• Journal of the Korean Chemical Society
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• v.63 no.1
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• pp.7-11
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• 2019

Olmutinib, N-[3-({2-[4-(4-methylpiperazine-1-yl)aniline]thieno[3,2-d]Pyrimidin-4-yl}oxy)phenyl]prop-2-enamide dihydrochloride monohydrate, $Olita^{TM}$ is an oral, third-generation epidermal growth factor receptor tyrosine kinase inhibitor (EGFR TKI) that was developed by Boehringer Ingelheim and Hanmi Pharmaceutical Co. Ltd for the treatment of non-small cell lung cancer (NSCLC). The aim of this work was to investigate the existence of polymorphs and pseudopolymorphs of olmutinib. Three crystal forms of olmutinib have been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). From the DSC and TG data it was confirmed that Form 1 is monohydrate, Form 2 is dihydrate, Form 3 is 1.5 hydrate. The PXRD patterns of three crystal forms were different respectively. After storage of 1 month at $2^{\circ}C$, 24% RH (Relative Humidity), Form 1, Form 2, and Form 3 were not transformed.

• Archives of Pharmacal Research
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• v.28 no.6
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• pp.730-735
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• 2005

Nine polymorphic modifications of doxazosin mesylate have been obtained by recrystallization in organic solvents under variable conditions. Different polymorphs of doxazosin mesylate were characterized by powder X-ray crystallography diffractometry (PXRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). Transformation of Form 1 and Form 2 was not occurred in three relative humidities ($0\%$, $51\%$, and $99\%$) at 20$\pm$0.5 for 30 days.

• Journal of Pharmaceutical Investigation
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• v.41 no.6
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• pp.371-376
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• 2011

The objective of this work was to investigate the existence of new crystal forms of tulobuterol which is used to prevent morning asthma attacks by ${\beta}_2$ agonist and the transformation of crystal forms. Three crystal forms of tulobuterol have been isolated by recrystallization and Form 2 was transformed to Form 4 at 52% RH and 95% RH and these four crystal forms are characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). The DSC and PXRD patterns of four crystal forms of tulobuterol were different respectively. The dissolution patterns of these three crystal forms of tulobuterol were studied and they showed significant differences in the dissolution rate. After storage of 2 months at 0% RH (silica gel, $20^{\circ}C$), 52% RH (saturated solution of $Na_2Cr_2O_7{\cdot}2H_2O/20^{\circ}C$) and 95% RH (saturated solution of $Na_2HPO_4/20^{\circ}C$), Form 1 and Form 3 were not transformed. But Form 2 was transformed to Form 4 at 52% RH and 95% RH.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.44 no.4
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• pp.43-50
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• 2012

The crystallinity index is an important characteristic of cellulose. The crystallinity value is different depending on the adopted instrument. In this study, we determined a crystallinity index of cotton and wood celluloses using wide-angle X-ray scattering (WAXS), powder X-ray diffractometer (PXRD), and cross polarization/magic angle spinning solid-state $^{13}C$ nuclear magnetic resonance spectroscopy (CP/MAS solid-state $^{13}C$ NMR). The specimen was prepared in forms of powder, sheet and pallet. With the comparison of the obtained crystallinity indices of the cellulose, the effects of the analysis instrument, the sample preparation and analysis method were investigated. Among three instruments, the crystallinity indices by PXRD and NMR had a good relationship and reproducibility, and WAXS gave the crystallinity index with poor reproducibility. In the case of analysis methods of crystallinity indices, the Segal method showed higher value than that of the Ruland-Vonk method. We expect that this study would be applicable to evaluate the crystallinity index of various cellulose materials with accuracy and reproducibility.

• Journal of Pharmaceutical Investigation
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• v.39 no.3
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• pp.173-176
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• 2009

A new crystal form of valsartan dipotassium was isolated by recrystallization using the one-pot method. The new crystal form was identified as a monohydrate form ($C_{24}H_{27}N_5O_3K_2.H_2O$) and characterized by diffential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and X-ray powder diffractometry (PXRD). The new crystal data demonstrated to be clearly different from those known for the tetrahydrate form ($C_{24}H_{27}N_5O_3K_2.4H_2O$). It was observed that the monohydrate of vasartan dipotassium salt was completely dissolved in water within 1 hour and its dissolution rate was much faster than anhydrous free form of valsartan.

• Journal of Korean Society of Water and Wastewater
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• v.26 no.1
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• pp.149-157
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• 2012

Experiments for As(V) removal using synthesized $Ca{\cdot}Al$-monosulfate was performed from the water contaminated with arsenate. Monosulfate is known as LDHs (Layered Double Hydroxides) which is one of the anionic clay minerals. Monosulfate was synthesized mixing $C_3A$ (tricalcium aluminate), gypsum (calcium sulfate), and water with an intercalation method. The product form the synthesis was characterized by FE-SEM, WDXRF, PXRD, and FT-IR. Experiments with different doses of monosulfate were carried out for kinetic. As a result of experiment, the concentration of As(V) was reduced from 0.67 mM to 0.19 mM (0.67mM of monosulfate) and 0.178 mM (1.34 mM of monosulfate). The concentration of sulfate was increased with As(V) decrease. The result of PXRD showed that the d-spacing of inter layer ($d_{003}$ peak) was shifted from 8.927 ${\AA}$ to 8.095 ${\AA}$ because the sulfate in the inter layer of monosulfate was exchanged arsenate with water molecules bonded. From the FT-IR results, a new single band (800 cm-1) was observed after the reaction of monosulfate and As(V). The arsenic removal can be regarded as anion exchange mechanism that is one of the characteristics of LDHs from the results of PXRD and FT-IR analysis.

