• Title/Summary/Keyword: XRPD

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Polymorphism of Q-35 (Balofloxacin) (Q-35(발오플록사신)의 결정다형)

  • Sohn, Young-Taek;Chun, He-Ryun
    • Journal of Pharmaceutical Investigation
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    • v.31 no.2
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    • pp.119-123
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    • 2001
  • Six polymorphic modifications of Balofloxacin (Q-35) were obtained by the recrystallization from different organic solvents and characterized by differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD). The dissolution patterns of these six modifications were also checked in distilled water at $37{\pm}0.5^{\circ}C$, 50 rpm for 60 minutes. The polymorphic modifications showed significant differences in the dissolution rate. The dissolution rate of Mod. 1 was faster than that of other polymorphic modifications. The transformation during storage was also studied.

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Crystal Form of A Camptothecin Derivative (Camptothecin 유도체의 결정형)

  • Sohn, Young-Taek;Moon, Hyun-Young
    • Journal of Pharmaceutical Investigation
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    • v.32 no.2
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    • pp.81-85
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    • 2002
  • Three polymorphic modifications of CKD-602, water soluble derivative of camptothecin, were obtained by the recrystallization from different organic solvents and characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and X-ray powder diffraction (XRPD). The major endothermic peaks of the DSC curve of Form 1, Form 2 and Form 3 was shown at $268.71^{\circ}C$, $247.83^{\circ}C$, $244.76^{\circ}C$, respectively. Form 2 was elucidated to be an acetic acid solvate and Form 3 was elucidated to be a methanol solvate. The dissolution patterns of these three modifications were also checked in distilled water at $37{\pm}0.5^{\circ}C$, for 30 minutes. The polymorphic modifications showed differences in the dissolution rate. The dissolution rate of Form 1 was faster than that of other polymorphic modifications. When stored at different relative humidity over the period of 3 months, all of the polymorphic modifications did not undergo transformation.

Polymorphic Forms of Furosemide Characterized by THz Time Domain Spectroscopy

  • Ge, Min;Liu, Guifeng;Ma, Shihua;Wang, Wenfeng
    • Bulletin of the Korean Chemical Society
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    • v.30 no.10
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    • pp.2265-2268
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    • 2009
  • Terahertz time domain spectroscopy (THz-TDS) is applied in transmission to identify the five forms of modifications of furosemide and one commercial product from 0.3 THz to 1.6 THz at room temperature. The different absorption spectra of the different forms are sensitive to crystal structures. Density function theory (DFT) calculation was used to understand the vibrational modes of furosemide in the THz region. X-ray powder diffractometry (XRPD) was applied to confirm the different forms of modifications. The results demonstrate that THz-TDS is a potential analytical technique in investigating polymorphic forms in the pharmaceutical fields.

Photo-induced Isomerization and Polymerization of (Z,Z)-Muconate Anion in the Gallery Space of [LiAl2(OH)6]+ Layers

  • Rhee, Seog-Woo;Jung, Duk-Young
    • Bulletin of the Korean Chemical Society
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    • v.23 no.1
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    • pp.35-40
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    • 2002
  • Photoreaction of guest organic anions in layered organic-inorganic hybrid materials was investigated. The layered hybrids were synthesized by an anion-exchange reaction of $[LiAl_2(OH)_6]Cl{\cdot}yH_2O$ layered double hydroxide with aqueous (Z,Z)- and (E,E)-muconates under inert atmospheric condition, to give new organicinorganic hybrids of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$ and $[LiAl_2(OH)_6]_2[(E,E)-C_6H_4O_4]{\cdot}H_2O$, respectively. The basal spacings calculated by XRPD of intercalates indicate that muconate anions have almost vertical arrangements against the host $[LiAl_2(OH)_6]^+$ lattices in the interlayer of organic-inorganic hybrid materials. When UV light was irradiated on the suspension of $[LiAl_2(OH)_6]_2[(Z,Z)-C_6H_4O_4]{\cdot}zH_2O$, the (Z,Z)-muconate anions of the gallery space of hybrids were polymerized in the aqueous media while it was isomerized into more stable (E,E)-muconate in the methanollic suspension in the presence of catalytic amount of molecular iodine. All the products were characterized using elemental analysis, TGA, XRPD, FT-IR, $^1H$ NMR and $^{13}C$ CP-MAS NMR.

