• Journal of the Korea Academia-Industrial cooperation Society
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• v.21 no.2
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• pp.595-600
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• 2020

The purpose of this paper was to prepare and evaluate solid dispersions (SD) that can increase the dissolution rate of dexibuprofen as a model drug with low solubility in water using saccharides and sugar alcohols as dispersion materials. DSC, XRD, content and content uniformity test, dissolution test, and disintegration test were conducted for physicochemical evaluation of the prepared SD. For the results, it was confirmed using differential scanning calorimetry that fructose, which has a melting point around 120 ℃ of the device operating temperature range, is a suitable excipient for the preparation of SD by the rotary hot-melt granulation (RHMG) method. X-ray diffraction analysis was conducted to confirm that the crystallinity of dexibuprofen was reduced. Disintegration test of the prepared tablet using SD-containing dexibuprofen and fructose confirmed a very fast disintegration time within 1~2 seconds and also showed that the dissolution rate was about 20% faster than that of the dexibuprofen raw material. Dexibuprofen with reduced crystallinity by SD confirmed through the RHMG method can be used to increase the dissolution rate of the drug and increase the disintegration time of the tablet. Thus, it can be used in the manufacturing of various solid preparations.

• Journal of Pharmaceutical Investigation
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• v.31 no.3
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• pp.151-160
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• 2001

The purpose of this study is to investigate the interaction of progesterone with various cyclodextrins (CDs) in the aqueous solution and in solid state, and finally to formulate a parenteral aqueous formulation. CDs used were ${\alpha}-$, ${\beta}-$, and ${\gamma}-CD$, $2-hydroxypropyl-{\beta}-CD$ (HPCD), sulfobutyl $ether-{\beta}-CD$ (SBCD), $dimethyl-{\beta}-CD$ (DMCD) and $trimethyl-{\beta}-CD$ (TMCD). The solubility studies of progesterone were performed in the presence of various CDs as a function of concentration or temperature. The solubility of progesterone increased in the rank order of ${\alpha}-CD$ < ${\beta}-CD$ < ${\gamma}-CD$ < TMCD$ < HPCD < DMCD < SBCD. Addition of SBCD (200 mg/ml) in water increased the aqueous solubility $(9.36\;{\mu}g/ml)$ about 3,200 times, and lowering the temperature facilitated the solubilization of progesterone. However, the addition of HPCD and SBCD in 20:80 (v/v) polyethylene glycol 300-water and propylene glycol-water cosolvents markedly decreased the solubility of progesterone, compared with solubilizing effects in water. Physical mixtures and solid dispersions of progesterone with HPCD or SBCD were prepared, and evaluated by differential scanning calorimetry (DSC), Fourier-transform infrared spectroscopy (FT-IR), near IR spectroscopy and dissolution studies. By DSC and IR studies, it was found that progesterone was dispersed in HPCD in monotectic state and dissolved rapidly from both solid dispersions. Based on solubility studies, new aqueous progesterone fonnulations (5 mg/ml) containing SBCD (200 mg/ml) could be prepared and did not form precipitates even after 2 months at $4^{\circ}C$. The solution was transparent when mixed with normal saline and 5% dextrose injection at 1: 1, 1:10 and 1:20 (v/v) even after 7 days. Permeation rates of progesterone through a cellulose membrane from 20% PEG 300 solution $(50\;{\mu}g/ml)$ containing HPCD or SBCD were compared with oily formulation. Permeation of progesterone from oily formulation did not occur up to 8 hr, but aqueous formulations showed fast permeation rates from early stage of permeation study. The addition of HPCD or SBCD retarded the permeation rates of progesterone with the increase of CD concentrations, suggesting the possibility of a controlled absorption from the site administered intramuscularly. These results demonstrate that it is feasible to develop a new progesterone parenteral aqueous injection (5 mg/ml) using SBCD.

• Polymer(Korea)
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• v.31 no.6
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• pp.518-525
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• 2007

The thermomechanical properties and morphologies of nanocomposite fibers of poly(ethylene terephthalate)(PET) incorporating thermally stable organoclays are compared. Dodecyltriphenyl-phosphonium-mica($C_{12}PPh-Mica$) and 1-hexadecane benzimidazole-mica ($C_{16}BIMD-Mica$) were used as reinforcing fillers in the fabrication of PET hybrid fibers. Dispersions of organoclays with PET were studied by using the in-situ polymerization method at various organoclay contents to produce nano-scale composites. The thermo-mechanical properties and morphologies of the PET hybrid fibers were determined using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide angle X-ray diffraction (XRD), electron microscopy (SEM and TEM), and a universal tensile machine (UTM). Transmission electron microscopy (TEM) micrographs show that some of the clay layers are dispersed homogeneously within the polymer matrix on the nano-scale, although some clay particles are agglomerated. We also found that the addition of only a small amount of organoclay is enough to improve the thermal stabilities and mechanical properties of the PET nanocomposite fibers. Even polymers with low organoclay content (<5 wt%) were found to exhibit much higher thermo-mechanical values than pure PET fibers.

