• 제목/요약/키워드: 31P NMR

검색결과 123건 처리시간 0.028초

Solid-State $^{31}P$ NMR Chemical Shielding Tensors in Binuclear Platinum Diphosphite Complexes

  • 우애자;Leslie G. Butler
    • Bulletin of the Korean Chemical Society
    • /
    • 제17권5호
    • /
    • pp.457-460
    • /
    • 1996
  • The principal elements of the 31P NMR chemical shielding tensors have been determined for three binuclear platinum diphosphite complexes, K4[Pt2(P2O5H2)4·2H2O ("Pt2"), K4[Pt2(P2O5H2)4Cl2]·2H2O ("Pt2Cl2"), and K4[Pt2(P2O5H2)4Br2]·2H2O ("Pt2Br2"), by using a Herzfeld-Berger graphical method for interpreting the 31P MAS spectrum. The orientations of 31P chemical shielding tensor relative to the molecular axis system are partially assigned with combination of the longitudinal relaxation study of HPO32- and the reference to known tensor orientations of related sites; the most chemical shielding component, δ33, is directed along the P-Pt bond axis. A discussion is given in which the experimental principal elements of the 31P chemical shielding tensor are related with the Pt-Pt bond distances in binuclear platinum diphosphite complexes.

Localized In Vivo $^{31}P$ NMR Studies on Rabbit Skeletal Muscle Tissue from Premortem to Postmortem Period

  • Choe, Bo-Young;Kim, Sung-Eun;Lee, Hyoung-Koo;Suh, Tae-Suk;Lee, Heung-Kyu;Shinn, Kyung-Sub
    • 한국자기공명학회논문지
    • /
    • 제3권1호
    • /
    • pp.1-11
    • /
    • 1999
  • Localized in vivo 31P NMR spectroscopy was applied to evaluate the postmortem catabolism of high energy phosphates in rabbit skeletal muscle tissue. In the premortem processes all of the important high energy phosphate metabolites were characterized, and particularly phosphocreatine (PCr) resonance signal was the strongest. In the immediate phases of the postmortem processes the signal intensities of PCr, phosphomonoesters (PME), phosphodiesters(PDE), $\alpha$-, $\beta$- and ${\gamma}$-adenosine triphosphate (ATP) resonance began to decrease while the signal intensity of inorganic phosphorus (Pi) resonance began to increase. The present study suggests that localized in vivo 31P NMR spectroscopy may provide more precise biochemical information of the early postmortem period based on the metabolic alterations of phosphate. The unique ability of localized in vivo 31P NMR spectroscopy to offer noninvasive information about tissue biochemistry in animals as well as human may have an impact on thanatochronology and medicolegal science.

  • PDF

Per-deuteration and NMR experiments for the backbone assignment of 62 kDa protein, Hsp31

  • Kim, Jihong;Choi, Dongwook;Park, Chankyu;Ryu, Kyoung-Seok
    • 한국자기공명학회논문지
    • /
    • 제19권3호
    • /
    • pp.112-118
    • /
    • 2015
  • Hsp31 protein is one of the members of DJ-1 superfamily proteins and has a dimeric structure of which molecular weight (MW) is 62 kDa. The mutation of DJ-1 is closely related to early onset of Parkinson's disease. Hsp31 displays $Zn^{+2}$-binding activity and was first reported to be a holding chaperone in E. coli. Its additional glyoxalase III active has recently been characterized. Moreover, an incubation at $60^{\circ}C$ induces Hsp31 protein to form a high MW oligomer (HMW) in vitro, which accomplishes an elevated holding chaperone activity. The NMR technique is elegant method to probe any local or global structural change of a protein in responses to environmental stresses (heat, pH, and metal). Although the presence of the backbone chemical shifts (bbCSs) is a prerequisite for detailed NMR analyses of the structural changes, general HSQC-based triple resonance experiments could not be used for 62 kDa Hsp31 protein. Here, we prepared the per-deuterated Hsp31 and performed the TROSY-based triple resonance experiments for the bbCSs assignment. Here, detailed processes of per-deuteration and the NMR experiments are described for other similar NMR approaches.

