• Title/Summary/Keyword: Ir-complexes

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Development of Separation and Trace Analysis Methods for Platinum Group Elements-Separation and Retention Behavior of Platinoid Metal Acetylacetonates in Reversed-Phase Liquid Chromatography (백금족 원소의 분리 및 미량분석법 개발에 관한 연구: 역상 액체 크로마토그래피에 의한 백금족 금속-아세틸아세톤 킬레이트들의 분리 및 머무름 거동)

  • Lee, Dai Woon;Kim, Kyung Soo;Park, Young Hun;Czea, Myoung Zoon;Chung, Koo Soon
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.107-119
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    • 1993
  • The purpose of this study is to investigated the elution behavior of platinoid metal acetylacetonates, which is the key to elucidate their retention mechanism and optimize their RPLC separation conditions. The retention data of four platinoid metal acetylacetonates have been measured on four different columns in methanol-water and acetonitrile-water systems. The retention of uncharged platinoid metal acetylacetonates is interpreted by solvophobic effect. The retention of platinoid metal acetylacetonates is also greatly influenced by the geometric structure of the complexes. The square planar chelates, $Pd(acac)_2$, $Pt(acac)_2$, are retained longer than the octahedral chelates, $Rh(acac)_3$, $Ir(acac)_3$. It is likely due to that square planar chelates show greater interaction with nonpolar stationary phase than octahedral chelates. The results of van't Hoff plots have shown that platinoid metal acetylacetonates is operated on the same retention mechanism in the temperature range of $25{\sim}45^{\circ}C$. The study of the retention mechanism by the enthalpy-entropy compensation phenomenon has indicated that the retention mechanism of octahedral chelates and square planar chelates do not vary with the composition change of methanol-water mobile phase, respectively. In acetonitrile-water mobile phase, however, the retention mechanism is observed to be more complicated. Optimum condition for the separation of four platinoid metal acetylacetonates is found to be 40% methanol, polymeric C18 column, and $45^{\circ}C$.

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Plasminogen Activator Inhibitor Type 1 Gene Polymorphism in Patients with Minimal Change Nephrotic Syndrome (소아 신증후군 환자에서 Plasminogen Activator Inhibitor Type 1 유전자 다형성)

  • Kim Young-Min;Hong Hyun-Kee;Kim Sung-Do;Cho Byoung-Soo
    • Childhood Kidney Diseases
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    • v.8 no.1
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    • pp.26-32
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    • 2004
  • Purpose : Hypercoagulability is present in patients with nephrotic syndrome. Plasminogen activator inhibitor type 1(PAI-1) is a major inhibitor of plasminogen activators. PAI-1 inactivates both tissue plasminogen activator(tPA) and urokinase plasminogen activator(uPA) by rapid formation of inactive 1:1 stoichiometric complexes. Recently some studies showed that the enhanced PAI-1 expression may be involved in the intraglomerular fibrinogen/fibrinrelated antigen deposition seen in nephrotic syndrome. Methods : PAI-1 gene promoter -844(G/A) polymorphism was evaluated in 146 children with minimal change nephrotic syndrome(MCNS) and 230 control subjects. The patients with MCNS were subdivided into 85 infrequent-relapser(IR) group and 61 frequent relapser(FR) group. PCR of PAI-1 gene promoter region including -844(G/A) and RFLP using the restriction enzyme Xhol were performed for each DNA samples extracted from the groups. Results : The distribution of PAI-1 genotype in the control group was G/G 81(32.5%), A/A 42(16.9%), and G/A 126(50.6%). The distribution of PAI-1 genotypes in the IR group of MCNS was G/G 29(34.1%), A/A 15(17.7%), and G/A 41(48.2%). The distribution of PAI-1 genotype in the FR group of MCNS was G/G 17(27.9%), A/A 18(29.5%), and G/A 26(42.6%). There was a significantly increased frequency of A/A genotype(P=0.0251) in the FR group of MCNS. Conclusion : Our results indicate that the PAI-1 gene promoter A/A genotype may be associated with the FR in MCNS.