Preperation and Struction of a 3-Dimensional Nickel(II) Coordination Polymer

  • 한원석;이순원
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.28-28
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    • 2002
  • The hydrothermal reaction of Ni(NO₃)·6H₂O with 4.4'-oxybis(benzoic acid) (OBCH₂) and trans-1,2-bis(4-pyridyl)ethylene (bipyen) led to the formation of a 3-dimensional coordination polymer with the empirical formular of [Ni(OBC)(bipyen)]·H₂O. The complex has been characterized by X-ray diffraction, elemental analysis, TGA, IR, X-ray power diffraction (XRPD), It crystallized triclinic space group P1 with a = 9.280(2)Å., b = 11.317(4) Å, c = 12.442(3) Å, Z = 2, R (ωR₂) = 0.0346 (0.0846).

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One-Pot Synthesis, Crystal Structures and Thermal Properties of Two Three-Dimensional Cobalt(II) Complexes

  • Tao, Bo;Lei, Wen;Cheng, Feiran;Xia, Hua
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1929-1933
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    • 2012
  • Two cobalt(II) compounds $[Co(2,2{^\prime}-bipy)(H_2O)_2(SO_4)]_n$ (1) and $[Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6]{\cdot}2H_2O$ (2) (2,2'-bipy = 2,2'-bipyridine, $H_4btec$ = 1,2,4,5-benzenetetracarboxylic acid), have been simultaneously synthesized by a one-pot slow solvent evaporation reaction. Their structures were determined by single-crystal X-ray diffraction and further characterized by X-ray powder diffraction (XRPD), IR, elemental and thermogravimetric analysis (TGA). The structural analysis reveals that compound 1 exhibits an infinite 1D chain structure with the octahedral Co(II) centers bridging by the tetrahedral ${\mu}_2-SO{_4}^{2-}$ ligands, while compound 2 possesses a dinuclear $Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6$ unit and the two adjacent octahedral Co(II) ions are linked by the bismonodentately coordinated btec ligand. Additionally, compound 2 exhibits blue fluorescent emission in the solid state at room temperature.

Synthesis and Infrared Light Reflecting Characteristics of TiO2/Mica Hybrid Composites (이산화 티타늄/마이카 복합 재료의 적외선 광반사 특성)

  • Kil, Hyun Suk;Rhee, Seog Woo
    • Applied Chemistry for Engineering
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    • v.27 no.1
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    • pp.16-20
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    • 2016
  • In this work, we describe the synthesis and infrared light reflecting characteristics of $TiO_2$/mica hybrid composites. $TiO_2$/mica composite materials were obtained by the hydrolysis and condensation reaction of titanium isopropoxide in an aqueous solution of acetic acid in the presence of mica particles. Amorphous phase of $TiO_2$ on the surface of mica was converted to the crystalline rutile phase via anatase phase by heat treatment ($600-1000^{\circ}C$, 1-3 h) of $TiO_2$/mica composite materials, and the size of crystals was controlled by heat treatment conditions. Physicochemical properties of mica and $TiO_2$/mica composites were investigated using FE-SEM, ED-XRF, and PXRD. The solar reflectance of $TiO_2$/mica composites in the near IR region (780~2,500 nm) measured using a diffuse reflectance NIR spectrophotometer was 88.6%, which is rather higher than that of calcined pure mica (86.6%). Therefore, $TiO_2$/mica composites can be used as NIR light reflective pigments.