• Polymer(Korea)
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• v.38 no.4
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• pp.510-517
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• 2014

A series of polyimide (PI) was prepared by reacting 4,4'-(hexafluoroisopropylidene)-diphthalic anhydride (6FDA) as the anhydride and bis(3-aminophenyl) sulfone (APS), bis[4-(3-aminophenoxy)-phenyl] sulfone (BAPS), 2,2-bis(4-aminophenyl)-hexafluoropropane (6FPD), 2,2-bis[4-(4-aminophenoxy)-phenyl]hexafluoropropane (6FBAPP), 2,2'-bis(trifluoromethyl)benzidine (TFDB), or 1,4-phenylenediamine (PDA) as the diamine. Residual stress behaviors were detected in-situ during thermal imidization of the polyimide precursors using a thin film stress analyzer (TFSA), and interpreted with respect to their morphology. According to the molecular orientation and packing order, the residual stress varied from 23.1 to 12.5 MPa, decreased with increasing chain rigidity. The thermal properties of the PI films were investigated using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and thermomechanical analysis (TMA). Their optical properties were measured by ultraviolet-visible spectrophotometer (UV-vis), and spectrophotometry. The properties of PI films were found to be strongly dependent upon the morphological structure. However, trade-offs between residual stress and optical properties were identified.

• Applied Chemistry for Engineering
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• v.26 no.6
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• pp.698-705
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• 2015

Two series of symmetric dimesogenic compounds containing a butylene or 1-methylbutylene spacer as a flexible group were synthesized. The mesogenic groups of synthesized compounds consist of an azobenzene group with a terminal substituent. Chemical structures as well as, thermal, mesomorphic, and photochemical properties of the synthesized compounds were investigated using FT-IR, $^1H-NMR$, differential scanning calorimetry (DSC), polarizing optical microscopy (POM), and UV-visible spectrometry. P-H, P-F, and $P-OC_6H_{13}$ showed monotropic liquid crystal phases, whereas the others showed enantiotropic liquid crystal phases. Compounds with butylene group as a flexible spacer exhibited wider mesophase temperature ranges and higher thermal transition temperatures than compounds containing a 1-methylbutylene group. Compounds with a high absolute value of the Hammett substituent constant exhibited high thermal transition temperatures and improved stability in the liquid crystal phase. Furthermore, in the absence or presence of UV light illumination, terminal substituents of the azomesogenic group were important factors in deciding the maximum absorbance wavelength (${\lambda}_{max}$) and the rate of photoisomerization (K).

• Clean Technology
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• v.23 no.4
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• pp.378-387
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• 2017

To obtain epoxy resin with permanently attached flame-retardant groups, phosphorus compound containing di-hydroxyl group [10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-oxa-10-phospha phenanthrene-10-oxide, DOPO-HQ] and silicone compound containing di-hydroxyl group (polydimethylsiloxane, hydroxyl terminated, PDMS) were reacted with uncured epoxy prepolymer (diglycidyl ether of bisphenol A, DGEBA) and then cured using 4,4-diaminodiphenylmethane (DDM) as a crosslinking agent. The properties of the resulting epoxy materials were characterized using Fourier transform infrared (FTIR) spectrometer, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), limiting oxygen index (LOI) test/vertical burning test (UL 94-V test), tensile properties test and impact test. This study examined the effect of phosphorus/silicone compound contents on the thermal/mechanical properties and flame retardancy of cured epoxy resins containing phosphorus and silicone compounds. It was found that the thermal/mechanical properties of epoxy resins containing phosphorus and silicone components were higher than those of simple epoxy resin. The flame-retardancy (LOI: 29.9 ~ 31.8% and UL 94-V: V-0) of all samples containing phosphorus compound and phosphrous compound/silicone compound was found to be passed the flame-retardant requirements (LOI: > 30%, UL 94-V: V-0) of LOI and vertical burning tests. However, the flame-retardancy (LOI: 21.4% and UL 94-V: no rating) of simple epoxy resin was found to be failed the flame-retardant requirements.