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Spectroscopic and Thermal Studies of [Cr2(NH2)2(H2O)2(SO4)2]·2H2O,[Cr(NCO)3(H2O)]·3H2O and [Fe O(OH)]·0.2H2O Compounds Formed by the Reactions of Urea with Cr2(SO4)3, Cr(CH3COO)3 AND Fe2(SO4)3

  • Sadeek, S.A.;Refat, M.S.;Teleb, S.M.
    • Journal of the Korean Chemical Society
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    • v.48 no.4
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    • pp.358-366
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    • 2004
  • The bridged disulphato complex $[Cr_2(NH_2)_2(H_2O)_2(SO_4)_2]{\cdot}2H_2O$, terminal triisocyanato $[Cr(NCO)_3(H_2O)]{\cdot}3H_2O$ complex and limonite, $[FeO(OH)]{\cdot}0.2H_2O$ compound were prepared by the reaction of $Cr_2(SO_4)_3{\cdot}xH_2O, Cr(CH_3COO)_3$ and $Fe_2(SO_4)_3$, respectively, with urea in aqueous media at $80^{\circ}C$. The infrared spectra of the products indicate that the absence of the bands of urea, but shows the characteristic bands of coordinated amide, water, bridged sulphato and isocyanato groups. Thermogravimetric (TG) and differential thermal analysis (DTA) measurements on the complexes are also recorded. The data obtained agree quite well with the expected structures. A general mechanisms describing the formation and its thermal decomposition of the complexes are suggested.

Preparation of PEG-Folate-graft-Polyethylenimine as a Gene Carrier (유전자 전달체로서 폴리(에틸렌 글리콜) 및 폴레이트로 수식된 폴리(에틸렌 이민)의 합성)

  • Seo Dong Hoan;Kim Seon Hwa;Khang GilSon;Chi Sang Cheol;Shin Byung Cheol;Kim Moon Suk
    • Polymer(Korea)
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    • v.29 no.2
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    • pp.135-139
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    • 2005
  • In this study, poly(ethylene imine) (PEI) modified by methoxypoly(ethylene glycol) (mPEG) and folate as a gene carrier was synthesized to decrease cytotoxicity and to improve in vivo targeting. mPEG was modified by glutaric anhydride (GA) to endow carboxylic end group, followed by the activation reaction with EDC (N-ethyl-N'-(3-dimethyl-aminopropyl) carbodiimide) and NHS (N-hydroxysuccinimide). The activated carboxylic end group of mPEG was reacted with the amines of PEI to give mPEG graft PEI. The mPEG-folate-graft-PEI was synthesized by the reaction of mPEG-PEI with folate pre-activated by EDC/NHS. The obtained copolymers were characterized by $^1H-NMR$ and FT-IR. Gel retardation assay and fluorescence measurement indicated that DNA formed the complexes with the synthesized copolymers above N/P charge ratio 2. The size of complexes was ranging from 100 nm to 300 m. In conclusion, we confirmed that the synthesized copolymer have the possibility as a DNA carrier.

Synthesis of New N2O Tridentate Ligands and Their Stability Constants of Transition Metal Complexes (새로운 N2O계 세 자리 리간드의 합성과 전이금속 착물 안정도상수)

  • Kim, Sun-Deuk;Park, Young-Sik
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.569-577
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    • 2003
  • Ligands, Br-PEMP, Cl-PEMP and $CH_3O-PEMP$ having Br, Cl and $CH_3O$ substituents at 5-position of the $N_2O$ tridentate ligand, 2-[(2-pyridine-2-ethylamio)-methyl]-phenol (H-PEMP) containing pyridine and phenol were synthesized. Another ligand, Naph-PEMP having pyridine and 2-hydroxy-1-naphthalene was also synthesized. The ligands were characterized using elemental analysis, UV-visible, IR, $^1H\;NMR\;and\;^{13}C$ NMR spectroscopy and mass analysis. The potentiometric titration study in aqueous solution revealed that the proton dissociation of the ligands occurred in three steps and the order of overall proton dissociation constants (log${\beta}$) was $CH_3O-PEMP$ > Naph-PEMP > H-PEMP > Cl-PEMP > Br-PEMP. The order of stability constants (logML and log$ML_2$) of their transition metal complexes was Co(II) < Ni(II) < Cu(II) > Zn(II). The order in their stability constants values of each transition metal complex agreed well with that in overall proton dissociation constant value of the ligands.

