• 제목/요약/키워드: low-field NMR

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Signal amplification by reversible exchange in various alcohol solvents

  • Jeong, Hye Jin;Namgoong, Sung Keon
    • 한국자기공명학회논문지
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    • 제25권4호
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    • pp.64-69
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    • 2021
  • In the developed NMR hyperpolarization techniques, Signal amplification by reversible exchange (SABRE) technique is thought to be a promising method to overcome the low sensitivity of bio-NMR/MRI. Most experiments using SABRE have been done in methanol, which is biologically harmful solvent. Therefore, more biological friendly solvent, such as ethanol can be more appropriate solvent to be applicable in bio-NMR and MRI. As the proof of concept, successful hyperpolarization on pyridine via SABRE is carried out in ethanol and its enhancement factor is calculated to be more than 150 folds. To investigate more about its possibility of hyperpolarization in different alcohol solvents, methanol and propanol are used for SABRE in the same condition. The overall polarization trend in different external magnetic field is similar but its polarization number is decreased with higher molecular weight solvents (the order from methanol to propanol). This result indicates that the efficiency of SABRE is different from solvent system despite its same functional group and similar properties. Higher para-hydrogen concentration, higher partial pressure of para-hydrogen, and deuterated solvent can increase the hyperpolarization in any solvents. With these series of successful SABRE results, future studies on SABRE in more biofriendly environment, on more various solvent systems, and with more substrates are needed and it will be the firm basis for applying the SABRE system on the future bio-NMR/MRI.

Heme 단백질의 Model로서의 Hemin 착물에 관한 $^1H$ NMR 연구 ($^1H$ NMR Study of mono-and di-cyanide ligated Hemin Complexes as Models of Hemoproteins)

  • 이강봉;김남준;권지혜;이재성;최영상
    • 분석과학
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    • 제7권4호
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    • pp.505-515
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    • 1994
  • DMSO(dimethylsuloxide-$d_6$) 용액 속에 존재하는 CN/CN 리간드의 hemin 착물과 CN/DMSO의 hemin 착물이 $^1H$ NMR로 기록되어지고 분석되어졌다. Hemin으로의 CN 착물화 과정은 온도에 따라 변화함을 NMR 스펙트럼이 보여 주며, 한 개의 CN 리간드에서 두 개의 CN 리간드착물로 바뀌는 과정의 열역학함수는 ${\Delta}H^{\circ}=736.6cal/mol$${\Delta}S^{\circ}=16.4eu$인 흡열과정을 나타낸다. CN/DMSO의 hemin 착물은 Curie behavior로부터의 벗어남은 high-spin 성격의 존재를 나태내고, 이는 Fe-DMSO 결합이 순간적으로 깨짐을 의미하며, 이러한 CN/DMSO hemin 착물이 한 개의 axial ligand가 약한 heme 단백질의 전자 및 분자구조의 model complex로 작용할 수 있음을 보여 준다.

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Analysis and reduction of thermal magnetic noise in liquid-He dewar for sensitive low-field nuclear magnetic resonance measurements

  • Hwang, S.M.;Yu, K.K.;Lee, Y.H.;Kang, C.S.;Kim, K.;Lee, S.J.
    • 한국초전도ㆍ저온공학회논문지
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    • 제15권2호
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    • pp.20-23
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    • 2013
  • For sensitive measurements of micro-Tesla nuclear magnetic resonance (${\mu}T$-NMR) signal, a low-noise superconducting quantum interference device (SQUID) system is needed. We have fabricated a liquid He dewar for an SQUID having a large diameter for the pickup coil. The initial test of the SQUID system showed much higher low-frequency magnetic noise caused by the thermal magnetic noise of the aluminum plates used for the vapor-cooled thermal shield material. The frequency dependence of the noise spectrum showed that the noise increases with the decrease of frequency. This behavior could be explained from a two-layer model; one generating the thermal noise and the other one shielding the thermal noise by eddy-current shielding. And the eddy-current shielding effect is strongly dependent on the frequency through the skin-depth. To minimize the loop size for the fluctuating thermal noise current, we changed the thermal shield material into insulated thin Cu mesh. The magnetic noise of the SQUID system became flat down to 0.1 Hz with a white noise of 0.3 $fT/{\surd}Hz$, including the other noise contributions such as SQUID electronics and magnetically shielded room, etc, which is acceptable for low-noise ${\mu}T$-NMR experiments.

