• 한국자기공명학회논문지
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• 제10권1호
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• pp.59-73
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• 2006

Spin-lattice relaxation pathway of $CH_2$ spin system by two dimensional NOESY sequence has been discussed. Two-dimensional spectra governed by dipolar relaxation mechanism were simulated in term of transfer mode, the generalization of conventionally used magnetization mode in one dimension. The transfer matrix directly related to the Redfield relaxation matrix can be constructed by the multiplet of transfer mode. The observable relaxation transfer modes causes to variation of the off-diagonal signal intensity of phase sensitive NOESY spectra from which variable spectral density can be extracted with simple group theoretical calculation. The variation of the J-coupling peak intensity as a function of the mixing time in 2-D spectra for $n-Undecane-5-^{13}C$ and Bromoacetic $2-^{13}C$ acid has been theoretically traced.

• Bulletin of the Korean Chemical Society
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• 제16권7호
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• pp.649-653
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• 1995

Solution-state structure of native F430 was determined by using NMR methods and NMR-based distance geometry (DG) computations. Structures were generated with loose NOE-derived interproton distance restraints (2.0-2.5 Å, 2.0-3.5 Å and 2.0-4.5 Å for strong, medium, and weak NOE cross-peak intensities, respectively). 2D NOESY back-calculations of structures were subsequently carried out for establishing the consistence between experimental data and DG-model structures. The back-calculated 2D NOESY spectra of resulting DG structures were well consistent with experimental 2D NOESY spectra. Superposition of 20 independent structures with macrocyclic ring atoms and all atoms of F430 afforded pairwise root mean square deviations (RMSD) of 0.025-0.125 Å and 0.64-1.3 Å, respectively. The macrocyclic rings of structures are well converged to a unique conformation with saddle-shaped deformation whereas most of side chains are not converged. The average dihedral angle (N1-N2-N3-N4, 27.78±1.50°) of 20 DG-structures exhibits that the macrocyclic ring conformation is puckered as much as 12,13-diepimeric F430 (28.75±4.07°).

• 한국자기공명학회논문지
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• 제1권2호
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• pp.103-111
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• 1997

Proper pulse sequences and experimental optimization for the 3D 15N edited TOCSY and NOESY spectra were described. Using sensitivity enhancement approach with coherent selection by pulsed field gradients described by Kay and co-workers, an considerable gain in sensitivity was achieved. The sensitivity was also improved by minimal water saturation using water flip-back pulse. Among the three types of TOCSY mixing pulse, named MLEV-17, DIPSI-2rc, DIPSI-2rc sequence gave the most sensitive spectrum. These results suggest an appropriate pulse sequence for for those 3D experiments for large proteins.

• Investigative Magnetic Resonance Imaging
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• 제12권1호
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• pp.8-19
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• 2008

