• 제목/요약/키워드: Electron paramagnetic resonance (EPR)

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Nd2XCd2-3XSiO4 (0.01≤X≤0.21) 고용체의 합성과 구조 규명 (Synthesis, Structure and Characterization of Nd2XCd2-3XSiO4 (0.01≤X≤0.21) Solid-Solutions)

  • Ramesh, S.;Das, B.B.
    • 대한화학회지
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    • 제55권3호
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    • pp.502-508
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    • 2011
  • [ $Nd_{2x}Cd_{2-3x}SiO_4$ ]($0.01{\leq}x{\leq}0.21$) [S1-S3: x=0.01, 0.11 and 0.21] 고용체를 졸-겔 방법을 통해 합성하였다. X선 분말회절(XRD) 측정은 $P2_1$/m 공간군의 단사정계를 보여준다. 평균 결정 크기는 20-45 nm이다. 주사전자현미경(SEM)으로 살펴본 모양은 구형의 특성을 보인다. 에너지 분산 X 선 분광기(EDS) 결과로부터 모든 구성 원소의 존재를 확인하였다. ~750 nm에서의 흡수 밴드는 $Nd^{3+}$ 이온의 $^4I_{9/2}{\rightarrow}^4F_{7/2}+^4S_{3/2}$ 전이에 기인한다. 10, 40, 77, 300 K에서 S1-S3의 전자 상자성 공명 (EPR) 선모양은 $Nd^{3+}$ 이온의 빠른 스핀 격자 이완에 기인하는 폭이 넓은 구분되지 않은 등방성의 선모양을 보여준다.

Inhibitory Effects of Exogenous Cu2+ and Zn2+ on the Cytochrome c Oxidase Activity

  • Min, Tong-Pil;Han, Sang-Hwa
    • BMB Reports
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    • 제28권4호
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    • pp.311-315
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    • 1995
  • Exogenous $Cu^{2+}$ or $Zn^{2+}$ at micromolar concentration had a strong inhibitory effect on detergent-solubilized cytochrome c oxidase. A similar effect was observed when $Cu^{2+}$ was added to vesicular cytochrome c oxidase, although the extent of inhibition was significantly larger for the uncoupled state than for the coupled state. Interestingly, the inhibition by $Zn^{2+}$ was almost negligible for both the coupled and uncoupled states. These results suggest that the binding sites for $Cu^{2+}$ ions are exposed to the extravesicular side. whereas those for $Zn^{2+}$ are exposed to the matrix side. The EPR spectra of bound $Cu^{2+}$ ions at 77 K indicate that each of the first two $Cu^{2+}$ ions is ligated by three or four histidine residues, as evidenced by distinct $^{14}N$ superhyperfine splitting. These $Cu^{2+}$ ions can not be removed readily by EDTA and inhibit the enzyme activity by as much as 80%.

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Cadaverine Protects Vibrio vulnificus from Superoxide Stress

  • Kang, In-Hye;Kim, Ju-Sim;Kim, Eui-Jin;Lee, Jeong
    • Journal of Microbiology and Biotechnology
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    • 제17권1호
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    • pp.176-179
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    • 2007
  • An electron paramagnetic resonance (EPR) signal characteristic of the 5,5'-dimethyl-l-pyrroline-N-oxide (DMPO)-OH spin adduct, which is formed from the reaction of DMPO with superoxide radicals generated by xanthine oxidasemediated reaction, was significantly reduced by the cadaverine or Escherichia coli Mn-containing superoxide dismutase (MnSOD). Likewise, cytochrome c reduction by superoxide was inhibited by cadaverine, and the inhibition level increased in proportion to the level of cadaverine. The cadA mutant of Vibrio vulnificus, which does not produce cadaverine because of the lack of lysine decarboxylase, exhibits less tolerance to superoxide stress in comparison with wild type. The results indicate that cadaverine scavenges superoxide radicals, and protects cells from oxidative stress.