• YAKHAK HOEJI
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• v.56 no.3
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• pp.164-172
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• 2012

This study was aimed to increase the solubility, dissolution and permeation rates of atorvastatin calcium (ATC) using bile salt and/or 2-hydroxypropyl-${\beta}$-cyclodextrin ($HP{\beta}CD$). From solubility studies, sodium deoxycholate (SDC) among bile salts studied was found to have the highest solubilizing effect on ATC ($4.4{\pm}0.4$ mg/ml), and the order of increasing solubility was SDC>sod. cholate>sod. glycocholate>sod. taurodeoxycholate>sod. taurocholate>conjugated bile acid. ATC solid dispersions were prepared at various ratios of drug to SDC and/or $HP{\beta}CD$, and evaluated by differential scanning calorimetry (DSC), dissolution studies and dissolution-permeation studies. DSC curves showed amorphous state of ATC in the physical mixture and solid dispersion. Dissolution rates of ATC-SDC solid dispersions and physical mixture were markedly increased at pH 6.8, but decreased at pH 1.2 with greater proportions of SDC due to the precipitation of SDC, compared with that of drug alone. On the other hand, dissolution rates of ATC-$HP{\beta}CD$ solid dispersion and physical mixture at pH 1.2 were varied with the ratio of drug to carriers. From duodenal permeation studies, it was found that fluxes of ATC (donor dose: 0.5 mg/3.5 ml) in the presence of 25 mM sodium glycocholate, SDC, sod. cholate and sod. taurocholate $(5.7{\pm}0.9$, $5.6{\pm}0.9$, $4.8{\pm}0.7$ and $4.6{\pm}0.9\;{\mu}g/cm^2/hr$, respectively) were enhanced, compared with drug alone ($3.4{\pm}0.9\;{\mu}g/cm^2/hr$). In the dissolution-permeation studies, 1 : 9 : 10 (w/w) ATC-SDC-$HP{\beta}CD$ solid dispersion increased the flux 2.2 times, compared with 1 : 5 : 4 (w/w) ATC-lactose-corn starch mixture as control. In conclusion, solid dispersions with bile salt and $HP{\beta}CD$ were found to be an effective means for increasing the dissolution and permeation rates of ATC.

• Applied Chemistry for Engineering
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• v.28 no.2
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• pp.237-244
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• 2017

Hyperbranched liquid crystalline polymers with azomesogenic and cholesteryl groups in their terminal positions were designed and synthesized by direct polycondensation reaction. The chemical structures and thermal and mesomorphic properties of the synthesized polymers were investigated by FT-IR, $^1H-NMR$, differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), and polarizing optical microscopy (POM). The inherent viscosities (${\eta}_{inh}$) of the polymers were measured to be between 0.30 and 0.50 dL/g in phenol/p-chlorophenol/1,1,2,2-tetrachloroethane (25/40/35 = w/w/w). The degree of branching (DB) in these polymers ranged from 0.37 to 0.75; they, as amorphous polymer, showed glass transition temperatures ranging from 80 to $120^{\circ}C$; the polymers readily dissolved in most of the organic solvents used in the experiments. Only hyperbranched polymers with a cholesteryl group as their mesogenic group showed liquid crystalline phases.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.10
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• pp.69-74
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• 2017

In this study, cholesteryl 4-n-alkoxybenzoates (Chol-n), with alkyl groups used for controlling the temperature of transition to the liquid crystal phase, were synthesized, and the effects of the length of the alkyl groups on the physical properties of the liquid crystal compounds were investigated. The chemical structures and thermal and liquid crystalline properties of the synthesized compounds were investigated by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy ($^1H$-NMR), differential scanning calorimetry (DSC), and polarizing optical microscopy (POM). The synthesized compounds showed melting transition temperatures ($T_m$) in the range of $103^{\circ}C$ to $143^{\circ}C$ and all of the compounds except Chol-6 exhibited a wide liquid crystal phase temperature range of about $60^{\circ}C$ to $100^{\circ}C$. No correlation between the number of carbon atoms in the molecule and the thermal properties of the compounds was found. All of the synthesized compounds showed an enantiotropic cholesteric phase, which was accompanied by a chiral smectic phase in the compounds Chol-6, Chol-8, Chol-9, and Chol-10. All of the compounds exhibited thermochromism in the liquid crystal state, and their color changed from red to blue as the temperature was increased.

• Membrane Journal
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• v.21 no.3
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• pp.222-228
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• 2011

Poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) graft copolymer was synthesized via atom transfer radical polymerization (ATRP) and used as an electrolyte for electrochromic device. Plasticized polymer electrolytes were prepared by the introduction of propylene carbonate (PC)/ethylene carbonate (EC) mixture as a plasticizer. The effect of salt was systematically investigated using lithium tetrafluoroborate ($LiBF_4$), lithium perchlorate ($LiClO_4$), lithium iodide (LiI) and lithium bistrifluoromethanesulfonimide (LiTFSI). Wide angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) measurements showed that the structure and glass transition temperature ($T_g$) of polymer electrolytes were changed due to the coordinative interactions between the ether oxygens of POEM and the lithium salts, as supported by FT-IR spectroscopy. Transmission electron microscopy (TEM) showed that the microphase-separated structure of PVC-g-POEM was not greatly disrupted by the introduction of PC/EC and lithium salt. The plasticized polymer electrolyte was applied to the electrochromic device employing poly(3-hexylthiophene) (P3HT) conducting polymer.