목적 : 본 연구에서는 인체 뇌 대사물질에 대하여 2D MR 기술인 correlation spectroscopy (COSY) 와 nuclear Overhauser effect/enhancement spectroscopy (NOESY)를 직접 적용하고, 데이터를 획득하여 인체 뇌대사물질들간의 스칼라 짝지움 (coupling)과 쌍극자 (dipolar) 상호작용- NOE에 대한 분석을 통하여 결합연결관계 및 공간연결관계에 대한 정보를 획득하고자 하였다. 대상 및 방법 : 모든 2-D (dimensional) MR 실험 (즉, COSY와 NOESY)은 z축 능동차폐 펄스경사자장, 삼중공명 동결탐침기가 장착된 Bruker Avance 500 (11.8 T) 장비에서 298 K에 수행되었다. MRS상에서 뇌 대사물질과 유사하도록만든 희석액을 만들었고, 최종 MRS 샘플은 10% $D_2O$를 이용하였다. 2-D 스펙트라는 2048 복합 (complex) 데이터 포인트로서 총 320개 의 free induction decay (FID)를 평균화 (averaging)하였고, $H_2O$에서 얻어진 스펙트라는 8012 Hz 였다. 반복지연 (repetition delay) 시간은 2초, 각각의 FID는 4개의 평균화를 선택하였다. 얻어진 2D-COSY, 2D-NOESY 데이터는 Top Spin 2.0 소프트웨어에서 후 처리기법 (post-processing)에 의해 분석되었다. 분석 대상 대사물질은 N-acetyl aspartate (NAA), creatine (Cr), choline (Cho), glutamine (Gln), glutamate (Glu), myo-inositol (Ins), lactate (Lac)로서 총 7 가지 화학물로서 주요 목표 피크로 정했다. 결과 : 인체 뇌 대사물질에 대한 대칭형태의 2D-COSY와 2D-NOESY 스펙트럼을 획득하였고, COSY 스펙트럼상에서는 오직 1.0-4.5 ppm 사이에서만 교차피크들이 생성된 반면 NOESY 스펙트럼상에서는 1.0-4.5 ppm 외에도 7.9 ppm에서 공명 교차피크를 발견할 수 있었다. COSY 스펙트럼을 통하여 lactate에서 메틸 프로톤과 CH 프로톤의 COSY 크로스피크가 발견되었고, NAA에서 메틸렌 프로톤들간과 메틸렌 프로톤과 NH프로톤의 크로스피크가 발견되었고, Ins에서 CH 프로톤 들간의 크로스피크가 발견되었다. NOESY 스펙트럼을 통하여 NAA 분자내 NH 프로톤과 메틸 (-CH3) 프로톤과의 NOESY 크로스피크가 발견되었고, lactate에서 메틸 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Cr에서 메틸 프로톤과 메틸렌 프로톤과의 크로스피크가 발견되었고, Glu에서 메틸렌 프로톤 들간과 또한 메틸렌 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Gln에서 메틸렌 프로톤과 CH 프로톤과의 크로스피크가 발견되었고, Ins에서 CH 프로톤 들간의 크로스피크가 발견되었다. 결론 : 본 연구에서는 in vitro 상태의 인체 뇌 대사물질에 2D-COSY와 2D-NOESY 기술을 직접 적용하고, 결합연결관계 및 공간연결관계에 대한 정보를 성공적으로 획득하여 분석하여 보았다. 본 연구 결과물은 향후 인체 내 in vivo 2D-COSY를 이용한 뇌 대사물질 연구에 매우 유용하리라 사료된다.

• Bulletin of the Korean Chemical Society
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• 제30권10호
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• pp.2481-2484
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• 2009

• 한국자원식물학회지
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• 제19권6호
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• pp.655-659
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• 2006

Two dineolignans (1,2) with nitric oxide inhibitory activities were isolated from Saururus chinensis (Saururaceae) using silica gel column chromatography. Although the structures, saucernetin-7 (1) and -8 (2), have been already reported, NMR assignment of the two compounds was completed aided by 2D-NMR spectroscopy including $^1H-^1H$ COSY, $^1H-^{13}C$ COSY, HMBC and NOESY NMR spectra. Compounds 1 and 2 exhibited significant nitride oxide inhibitory activity in LPS-induced RAW 264.7 cells with $IC_{50}$ values of $11.3{\mu}M\;and\;7.1{\mu}M$, respectively.

• 약학회지
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• 제39권1호
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• pp.85-93
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• 1995

Acidic and alkaline hydrolysis of diol-type ginseng saponins produced a new glycoside, (20E)-ginsenoside Rh$_{3}$, and its stereoisomer (20Z)-, which were further subjected to alkaline by drolysis to give their aglycones, (20E)- and (20Z)-3$\beta$, 12$\beta$-dihydroxy-dammar-20(22),24-diene. The ratio of stereoisomeric mixtures was estimated to be ca. 5:1 from intensities of the peaks in $^{1}$H- and $^{13}$C-NMR spectra. The $^{1}$H- and $^{13}$C-NMR signals of ginsenoside Rh$_{3}$, which have remained unclarified, were completely assigned by the extensive application of modern NMR techniques.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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• pp.202.3-202.3
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• 2003

