• 대한화학회지
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• 제50권3호
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• pp.183-189
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• 2006

초음파를 이용한 응축 반응을 이용하여 다양한 치환기가 붙은 4-methoxy-1-naphthyl ketone화합물들을 90% 이상의 높은 수율로 합성하였으며, 생성된 화합물물들을 미세 분석법, IR, 1H, 13C NMR 분석법 등을 이용하여 확인하였다. IR 스펙트럼에서 s-cis와 s-trans C=O stretching 모드를 확인하였으며, NMR 데이터로부터 에틸렌의 탄소와 수소에 대한 chemical shift를 확인하였다. 이러한 분광데이터를 이용하여 여러 분자들에 대한 Hammet 치환기 상수 값 들을 얻을 수 있었으며, 이들로부터 가용매 분해반응에 미치는 치환기 효과를 해석할 수 있었다.

• 한국식품과학회지
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• 제35권4호
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• pp.653-659
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• 2003

황색콩과 검은콩의 원산지를 판별하기 위하여 일반성분 및 20 MHz pulsed NMR을 이용하여 자기완화시간을 측정하였다. 일반성분으로는 황색콩은 조지방 함량 만이 원산지별 차이를 나타내었고, 검은콩의 경우에는 수분과 단백질 함량이 원산지별 차이를 보였다. 20 MHz pulsed NMR을 이용하여 자기완화시간 및 고형지방함량을 측정한 결과 황색콩은 고형지방함량과 $T_2-CPMG$ 측정시 원산지에 따라 유의적인 차이를 나타내었으며, 검은콩은 $T_1-SR$을 제외한 모든 측정항목에서 원산지별 차이를 나타내었다. 황색콩과 검은콩의 원산지 판별 분석시 일반성분만으로 정준판별분석을 시행한 결과 $70{\sim}91.7%$의 정확도를 나타내었으나, NMR 자기완화시간 및 고형지방함량을 이용한 경우 100%의 정확성으로 원산지를 판별해낼 수 있었다.

• 분석과학
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• 제17권2호
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• pp.98-107
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• 2004

본 연구에서는 $^1H$ NMR 분광분석법 및 HPLC를 이용하여 자동차 부품에 사용된 아크릴 코팅의 성분 및 함량을 분석하였다. $^1H$ NMR 분석 결과 아크릴 코팅은 88.40 wt%의 PMMA, 7.05 wt%의 MMA 및 2.36 wt%의 allyl methacrylate를 포함하고 있다. 또한, 고분자 첨가제로 벤조트리아졸 (Hisorb 328) 및 oxanilide 광안정제, BHT 및 DMP가 $^1H$ NMR 스펙트럼에서 확인되었고 정량적으로 측정되었다. 그러나, Bondapak C18 칼럼, 메탄올 이동상, PDA 검출기를 사용한 역상 HPLC 분석을 통해서는 두개의 광안정제만이 확인되었다. 두 광안정제의 함량은 UV-Vis 흡광광도계를 이용한 정량분석법을 통해 측정되고 NMR 분석 결과와 비교하였다. $^1H$ NMR 스펙트럼으로부터 얻은 분석 정보들이 HPLC에서 얻는 것들 보다 우수하였다.

• Bulletin of the Korean Chemical Society
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• 제35권7호
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• pp.1944-1950
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• 2014

Employment of a time consuming, sophisticated calculation using the all-atom force field and generalized-Born implicit solvent model (GBIS) for refinement of NMR structures has become practical through advances in computational methods and capacities. GBIS refinement improves the qualities of the resulting NMR structures with reduced computational times. However, the contribution of GBIS to NMR structures has not been sufficiently studied in a quantitative way. In this paper, we report the effects of GBIS on the refined NMR structures of ubiquitin (UBQ) and GB1 with subsets of distance restraints derived from experimental data. Random omission prepared a series of distance restraints 0.05, 0.1, 0.3, 0.5, and 0.7 times smaller. For each number, we produced five different restraints for statistical analysis. We then recalculated the NMR structures using CYANA software, followed by GBIS refinements using the AMBER package. GBIS improved both the precision and accuracy of all the structures, but to varied levels. The degrees of improvement were significant when the input restraints were insufficient. In particular, GBIS enabled GB1 to form an accurate structure even with distance restraints of 5%, revealing that the root-mean-square deviation was less than 1 ${\AA}$ from the X-ray backbone structure. We also showed that the efficiency of searching the conformational space was more important for finding accurate structures with the calculation of UBQ with 5% distance restraints than the number of conformations generated. Our data will provide a meaningful guideline to judge and compare the structural improvements by GBIS.

• 대한화학회지
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• 제55권4호
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• pp.590-593
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• 2011

새로운 유기주석(IV) 착물을 $Bu_2SnCl_2$과 N, O 및 S 주개 리간드인 5-(p-dimethylaminobenzylidene)rodanine(HL)로 부터 제조하였다. 염기 존재 하에 리간드는 탈양성자화되며, SnBuCl2L의 분자식을 갖는 착물이 형성되었다. 이 착물은 IR, $^1H$ NMR, $^{119}Sn$ NMR 및 원소분석을 통하여 전반적으로 특성을 분석하였다. 분광학적인 데이터로부터 리간드는 산소원자를 통하여 주석에 배위됨을 알았으며, 배위수가 4임을 용액에서 $^{119}Sn$ NMR 데이터에 의해 결정하였다.

