+water, and methylene chloride+hexane were used, and the solubility of nifedipine decreased with increasing antisolvent concentrations in the mixtures. In case of acetone+water, the solubility maximum was observed due to the density anomaly of the mixture, and this phenomenon was not observed in other systems. The crystallized nifedipine particles exhibited the bladed, equant, and prismatic habits, and the particles size was significantly reduced compared to the raw material. The average particle size of raw nifedipine was 337 ㎛, and the size of crystallized particles was in the range of 11.6~69.8 ㎛. All the crystallized nifedipine particles had the same thermal behavior and this result was not influenced by the change of solvent and antisolvent.

Air-Processed Efficient Perovskite Solar Cell via Antisolvent Additive Engineering (안티솔벤트 첨가제 공정에 의한 대기 중 고효율 페로브스카이트 태양전지 제작)

  • Se-Yeong Baek;Seok-Soon Kim
    • Applied Chemistry for Engineering
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    • v.35 no.2
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    • pp.128-133
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    • 2024
  • Although antisolvent-assisted crystallization is one of the promising processes to produce high-quality perovskite films, general antisolvents such as chlorobenzene (CB) have toxic and volatile properties. In addition, CB is not suitable to control the crystallization of perovskite in the atmospheric air. In this work, isopropyl acetate (IA) is used as an eco-friendly antisolvent to demonstrate air-processed perovskite solar cells, and ethyl-4-cyanocinnamate (E4CN) with a cyano group, carbonyl group, and aromatic ring is introduced in IA to improve the performance and stability of devices. Defects at the surface and grain boundaries of the perovskite layer, such as un-coordinated Pb2+ and iodine, can be decreased resulting from the interaction of E4CN and perovskite, and thus reduced recombination and enhanced carrier transport can be expected. As a result, the perovskite device with E4CN achieves a high maximum power conversion efficiency (PCE) of 18.89% and outstanding stability, maintaining 60% of the initial efficiency for 300 h in the air without any encapsulation.

Preparation and Evaluation of Paclitaxel Solid Dispersion by Supercritical Antisolvent Process (초임계유체를 이용한 파클리탁셀고체분산체의 제조 및 평가)

  • Park, Jae-Hyun;Chi, Sang-Cheol;Woo, Jong-Soo
    • Journal of Pharmaceutical Investigation
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    • v.38 no.4
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    • pp.241-247
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    • 2008
  • Paclitaxel is a taxane diterpene amide, which was first extracted from the stem bark of the western yew, Taxus brevifolia. This natural product has proven to be useful in the treatment of a variety of human neoplastic disorders, including ovarian cancer, breast and lung cancer. Paclitaxel is a highly hydrophobic drug that is poorly soluble in water. It is mainly given by intravenous administration. Therefore, The pharmaceutical formulation of paclitaxel ($Taxol^{(R)}$; Bristol-Myers Squibb) contains 50% $Cremophor^{(R)}$ EL and 50% dehydrated ethanol. However the ethanol/Cremophor EL vehicle required to solubilize paclitaxel in $Taxol^{(R)}$ has a pharmacological and pharmaceutical problems. To overcome these problems, new formulations for paclitaxel that do not require solubilization by $Cremophor^{(R)}$ EL are currently being developed. Therefore this study utilized a supercritical fluid antisolvent (SAS) process for cremophor-free formulation. To select hydrophilic polymers that require solubilization for paclitaxel, we evaluated polymers and the ratio of paclitaxel/polymers. HP-${\beta}$-CD was used as a hydrophilic polymer in the preparation of the paclitaxel solid dispersion. Although solubility of paclitaxel by polymers was increased, physical stability of solution after paclitaxel/polymer powder soluble in saline was unstable. To overcome this problem, we investigated the use of surfactants. At 1/20/40 of paclitaxel/hydrophilic polymer/ surfactant weight ratio, about 10 mg/mL of paclitaxel can be solubilized in this system. Compared with the solubility of paclitaxel in water ($1\;{\mu}g/mL$), the paclitaxel solid dispersion prepared by SAS process increased the solubility of paclitaxel by near 10,000 folds. The physicochemical properties was also evaluated. The particle size distribution, melting point and amophorization and shape of the powder particles were fully characterized by particle size distribution analyzer, DSC, SEM and XRD. In summary, through the SAS process, uniform nano-scale paclitaxel solid dispersion powders were obtained with excellent results compared with $Taxol^{(R)}$ for the physicochemical properties, solubility and pharmacokinetic behavior.

Preparation of Zein Microparticles Using Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 Zein 미립자 제조)

  • Ryu, Jong-Hoon;Lim, Gio-Bin
    • KSBB Journal
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    • v.27 no.4
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    • pp.237-242
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    • 2012
  • In this study, zein microparticles and drug-loaded zein microparticles were prepared using supercritical ASES technique. The effects of operating parameters on particle size and morphology were investigated. ASES-processed zein microparticles consisted of agglomerates of very fine unit particles. As temperature increased, the size of unit particles increased and their morphology became more spherical. The addition of water to the solvents for zein resulted in the formation of more spherical microparticles. The release characteristics of drug-loaded zein microparticles were also studied.