Study on the Purification of 5'-Ribonucleotide (5'-Ribonucleotide의 분리(分離) 정제(精製)에 관(關)한 연구(硏究))

  • Ryung, Young;Choi, Sung-Kwan;Chung, Kab-Teack
    • Korean Journal of Food Science and Technology
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    • v.16 no.3
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    • pp.368-374
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    • 1984
  • The purification of 5'-riboncleotide using ion exchange resins has been studied and the optimum conditions were determined. The amount used of Amberlite IR120 ion exchange resin in 2nd resin tower could be reduced up to 20% by pretreating the hydrolyzed RNA solution in 1st resin tower. The amount used of regenerant could be also reduced up to 20% by desalting the hydrolyzed RNA solution in the 1st tower, because the desalted solution eluted easily by the water in the 2nd tower. The crystal obtained in this experiment was the mixed-crystals of $5'-IMP.Na_2\;and\;5'-GMP.Na_2$. The crystallization of the complexes formed from $5'-IMP.Na_2\;and\;5'-GMP.Na_2$ gave the best result at pH 7.6. The yield of crystal complexes formed from $5'-IMP.Na_2\;and\;5'-GMP.Na_2$ was obtained higher in high MeOH concentration. However, in higher than 60% MeOH concentration the products was amorphous. The higher content of MeOH for the crystallization of the product gave the smaller value of $5'-IMP.Na_{2}/5'-GMP.Na_2$.

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Theoretical Investigation for the Molecular Structures and Dimerization Energies for Complexes of H2O-C6H6 Dimer (물(H2O)과 벤젠(C6H6) 이합체의 분자 구조 및 결합 에너지에 관한 이론 연구)

  • Sun, Ju-Yong;Kim, Seung-Joon
    • Journal of the Korean Chemical Society
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    • v.53 no.1
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    • pp.7-16
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    • 2009
  • The global minimum structures of the benzene-water, Bz-$H_2O$ and benzene-water cation complex, [Bz-$H_2O]^+$ have been investigated using ab initio and density functional theory(DFT) with very large basis sets. The highest levels of theory employed in this study are B3LYP/cc-pVQZ for geometry optimization and MP2/aug-cc-pVTZ//B3LYP/aug-cc-pVTZ for binding energy. The harmonic vibrational frequencies and IR intensities are also determined at the various levels of theory to confirm whether the structure of water complex is affected by the presence of benzene. The binding energies of Bz-$H_2O$ (N-1) structure are predicted to be 3.92 kcal/mol ($D_e$) and 3.11 kcal/mol ($D_0$) after the zero-point vibrational energy correction at the MP2/cc-pVQZ//B3LYP/cc-pVQZ level of theory. The binding energies of [Bz-$H_2O]^+$ (C-1) structure are predicted to be 9.06 kcal/mol for $D_e$ and 7.82 kcal/mol for $D_0$ at the same level of theory.

Antitumor Activity and Nephrotoxicity of the Novel Platinum(II) Coordination Complex (새로운 Platinum (II) Complex [Pt (II)(trans-d-dach)(DPPE)] $(NO_3)_2$의 항암효과 및 신독성에 관한 연구)