Modulation of the Specific Interaction of Cardiolipin with Cytochrome c by Zwitterionic Phospholipids in Binary Mixed Bilayers: A $^2H$-and $^{31}P$-NMR Study

  • Kim, Andre;Jeong, In-Chul;Shim, Yoon-Bo;Kang, Shin-Won;Park, Jang-Su
    • BMB Reports
    • /
    • 제34권5호
    • /
    • pp.446-451
    • /
    • 2001
  • The interaction of cytochrome c with binary phospholipid mixtures was investigated by solid-state $^2H$- and $^{31}P$-NMR. To examine the effect of the interaction on the glycerol backbones, the glycerol moieties of phosphatidylcholine (PC), and cardioliph (CL) were specifically deuterated. On the binding of cytochrome c to the binary mixed bilayers, no changes in the quadrupole splittings of each of the components were observed for the PC/PG, PE/CL and PE/PG liposomes. In contrast, the splittings of CL decreased on binging of protein to the PC/CL liposomes, although those of PC did not change at all. This showed that cytochrome c specifically interacts with CL in PC/CL bilayers, and penetrates into the lipid bilayer to some extent so as to perturb the dynamic structure of the glycerol backbone. This is distinctly different from the mode of interaction of cytochrome c with other binary mixed bilayers. In the $^{31}P$-NMR spectra, line broadening and a decrease of the chemical shift anisotropy were observed on the binding of cytochrome c for all binary mixed bilayers that were examined. These changes were more significant for the PC/CL bilayers. Furthermore, the line broadening is more significant for PC than for CL in PC/CL bilayers. Therefore, it can be concluded that with the polar head groups, not only CL but also PC are involved in the interaction with cytochrome c.

  • PDF

견 피브로인의 인산화와 그 특성 (Phosphorylation of silk fibroin and its properties)

  • 문장희;김정호;배도규;신봉섭
    • 한국잠사곤충학회지
    • /
    • 제43권2호
    • /
    • pp.116-124
    • /
    • 2001
  • STMP로 견 피브로인을 인산화 시키는 반응에서, 처리 조건별로 실험하여 적정 조건을 구하였고, 인이 결합되는 위치를 규명하기 위해 FT-IR과 $^{31}$ P NMR분석을 행했고, 인산화된 견 피브로인의 특성을 평가하여 다음과 같은 결론을 얻었다. 1. 견 피브로인을 STMP로 인산화 시킬 때, 알칼리도가 클수록, 처리 온도가 높을수록 인산화 정도가 증가되었다 2.처리시간에 따른 인산화 정도는 1hr까지는 급격하게 증가하였고, 1hr 이후에는 서서히 증가되어 비교적 단시간에 인산화가 많이 진행되었다. 3. STMP 농도에 따른 인산화 정도는 50%까지는 급격히 증가되지만, 100% 이상에서는 증가가 미약하였다 4. 인산화된 견 피브로인의 FT-IR분석에서, 각 시료는 ∝-helix에 가까운 형태이었고, 아미노기에 의한 인산화 반응(phosphoramidation)은 고려되지 않았다 5. $^{31}$ P NMR분석 결과에서는 인산화가 polyphosphate형태로 되어 있다는것을 알 수 있었다. 6. 인산화가 많이 될수록 탁도와 거품팽창성, 그리고 거품안정성은 증가하였으며, 용해도는 오히려 감소하였다. 무처리 시료에 비해 거품팽창성은 1.6배, 거품안정성은 2배로 증가하였다. 7. 유화력는 시료 P100 까지는 증가되다가 그 이상에서는 약간 감소하는 경향으로 나타났으며, 유화안정성은 인산화 정도가 많이 될수록 증가하였다. 유화력은 최고 18%, 유화안정성은 21%가 증가되었다.

  • PDF

Characterization of the Catalytic Heteropoly Compounds using Solid-state NMR

  • Kim, Y;Lee, W
    • 한국자기공명학회논문지
    • /
    • 제1권1호
    • /
    • pp.45-58
    • /
    • 1997
  • Heteropoly compounds, H3PMo12O40, CsxH3-xPMo12O40, and vanadium containing heteropoly compound were characterized by Solid-state broad line 1H MAS NMR, 31P MAS NMR, and High Speed MAS 51V NMR spectroscopy of quadrupolar nuclei. The effects of calcination, dehydration, and the number of protons on the structure of heteropoly compounds were studied. The results of this study demonstrate that these Solid-state NMR techniques are very useful tools to study heteropoly compounds.