Two Known compounds, syringaresinol monoglucoside(8), chimaphilin(14), together with three new compounds, (9)[mp. $106{\sim} 111^{\circ}C$, C_{29}H_{44}O_{13}$], (10)[mp. $180{\sim}182^{\circ}C$, $C_{15}H_{20}O_{9}$] and (11)[mp. $100{\sim}105^{\circ}C$, $C_{18}H_{28}O_{8}$] were isolated from the BuOH fractionof Pyrola japonics(Pyrolaceae). The structures of the known compounds were determined by chemical and spectorscopic methods. The assignments of the $^{1}H-$ and $^{13}C-NMP$ spectra of these compounds were carried out by two-dimensional $^1H-^1H-COSY$, NOESY and $^1H-^{13}C$ multiple-bond, multiplequantum spectroscopic correlation techniques. The characterization of the three new compounds is now in progress.

• 한국자기공명학회논문지
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• 제20권3호
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• pp.95-101
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• 2016

Apolipoprotein B-100 (Apo-B100) is a major component of low density lipoprotein (LDL). Apo B-100 protein has 4,536 amino acid sequence and these amino acids are classified into peptide groups A to G with subsequent 20 amino acids (P1-P302). The peptide groups were act as immunoglobulin (Ig) antigens which oxidized via malondialdehyde (MDA). The mimetic peptide P1 (EEEMLENVSLVCPKDAT RFK) out of D-group peptides carrying the highest value of IgG antigens were selected for structural studies that may provide antigen specificity. Circular Dichroism (CD) spectra were measured for peptide secondary structure in the range of 190-250 nm. Experimental results show that P1 exhibit partial of ${\beta}-sheet$ and random coil structure. Homonuclear (COSY, TOCSY, NOESY) 2D-NMR experiments were carried out for NMR signal assignments and structure determination for P1. On the basis of these completely assigned NMR spectra and distance data, distance geometry (DG) and Molecular dynamics (MD) were carried out to determine the structures of P1. The proposed structure was selected by comparisons between experimental NOE spectra and back calculated 2D NOE results from determined structure showing acceptable agreement. The total Root-Mean-Square-Deviation (RMSD) value of P1 obtained upon superposition of all atoms was in the range $0.33{\AA}$. The solution state P1 has mixed structure of ${\beta}-sheet$ (Glu[1] to Cys[12]) and random coil (Pro[13] to Lys[20]). These NMR results are well consistent with secondary structure from experimental results of circular dichroism. Structural studies based on NMR may contribute to the studies of atherosclerosis and observed conformational characteristics of apo B-100 in LDL using monoclonal antibodies.

• 한국자기공명학회논문지
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• 제24권4호
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• pp.136-142
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• 2020

Apolipoprotein B-100 (apo B-100), the main protein component that makes up LDL (Low density lipoprotein), consists of 4,536 amino acids and serves to combine with the LDL receptor. The oxidized LDL peptides by malondialdehyde (MDA) or acetylation in vivo were act as immunoglobulin (Ig) antigens and peptide groups were classified into 7 peptide groups with subsequent 20 amino acids (P1-P302). The biomimetic peptide P99 (KGTYG LSCQR DPNTG RLNGE) out of B-group peptides carrying the highest value of IgM antigens were selected for structural studies that may provide antigen specificity. Circular Dichroism (CD) spectra were measured for peptide secondary structure in the range of 190-260 nm. Experimental results show that P99 has pseudo α-helice and random coil structure. Homonuclear (COSY, TOCSY, NOESY) 2D-NMR experiments were carried out for NMR signal assignments and structure determination for P99. On the basis of these completely assigned NMR spectra and proton distance information, distance geometry (DG) and molecular dynamic (MD) were carried out to determine the structures of P99. The proposed structure was selected by comparisons between experimental NOE spectra and back-calculated 2D NOE results from determined structure showing acceptable agreement. The total Root-Mean-Square-Deviation (RMSD) value of P99 obtained upon superposition of all atoms were in the set range. The solution state P99 has mixed structure of pseudo α-helix and β-turn(Gln[9] to Thr[13]). These NMR results are well consistent with secondary structure from experimental results of circular dichroism. Structural studies based on NMR may contribute to the prevent oxidation studies of atherosclerosis and observed conformational characteristics of apo B-100 in LDL using monoclonal antibodies.