  • Jung Jee-Chang;Lee Moon-Ho;Chang Sung-Goo;Rho Young-Soo
    • The Korean Journal of Pharmacology
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    • v.31 no.1 s.57
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    • pp.103-114
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    • 1995
  • Platinum coordination complexes are currently one of the most compounds used in the treatment of solid tumors. However, its use is limited by severe side effects such as renal toxicity. Our platinum-based drug discovery program is aimed at developing drugs capable of diminishing toxicity and improving antitumor activity. We synthesized new Pt (Ⅱ) complex analogue containing 1,2-diaminocyclohexane (dach) as carrier ligand and 1,2-bis(diphenylphosphino) ethane (DPPE) as a leaving group. Furthermore, nitrate was added to improve the solubility. A new series of [Pt(trans-ddach)(DPPE).$2NO_3(PC)$ was synthesized and characterized by their elemental analysis and by various spectroscopic techniques [infrared (IR), $^{13}carbon$ nuclear magnetic resonance (NMR)]. PC demonstrated acceptable antitumor activity aganist P388, L-1210 lymphocytic leukemia cells and SK=OV3 human ovarian adenocarcinoma cells, and significant. activity as compared with that. cisplatin. The toxicity of PC was found quite less than thar of cisplatin using MTT, $[^3H]$ thymidine uptake and glucose consumption tests in rabbit proximal tubule cells, human kidney cortical cells and human renal cortical tissues. Based on these results, this novel platinum compound represent a valuable lead in the development of a new anticancer chemotherapeutic agent capable of improving antitumor activity and low toxicity.

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Formation of Complex Between Polyelectrolytes and pH/Temperature Sensitive Copolymers (고분자전해질과 pH/온도감응성 고분자 사이의 복합체 형성에 관한 연구)

  • Yoo, Mi Kyong;Sung, Yong Kiel
    • Journal of the Korean Chemical Society
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    • v.42 no.1
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    • pp.84-91
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    • 1998
  • Random copolymers of N-isopropyl acrylamide (NIPAAm) and acrylic acid (AAc) which exhibit temperature- and pH-responsive behavior were synthesized by free-radical polymerization. The copolymers were characterized by means of FT-IR spectrometry and titration. The influence of polyelectrolyte on the lower critical solution temperature (LCST) of pH/temperature-sensitive polymers was investigated in the pH range of 2-12. The LCSTs of PNIPAAm/water in poly(NIPAAm-co-AAc) were determined by cloud-point measurements. A polyelectrolyte complex was prepared by mixing poly(NIPAAm-co-AAc) with poly(allylamine) (PAA) or poly(L-lysine) (PLL) solutions as anionic and cationic polyelectrolytes, respectively. Back titration was performed to determine the content of AAc and to study the effect of comonomer ionization on the LCST. The LCSTs of PNIPAAm/water in the copolymers were strongly affected by pH, presence of polyelectrolyte, AAc content, and charge density on the polymer. The polyelectrolyte complexes were formed at neutral condition. The influence of more hydrophobic PLL as polyelectrolyte on the cloud-point of PNIPAAm/water in the copolymer was stronger than that of poly(allylamine) (PAA).

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Analysis of adsorption behavior of lead ion on to surface modified AlPO4 materials (표면처리된 AlPO4에 대한 납 이온의 흡착 거동 분석)

  • Kim, Young-Ho;Kil, Hyun-Suk;Kang, Kwang-Cheol;Choi, Suk-Nam;Rhee, Seog-Woo
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.275-281
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    • 2011
  • $AlPO_4$-type material was synthesized by a reaction of $Al(OH)_3$ and H3PO4 with organic templates from wastewater of detergent manufacturer. The surface of material was coated with carboxylate groups by the reaction of succinic anhydride with surface amino groups which were formed by treatment of the material with APTMS. Powder XRD patterns showed the characteristic patterns of $AlPO_4$. Morphology of the material was examined using a SEM and the functional groups were investigated by FT-IR analysis. The surface charge of a aqueous suspension was analyzed: $AlPO_4-NH_2$ has positively charged surface while $AlPO_4$-COOH has negatively charged one. They were used for the removal of toxic metals from aqueous solution. The lead ions were adsorbed on the surface by the formation of complexes with carboxylate of surface and $K_d$ was 91.1 mL/g. In conclusion, the $AlPO_4$-COOH might be applicable in the removal of toxic metal ions from aqueous system.