• Journal of the Korean Chemical Society
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• v.62 no.5
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• pp.352-357
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• 2018

Celecoxib (4-[5-(4-methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]benzenesulfonamide) is a cyclooxygenase-2 inhibitor used in the treatment of arthritis, acute pain, and dysmenorrhoea. Celecoxib is a Biopharmaceutics Classification System (BCS) class II compound whose oral bioavailability is highly limited owing to its poor aqueous solubility. Several polymorphs of celecoxib have been identified as Form I, Form II, and Form III with melting points of about $162.8^{\circ}C$, $161.5^{\circ}C$, and $160.8^{\circ}C$, respectively. Form IV was generated from the precipitated suspension in the presence of HPMC (Hydroxypropyl methylcellulose) and Polysorbate 80. A rapid rate of dissolution is useful because the rate of dissolution of a drug typically increases its bioavailability. The aim of this study was to investigate the possibility of production of new crystal form of celecoxib that has higher solubility than Form III. New crystal form of celecoxib (Form A) has been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). Form A was dissolved faster than Form III. At 30 minutes, the dissolution of Form A was 97.3%, whereas the dissolution of Form III was 82.2% (p < 0.1). After storage of three months at $20^{\circ}C$, in 24% RH (Relative Humidity), the crystal form was not transformed.

• Journal of Korean Society of Water and Wastewater
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• v.26 no.1
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• pp.141-148
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• 2012

The objective of this study is to remove arsenate from artificially contaminated wastewater using CaAl-ettringite and CaAl-monosulfate which were synthesized in laboratory. The study was carried on the basis of solidification/stabilization of waste using cement. Monosulfate and ettringite are constituents of cement paste. The CaAl-ettringite has a chemical formula of $Ca_6Al_2O_6(SO_4)_3{\cdot}32H_2O$ and has a needle like morphology. Whereas CaAl-monosulfate $Ca_4Al_2O_6(SO_4){\cdot}12H_2O$ has layered double hydroxide structure (LDH) in which the mainlayer consists of Ca and Al and S as interlayer. Ettringite and monosulfate were synthesized by reaction of tricalcium aluminate and gypsum and hydrating this mixture at elevated temperature. The synthesized mineral were characterized by PXRD and FESEM to ensure purity. It was found that concentrations of As(V) in contaminated water were reduced from initial concentration of 1.335 mmol/L to 0.054 mmol/L and 0.300 mmol/L by CaAl-monosulfate and CaAl-ettringite respectively. The post experimental results of PXRD and FESEM analysis indicate that arsenate removal was by ion exchange.

• Journal of Pharmaceutical Investigation
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• v.39 no.2
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• pp.117-120
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• 2009

Two crystal forms of ziprasidone have been isolated by recrystallization from different organic solvents and characterized by differential scanning calorimetry, powder X-ray diffractometry and thermogravimetric analysis. It was confirmed that Form 2 has the same crystal structure as Form 1.

• Journal of Pharmaceutical Investigation
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• v.41 no.4
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• pp.239-247
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• 2011

Simvastatin is an inhibitor of 3-hydroxy-3-methylglutaryl-coenzyme A (HMG-CoA) reductase, which catalyzes the conversion of HMG-CoA to mevalonate, an early and rate-limiting step in the biosynthesis of cholesterol. Simvastatin has good permeability, but it also has low solubility (BCS class II), which reduces its bioavailability. To overcome this problem, a solid dispersion is formed using a spray-dryer with polymeric material carrier to potentially enhance the dissolution rate and extend drug absorption. As carriers for solid dispersion, Gelucire$^{(R)}$44/14 and Gelucire$^{(R)}$ 50/13 are semisolid excipients that greatly improve the bioavailability of poorly-soluble drugs. To avoid any toxic effects of an organic solvent, we used aqueous medium to melt Tween$^{(R)}$ 80 and distilled water. The structural behaviors of the raw materials and the solid dispersion were analyzed by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). The DSC and PXRD data indicated that the crystalline structure of simvastatin was transformed to an amorphous structure through solid dispersion. Then, solid dispersion-based tablets containing 20 mg simvastatin were prepared with excipients. Dissolution tests were performed in distilled water and artificial intestinal fluid using the USP paddle II method. Compared with that of the commercial tablet (Zocor$^{(R)}$ 20 mg), the release of simvastatin from solid dispersion based-tablet was more efficient. Although the stability study is not complete, this solid dispersion system is expected to deliver poorly water-soluble drugs with enhanced bioavailability and less toxicity.