SNARE Assembly and Membrane Fusion: A Paramagnetic Electron Magnetic Resonance Study

  • Kweon, Dae-Hyuk
    • 한국생물물리학회:학술대회논문집
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    • 한국생물물리학회 2003년도 정기총회 및 학술발표회
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    • pp.32-32
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    • 2003
  • In the neuron, SNARE (soluble N-ethylmaleimide-sensitive factor attachment protein receptors) assembly plays a central role in driving membrane fusion, a required process for neurotransmitter release. In the cytoplasm, vesicular SNARE VAMP2 (vesicle-associated membrane protein 2) engages with two plasma membrane SNAREs syntaxin 1A and SNAP-25 (synaptosome-associated protein of 25 kDa) to form the core complex that bridges two membranes. While various factors regulate SNARE assembly, the membrane also plays the regulatory role by trapping VAMP2 in the membrane. The fluorescence and EPR analyses revealed that the insertion of seven C-terminal core-forming residues into the membrane controls complex formation of the entire core region, even though preceding 54 core-forming residues are fully exposed and freely moving. When two interfacial Trp residues in this region were replaced with hydrophilic serine residues, the mutation supported rapid complex formation.

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EPR Studies of the Active Sites of Carbon Monoxide Dehydrogenase from Clostridium thermoaceticum

  • Shin, Woonsup;Lindahl, Paul A.
    • 분석과학
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    • 제8권4호
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    • pp.869-876
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    • 1995
  • The active sites of the nickel and iron-containing enzyme, carbon monoxide dehydrogenase (CODH) from clostridium thermoaceticum were investigated using Electron Paramagnetic Resonance (EPR) technique. CODH exhibits several spectral features called NiFeC, $g_{ave}=1.82$, $g_{ave}=1.86$. FCII signals which are originated from different clusters in this enzyme. CODH is know to catalyze two different kinds of reactions - acetyl-CoA synthesis and CO oxidation. The acetyl-CoA synthesis activity can be followed by monitoring CO/acetyl-CoA exchange. The addition of 1,10-phenanthroline (phen) to CODH selectively destroyed the CO/acetyl-CoA exchange activity and eliminated the NiFeC signal completely. CO oxidation activity and other EPR signals were unaffected. Such behavior demonstrates that CODH has two distinct active sites and that the NiFe complex is only responsible for the CO/acctyl-CoA exchange activity. Phen caused the removal of only 30% of Ni in the NiFe complex ($0.3Ni/{\alpha}{\beta}$) as shown by the quantitative metal analysis. The phen-treated CODH could be reactivated fully by incubation In $Ni^{2+}$ solution. Radioactive $^{63}Ni^{2+}$ was used to quantitate the amount of the $Ni^{2+}$ incorporated into phen-treated enzyme and showed that the amount was the same as the removed by the phen treatment. i.e. $0.3Ni/{\alpha}{\beta}$. This indicates that only 30% of NiFe complexes are labile and responsible for the CO/acctyl-CoA exchange activity, the other 70% are non-labile and have no exchange activity. This is the first clear evidence that the NiFe complex is heterogencous and labile and non-labile Ni sites arc interacting differently with substrates and chelating agents like phen.

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Formation of Au Particles in Cu2-xICu2IIO3-δ (x ≈ 0.20; δ ≈ 0.10) Oxide Matrix by Sol-Gel Growth