NMR Studies on the Structure of Human Annexin I

  • Lee, Yeon-Hee;Han, Hee-yong;Oh, Jee-Young;Na, Doe-Sun;Lee, Bong-Jin
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 1997년도 춘계학술대회
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    • pp.86-86
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    • 1997
  • Human annexin I is a member of annexin family of calcium dependent phospholipid binding proteins, which have been implicated in various physiological roles including phospholipase A$_2$ (PLA$_2$) inhibition, membrane fusion and calcium channel activity. In this work, the structure of N-terminally truncated human annexin I (Δ-annexin I) and its interactions with Ca$\^$2+/, ATP and cAMP were studied at atomic level by using $^1$H, $\^$15/N, $\^$l3/C NMR (nuclear magnetic resonance) spectroscopy. The effect of Ca$\^$2+/ binding on the structure of Δ-annexin I was investigated, and compared with that of Mg$\^$2+/ binding. The addition of Ca$\^$2+/ to Δ-annexin I caused some changes in the high field and low field regions of $^1$H NMR spectra. Whereas, upon addition of Mg$\^$2+/ to Δ-annexin I, almost no change could be observed. Also we found that the binding ratio of ATP to Δ-annexin I is 1. Because Δ-annexin I is a large protein with 35 kDa molecular weight, site-specific (carbonyl-$\^$l3/C, amide-$\^$15/N) labeling technique was used to determine the interaction sites of Δ-annexin I with Ca$\^$2+/ and ATP. Assignments of all the histidinyl carbonyl carbon resonances have been completed by using Δ-annexin I along with its specific 1,2-subdomain. The carbonyl carbon resonances originating from His52 and His246 of Δ-annexin I were significantly affected by Ca$\^$2+/ binding, and some Tyr and Phe resonances were also affected. The carbonyl carbon resonances originating from His52 is significantly affected by ATP binding, therefore His52 seems to be involved in the ATP binding site of Δ-annexin I.

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NMR Studies on the Structure of Human Annexin I

  • Han, Hee-Yong;Bang, Keun-Su;Na, Doe-Sun;Lee, Bong-Jin
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 1996년도 춘계학술대회
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    • pp.182-182
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    • 1996
  • Annexin I is a member of the annexin family of calcium dependent phospholipid binding proteins and has anti-inflammatory activity by inhibiting phospholipase A$_2$ (PLA$_2$). Recent X-ray crystallographic study of annexin I identified six Ca$\^$2+/ binding bites, which was different types (type II, III) from the well-known EF-hand motif (type I). In this work, the structure of annexin I was studied at atomic level by using $^1$H, $\^$15/N and $\^$l3/C NMR(nuclear magnetic resonance) spectroscopy, and the effect of Ca$\^$2+/ binding on the structure of annexin I was studied, and compared with that of Mg$\^$2+/ binding, When Ca$\^$2+/ was added to annexin I, NMR peak change was occured in high- and low-field regions of $^1$H-NMR spectra. NMR peak change by Ca$\^$2+/ binding was different from that by Mg$\^$2+/ binding. Because annexin I is a larger protein with 35 kDa molecular weight, site-specific (amide-$\^$15/N, carbonyl-$\^$l3/C) labeling technique was also used. We were able to detect methionine, tyrosine and phenylalanine peaks respectively in $\^$13/C-NMR spectra, and each residue was able to be assigned by the method of doubly labeling annexin I with [$\^$13/C] carbonyl-amino acid and [$\^$15/N] amide-amino acid. In $\^$l3/C-NMR spectra of [$\^$13/C] carbonyl-Met labeled annexin I, we observed that methionine residues spatially located near Ca$\^$2+/ binding Sites Were Significantly effected by Ca$\^$2+/ binding. From UV spectroscopic data on the effect of Ca$\^$2+/ binding, we knew that Ca$\^$2+/ binding sites of annexin I have cooperativity in Ca$\^$2+/ binding. The interaction of annexin I with PLA$_2$ also could be detected by using heteronuclear NMR spctroscopy. Consequently, we expect that the anti-inflammatory action mechanism of annexin I may be a specific protein-protein interaction. The residues involved in the interaction with PLA$_2$ can be identified as active site by assigning NMR peaks effected by PLA$_2$ binding.

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NMR relaxation 기법을 이용한 한국산과 중국산 대두의 원산지 판별 (The Geographical Discrimination of Korean and Chinese Soybeans (Glycine max(L.) merrill) Using NMR Relaxation Methods)

  • 김미현;노정해;이철호
    • 한국식품과학회지
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    • 제41권3호
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    • pp.292-295
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    • 2009
  • 국내산 콩 25종과 중국산 콩 24종을 일반성분 분석을 실시하고 10MHz pulsed NMR의 relaxation pattern을 이용하여 농산물의 원산지에 따른 차이를 구명하고 이에 따른 정확하고 신속한 원산지 판별이 가능하도록 하였다. 국내산과 중국산 콩의 일반성분 분석을 실시한 결과 수분, 지방, 회분에 유의적 차이가 없었고 조단백질 함량에서는 국내산이 중국산보다 높았다. T1-IR을 이용하여 측정한 NMR값은 중국산 콩이 국내산 콩보다 짧은 이완시간을 갖는 것으로 나타났으며(p<0.0001), $T_1-Sr$도 마찬가지였다(p<0.0001). 횡이완시간 중 $T_2-SE$의 값은 국내산이 중국산보다 높게 나타났다(t-test, p<0.0086). $T_1-IR$$T_1-SR$ 두 개의 변수를 이용하여 판별식을 작성한 경우 국내산과 중국산 모두 96%의 판별 가능성을 보였으며, $T_1-IR$$T_1-SR$, $T_2-SE$, $T_2-CPMG$의 모든 변수를 이용하여 판별한 결과 국내산과 중국산 콩의 판별 정확성이 100%로 나타났다. 이 연구를 통하여 저자장 NMR을 이용하여 국내산과 중국산 콩을 유의적 선별해 낼 수 있는 가능성을 확인하였다.