• 한국자기공명학회:학술대회논문집
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• 한국자기공명학회 2002년도 International Symposium on Magnetic Resonance
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• pp.90-90
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• 2002

Syndecans, transmembrane heparan sulfate proteoglycans, are coreceptors with integrin in cell adhesion process. It forms a ternary signaling complex with protein kinase C and phosphatidylinositol 4,5 bisphosphate (PIP2) for integrin signaling. NMR data indicates that cytoplasmic domain of syndecan-4 (4L) undergoes a conformational transition in the presence of PIP2, forming oligomeric conformation. The structure based on NMR data demonstrated that syndecan-4L itself forms a compact intertwined symmetric dimer with an unusual clamp shape for residues Leu$^{186}$ -Ala$^{195}$ . The molecular surface of the syndecan-4L dimer is highly positively charged. In addition, no inter-subunit NOEs in membrane proximal amino acid resides (Cl region) has been observed, demonstrating that the Cl region is mostly unstructured in syndecan-4L dimmer. However, the complex structure in the presence of PIP2 induced a high order multimeric conformation in solution. In addition, phosphorylation of cytoplasmic domain induces conformational change of syndecan-4, resulting inhibition of PKC signaling. The NMR structural data strongly suggest that PIP2 promotes oligomerization of syndecan-4 cytoplasmic domain for PKC activation and further induces structural reorganization of syndecan for mediating signaling network in cell adhesion procedure.

• 폴리머
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• 제39권2호
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• pp.287-292
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• 2015

다양한 함량의 테레프탈산, 에틸렌글리콜, 1,4-싸이클로헥산 디메탄올, 이소소바이드로 구성된 일련의 바이오 기반 삼원 공중합체들의 특성을 $^1H$ NMR과 $^{13}C$ NMR을 이용하여 연구하였다. NMR 분석 결과 모두 랜덤한 미세 구조를 가졌고 시퀀스 분포는 이소소바이드의 함량에 따라 영향을 받았다. 시차주사열량계(DSC) 데이터로부터 유리전이온도는 주로 이소소바이드 함량이 증가함에 따라 증가하는 것을 알 수 있었다. 또한 확장된 Fox 식을 이용하여 각 성분의 함량에 따른 삼원공중합체의 유리전이 온도를 예측하고자 하였다.

• 한국자기공명학회논문지
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• 제26권1호
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• pp.1-9
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• 2022

There are two distinct approaches to improving the quality of protein NMR structures during refinement: all-atom force fields and accumulated knowledge-assisted methods that include Rosetta. Mao et al. reported that, for 40 proteins, Rosetta increased the accuracies of their NMR-determined structures with respect to the X-ray crystal structures (Mao et al., J. Am. Chem. Soc. 136, 1893 (2014)). In this study, we calculated 32 structures of those studied by Mao et al. using all-atom force field and implicit solvent model, and we compared the results with those obtained from Rosetta. For a single protein, using only the experimental NOE-derived distances and backbone torsion angle restraints, 20 of the lowest energy structures were extracted as an ensemble from 100 generated structures. Restrained simulated annealing by molecular dynamics simulation searched conformational spaces with a total time step of 1-ns. The use of GPU-accelerated AMBER code allowed the calculations to be completed in hours using a single GPU computer-even for proteins larger than 20 kDa. Remarkably, statistical analyses indicated that the structures determined in this way showed overall higher accuracies to their X-ray structures compared to those refined by Rosetta (p-value < 0.01). Our data demonstrate the capability of sophisticated atomistic force fields in refining NMR structures, particularly when they are coupled with the latest GPU-based calculations. The straightforwardness of the protocol allows its use to be extended to all NMR structures.

• 한국자기공명학회논문지
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• 제3권1호
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• pp.52-59
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• 1999

Authors synthesized common intermediates which are applicable for potential antibiotics. Their complete 13C and 1H NMR chemical shift data as well as carbon-and proton-fluorine coupling constants are reported. The knowledge of proton and carbon-fluorine coupling constants may help one assign the NMR data of the fluorinated quinolone derivatives. These results agree with the data published previously.

• 한국자기공명학회논문지
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• 제4권2호
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• pp.116-124
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• 2000

Singular value decomposition (SVD) has been used during past few decades in the advanced NMR data processing and in many applicable areas. A new modified SVD, piecewise polynomial truncated SVD (PPTSVD) was developed far the large solvent peak suppression and noise elimination in U signal processing. PPTSVD consists of two algorithms of truncated SVD (TSVD) and L$_1$ problems. In TSVD, some unwanted large solvent peaks and noises are suppressed with a certain son threshold value while signal and noise in raw data are resolved and eliminated out in L$_1$ problem routine. The advantage of the current PPTSVD method compared to many SVD methods is to give the better S/N ratio in spectrum, and less time consuming job that can be applicable to multidimensional NMR data processing.