Precipitation of Acetaminophen in Supercritical Carbon Dioxide (초임계 이산화탄소 내에서 아세트아미노펜 미세입자 제조)

  • Choi, Sungwoo;Oh, Kyungshil;Kim, Hwayong
    • Clean Technology
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    • v.10 no.4
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    • pp.215-220
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    • 2004
  • Micronized acetaminophen was precipitated from ethanol solution using supercritical $CO_2$ as antisolvent. A coaxial nozzle was used to introduce the supercritical $CO_2$ and the acetaminophen/ethanol solution. The effects of pressure, temperature, $CO_2$ flow rate and solvent flow rate were studied in the constant pressure and temperature condition. The particle size and morphology were influenced by the variations of precipitation condition. The particle size and morphology were analyzed with scanning electron microscopy.

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Preparation of Poly(N-vinyl-2-pyrrolidone) Microparticles Using Supercritical Anti-solvent (초임계 반용매법을 이용한 폴리비닐피롤리돈 미세입자의 제조)

  • Shin, Moon-Sam;Kim, Hwa-Yong
    • Clean Technology
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    • v.14 no.4
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    • pp.242-247
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    • 2008
  • Poly(N-vinyl-2-pyrrolidone) (PVP) has been used as biocompatible and biodegradable polymer in cosmetics, pharmaceuticals and electronics. Micro-particles of PVP were produced using an aerosol solvent extraction system (ASES). Dichloromethane (DCM) and supercritical carbon dioxide were used as solvent and antisolvent, respectively. The mean diameter of the obtained polymer particles ranged from 0.184 to $0.249\;{\mu}m$. The relationship between particle size and initial drop size was also considered.

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Phase Behavior of Poly(methylmethacrylate) (PMMA) in Varions Solvents at High Pressure (고압상태의 다양한 용매 내에서 Poly(methylmethacrylate) (PMMA)의 상거동)

  • Kim, Je-Il;Yoo, Ki-Pung;Lim, Jong-Sung
    • Clean Technology
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    • v.13 no.1 s.36
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    • pp.28-33
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    • 2007
  • We measured cloud points of Poly(methylmethacrylate) (PMMA) in various solvents using the high-pressure variable volume view cell apparatus. The solvents used for dissolving PMMA were chlorodifluoromethane (HCFC-22), dimethylether (DME), 1,1,1-trifluoroethane (HFC-143a), 1,1-difluoroethane (HFC-152a) and 1,1,1,2-tetrafluoroethane (HFC-134a), and the effect of $CO_2$ concentration on the phase behavior of $PMMA+HCFC-22+CO_2$ system and $PMMA+DME+CO_2$ system was observed. PMMA was dissolved well in HCFC-22 from about 340 K, 5MPa and in DME from about 300 K, 28MPa. However, PMMA was not dissolved at all up to 423.15 K, 160MPa in the other fluorine compound such as HFC-l43a, HFC-152a and HFC-134a. PMMA+HCFC-22, $PMMA+HCFC-22+CO_2$ and PMMA+DME systems exhibit the lower critical solution temperature (LCST) behavior, however, $PMMA+DME+CO_2$ system exhibits the upper critical solution temperature (UCST) behavior. In the $CO_2$ mixture, the cloud point pressure of PMMA was increased dramatically proportional to the amount of $CO_2$ added, and from this result, it was known that $CO_2$ could be used as an antisolvent for fabricating PMMA nano-particles. And the cloud point of PMMA could be controlled by changing the concentration of $CO_2$.

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Cooling and Antisolvent Crystallization of Potassium Bicarbonate in the Presence of Sterically Hindered Alkanolamines (입체 장애 알카놀아민 혼합 수용액에서 중탄산칼륨 결정의 냉각 반용매 결정화)

  • Jo, Chang Sin;Jung, Taesung;Yoon, Hyoung Chul;Kim, Jong-Nam;Rhee, Young Woo
    • Clean Technology
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    • v.20 no.4
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    • pp.383-389
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    • 2014
  • $CO_2$ absorption processes have a good potential for large scale capture of $CO_2$ but a large amount of absorbing solution has to be regenerated, undesirably increasing the consumption of energy such as sensible heat and latent heat of vaporization. In this study, a cooling crystallization process which would separate the $CO_2$-rich potassium bicarbonate crystals from $CO_2$-lean water was developed to reduce the energy penalty. Sterically hindered alkanolamine additives were used to enhance the $CO_2$ removal efficiency and their antisolvent effect on the crystallization was found in a continuous cooling crystallizer. The production yields of crystals were increased in the sequence of 2-amino-2-methyl-1-propanol (AMP) < 2-amino-2-methyl-1,3-propanediol (AMPD) < 2-amino-2-hydroxymethyl-1,3-propanediol (AHPD), which are related to the number of hydroxyl groups in the additive molecules. Using $^{13}carbon$ nuclear magnetic resonance, the additives favored the formation of bicarbonate ions by steric hindrance effect and increased the supersaturation of $KHCO_3$. It is shown that the additives increase the mean size of crystals and crystal growth rate by increasing supersaturation. The additives are promising for enhancing the $CO_2$ removal efficiency and reducing the regeneration energy cost of $CO_2$ absorbing solution by promoting $KHCO_3$ crystallization.