  • Das, Bidhu Bhusan;Palanisamy, Kuppan;venugopal, Potu;Sandeep, Eesam;Kumar, Karrothu Varun
    • 대한화학회지
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    • 제61권1호
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    • pp.29-33
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    • 2017
  • Formation of Au particles in nonstoichiometric $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxide from aniline + hydrochloric acid mixtures and chloroauric acid in the ratios 30 : 1; 60 : 1; 90 : 1 (S1-S3) by volume and 0.01 mol of copper acetate, $Cu(OCOCH_3)_2.H_2O$, in each case is performed by sol-gel growth. Powder x-ray diffraction (XRD) results show Au particles are dispersed in tetragonal nonstoichiometric dicopper (I) dicopper (II) oxides, $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$). Average crystallite sizes of Au particles determined using Scherrer equation are found to be in the approximate ranges ${\sim}85-140{\AA}$, ${\sim}85-150{\AA}$ and ${\sim}80-150{\AA}$ in S1-S3, respectively which indicate the formation of Au nano-micro size particles in $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Hysteresis behaviour at 300 K having low loop areas and magnetic susceptibility values ${\sim}5.835{\times}10^{-6}-9.889{\times}10^{-6}emu/gG$ in S1-S3 show weakly ferromagnetic nature of the samples. Broad and isotropic electron paramagnetic resonance (EPR) lineshapes of S1-S4 at 300, 77 and 8 K having $g_{iso}$-values ${\sim}2.053{\pm}0.008-2.304{\pm}0.008$ show rapid spin-lattice relaxation process in magnetic $Cu^{2+}$ ($3d^9$) sites as well as delocalized electrons in Au ($6s^1$) nano-micro size particles in the $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Broad and weak UV-Vis diffuse reflectance optical absorption band ~725 nm is assigned to $^2B_{1g}{\rightarrow}^2A_{1g}$ transitions, and the weak band ~470 nm is due to $^2B_{1g}{\rightarrow}^2E_g$ transitions from the ground state $^2B_{1g}$(${\mid}d_{x^2-y^2}$>) of $Cu^{2+}$ ($3d^9$) ions in octahedral coordination having tetragonal distortion.

Membrane Topology of Helix 0 of the Epsin N-terminal Homology Domain

  • Kweon, Dae-Hyuk;Shin, Yeon-Kyun;Shin, Jae Yoon;Lee, Jong-Hwa;Lee, Jung-Bok;Seo, Jin-Ho;Kim, Yong Sung
    • Molecules and Cells
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    • 제21권3호
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    • pp.428-435
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    • 2006
  • Specific interaction of the epsin N-terminal homology(ENTH) domain with the plasma membrane appears to bridge other related proteins to the specific regions of the membrane that are invaginated to form endocytic vesicles. An additional $\alpha$-helix, referred to as helix 0 (H0), is formed in the presence of the soluble ligand inositol-1,4,5-trisphosphate [$Ins(1,4,5)P_3$] at the N terminus of the ENTH domain (amino acid residues 3-15). The ENTH domain alone and full-length epsin cause tubulation of liposomes made of brain lipids. Thus, it is believed that H0 is membrane-inserted when it is coordinated with the phospholipid phosphatidylinositol-4,5-bisphosphate [$PtdIns(4,5)P_2$], resulting in membrane deformation as well as recruitment of accessory factors to the membrane. However, formation of H0 in a real biological membrane has not been demonstrated. In the present study, the membrane structure of H0 was determined by measurement of electron paramagnetic resonance (EPR) nitroxide accessibility. H0 was located at the phosphate head-group region of the membrane. Moreover, EPR line-shape analysis indicated that no pre-formed H0-like structure were present on normal acidic membranes. $PtdIns(4,5)P_2$ was necessary and sufficient for interaction of the H0 region with the membrane. H0 was stable only in the membrane. In conclusion, the H0 region of the ENTH domain has an intrinsic ability to form H0 in a $PtdIns(4,5)P_2$-containing membrane, perhaps functioning as a sensor of membrane patches enriched with $PtdIns(4,5)P_2$ that will initiate curvature to form endocytic vesicles.

${\gamma}$-선에 조사된 황산칼륨 단결정의 상자성 결함에 관한 전자스핀공명 연구 (ESR Study of Paramagnetic Defects of the ${\gamma}$-irradiated Potassium Sulfate Single Crystal)

  • 여철현;정원양;홍종인;김은옥;양정성
    • 대한화학회지
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    • 제25권6호
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    • pp.367-375
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    • 1981
  • 황산칼륨($K_2SO_4$) 포화용액으로부터 증발법으로 $K_2SO_4$ 단결정을 최적조건에서 생성시킨다. 이 단결정은 약 $12{\times}10^6$ 렌트켄의 ${\gamma}$-선에 조사시키면 그 결정내에 상자성 중심 또는 상자성 결합을 형성한다. 이 상자성 중심들의 전자스핀공명(ESR) 스펙트라를 상온에서 X-띠 전자스핀 공명 분광분석기로 얻는다. 상자성종들의 ESR 피이크들은 무등방성을 보이지만 $SO_3-$기만은 g = 2.0036인 가우스형 등방성 피이크이었다. 무등방성피이크들의 각도 의존성을 나타내기 위하여 서로 직교하는 a, b, c 결정축으로 단결정을 회전시키면서 여러 각도에서 ESR 스펙트라를 기록하였다. 무등방성 피이크들과 등방성 피이크의 선위치관계로부터 g값들을 계산하고 각 상자성 중심에 대응하는 g-값의 9매트릭스 원소들을 대각화 시켜 주 g-값과 방향여현을 얻는다. 이들 특성 주 g-값과 방향여현을 사용하여 모든 상자성 결합구조를 확인하였다.