  • PDF

$^{31}$P NMR을 이용한 카올리나이트에 흡착된 인산염의 연구 (A Study of Phosphate Adsorption on Kaolinite by $^{31}$P NMP Spectroscopy)

  • 김영규
    • 한국광물학회지
    • /
    • 제13권4호
    • /
    • pp.186-195
    • /
    • 2000
  • To study phosphate adsorption on kaolinite, $^{31}$ P MAS NMR(magic angle spinning nuclear magnetic resonance spectroscopy)has been used for kaolinite reacted in 0.1 M phosphate solutions at pH’s from 3 to 11. There are at least 3 different forms of phosphate on kaolinite. One is the phosphate physically adsorbed on kaolinite surface (outer-sphere complexes) or species left after vacuum-filtering. The second is the phosphate adsorbed by ligand exchange (inner-sphere complexes), and the third is Al-phosphate precipitates which are pH dependent. Most of the inner-spherer complexes and surface precipitates are mainly on hydroxided Al(aluminol) rather than hydroxided Si(silanol). These are pertinent with the results obtained from the phosphate adsorption experiments on silica gel and ${\gamma}$-Al$_2$O$_3$ as model compounds, respectively. The two peaks with more negative chemical shifts(more shielded) than the ortho-phosphate peak (positive chemical shift) are assigned to be the inner-sphere complexes and surface precipitates. The $^{31}$ P chemical shifts of the Al-phosphate precipitates are more negative than those of inner-sphere complexes at a given pH due to the larger number of P-O-Al linkages per tetrahedron. The chemical shifts of both the inner-sphere complexes and surface precipitates are more negative than those of inner-sphere complexes at a given pH due to the larger number of P-O-Al linkages per tetrahedron. The chemical shifts of both the inner-sphere complexes and surface precipitates become progressively less shielded with increasing pH. For the inner-sphere complexes, decreasing phosphate protonation combined with peak averaging by rapid proton exchange among phosphate tetrahedra with different numbers of protons is though to be the reason for the peak change. The decreasing shielding with increasing pH for surface precipitates is probably due to the decreasing average number of P-O-Al linkages per tetrahedron combined with decreasing protonation like inner-sphere complexes.

  • PDF

해저 퇴적물에 함유된 인의 존재 형태에 대한 연구 (Investigation of Phosphorus Species in Marine Sediment)

  • 김영규
    • 한국광물학회지
    • /
    • 제16권2호
    • /
    • pp.151-159
    • /
    • 2003
  • 국내 최초로 $ 31^{P}$NMR 및 XRD를 이용하여 월성원자력 발전소 인근의 해저 저질토에 대하여 퇴적물의 광물학적인 성분 분석 및 인의 존재형태에 대한 연구를 수행하였다. 약 30 cm의 코아에 대한 연구결과, 광물종은 심도별로 변화가 없었으며 주 구성광물은 석영, 알바이트, 미사장석, 방해석과일라이트, 스멕타이트, 녹니석, 그리고 카올리나이트 등이 동정되었다. $^{31}$ P NMR 결과는 다른 외국의 해양 퇴적물에서 보고된 것과 같은 다양한 종의 인은 발견되지 않았으며, 단지 주로 orthophosphate-monoester와 함께 orthophosphate-diester로 판단되는 인이 아주 미량으로 같이 존재하는 것으로 밝혀졌으며 광물종의 경우와 마찬가지로 심도별 인의 종의 변화가 거의 없음을 보여준다. 본 연구 지역의 인은 주로 해양 생물로부터 기인한 것으로 판단된다. 인의 존재형태는 본 지역의 시료들이 산화환경에 있었음을 지시하며 XRD의 실험결과와 더불어 유추할 수 있듯이 본 시료에 대하여 동일한 퇴적환경과 산화환경이 계속되어 왔거나, 아니면 다양한 환경에 있던 것들이 후의 외부적 교란에 의하여 서로 혼합되어 표면의 산화환경에 계속적인 노출이 있었음을 지시한다.