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층상구조의 Na1.9Li0.1Ti3O7과 그 구리 혼입 유도체의 EPR 및 전기적 연구 (EPR and Electrical Studies in Layered Na1.9Li0.1Ti3O7 and its Copper Doped Derivatives)

  • Pal, D.;Chand, Prem;Tandon, R.P.;Shripal
    • 대한화학회지
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    • 제49권6호
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    • pp.560-566
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    • 2005
  • 순수한 또는 미량의 구리(몰 퍼센트(0.0$Na_{1.9}Li_{0.1}Ti_{3-X}Cu_XO_{7-X}$) 물질을 합성하였다. 상온에서 모든 구리 혼입 유도체와 다양한 낮은 온도에서 0.05몰 퍼센트 Cu 혼입 유도체의 EPR 특성을 조사하였다. 격자 안의 $Ti^{4+}$자리에 $Cu^{2+}$가 치환됨으로 인한 TiO6 팔면체의 찌그러짐이 나타났다. 또한, log(${\sigma}_{d.c.}T$) 대 1000/T 그래프를 통하여 세개의 특징적인 영역이 관찰되어진다. 가장 낮은 온도 영역은 모든 구리 혼입 유도체의 polaron 과 Li이 치환된 $Na_2Ti_3O_7$의 이온 전도도에 기인한다. 중간 온도영역의 전도 메커니즘은 관련된 층간의 이온 전도도에 기인하며 가장 높은 온도 영역에서는 변형된 층간 이온 전도도에 기인한다.

ESR, ESEM을 이용한 이온 교환된 MoH-SAPO-34에 대한 Mo의 화학종, 위치 및 흡착상호작용에 관한 연구 (Study on Mo(V) Species, Location and Adsorbates Interactions in MoH-SAPO-34 by Employing ESR and Electron Spin-Echo Modulation Spectroscopies)

  • 백건호;장창기;류창국;조영환;소현수
    • 대한화학회지
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    • 제46권1호
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    • pp.26-36
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    • 2002
  • $MoO_3$와 H-SAPO-34의 고체상 반응은 상자기성의 Mo(V) 화학종을 띤다. 탈수하면 Mo(V) 화학 종이 약하게 나타나지만 계속적으로 활성화 시키면 ESR로 규명할 수 있는 $Mo(V)_{5c}$$Mo(V)_{6c}$와 같은 Mo(V) 화학종이 생성된다. ESR과 ESEM 자료들은 $(MoO_2)^+$$(MoO)^{3+}$ 같은 옥소-몰리브덴 화학 종을 보여준다. $(MoO_2)^+$ 화학 종이 다음과 같이 더 합리적인 것 같이 보여진다. H-SAPO-34는 낮은 골격전하를 갖기 때문에 높은 양전하를 갖는 $(MoO)^{3+}$는 쉽게 안정화 되지 못한다. 소성된 H-SAPO-34와 도데카몰리브덴 규산 용액 사이의 용액 상태 반응은 단지 $MoO^{2+}$ 화학 종만을 발생한다. 마름모형 ESR 신호는 $D_2O$, $CD_3OH$, $CH_3CH_2OD$$ND_3$를 흡착할 때 관측되었다. Mo(V) 화학 종의 배위구조와 위치는 트리 펄스 전자 스핀반향 자료로 측정하였다. MoH-SAPO-34에 메탄올, 에틸렌 암모니아와 물이 흡착될 때 3분자, 1분자, 1분자와 1분자가 $(MoO_2)^+$에 각각 직접 배위하였다.