SHARPER-DOSY: Sensitivity enhanced diffusion-ordered NMR spectroscopy.
SHARPER-DOSY: Sensitivity enhanced diffusion-ordered NMR spectroscopy.
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DOI：
10.1038/s41467-023-40130-2
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发表时间：
2023-07-21
影响因子：
16.6
通讯作者：
Uhrin, Dusan
中科院分区：
文献类型：
--
作者：
Peat, George;Boaler, Patrick J.;Dickson, Claire L.;Lloyd-Jones, Guy C.;Uhrin, Dusan
自世纪中期发现以来，核磁共振（NMR）的灵敏度稳步提高，部分原因是设计了新的、复杂的NMR实验。在这里，我们报告的液态NMR方法，显着增加了纯化合物的扩散系数测量的灵敏度，允许估计它们的大小使用的材料量大大减少。在这种方法中，通过分析窄而强的单态来测量扩散系数，这些单态对磁场的不均匀性是不变的。通过嵌入在由非选择性180°或90°脉冲分开的短（<0.5 ms）自旋回波间隔中的信号采集来获得单重态，抑制共振的化学位移演变及其由于J耦合引起的分裂。灵敏度提高10−100倍，节省时间100−10000倍。使用高场冷冻探针NMR光谱仪，这使得有可能在几分钟内测量中等大小的有机分子的扩散系数，只需几百纳克的材料。自发现以来，核磁共振的灵敏度稳步提高。在这里，作者报告了一种液态NMR方法，该方法将扩散系数测量的灵敏度提高了10-100倍，允许使用微克量的化合物，同时将测量时间减少到几分钟。
Since its discovery in mid-20th century, the sensitivity of Nuclear Magnetic Resonance (NMR) has increased steadily, in part due to the design of new, sophisticated NMR experiments. Here we report on a liquid-state NMR methodology that significantly increases the sensitivity of diffusion coefficient measurements of pure compounds, allowing to estimate their sizes using a much reduced amount of material. In this method, the diffusion coefficients are being measured by analysing narrow and intense singlets, which are invariant to magnetic field inhomogeneities. The singlets are obtained through signal acquisition embedded in short (<0.5 ms) spin-echo intervals separated by non-selective 180° or 90° pulses, suppressing the chemical shift evolution of resonances and their splitting due to J couplings. The achieved 10−100 sensitivity enhancement results in a 100−10000-fold time saving. Using high field cryoprobe NMR spectrometers, this makes it possible to measure a diffusion coefficient of a medium-size organic molecule in a matter of minutes with as little as a few hundred nanograms of material. Since its discovery, the sensitivity of Nuclear Magnetic Resonance has increased steadily. Here the authors report on a liquid-state NMR methodology that increases the sensitivity of the diffusion coefficient measurements 10–100- fold, allowing to use microgram quantities of compounds, while reducing the measurement time to few minutes.
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在可变场和方向的氮气中心钻石中的局部和散装（13）C超极化。
影响因子：
16.6
作者：
Álvarez GA;Bretschneider CO;Fischer R;London P;Kanda H;Onoda S;Isoya J;Gershoni D;Frydman L
通讯作者：
Frydman L
影响因子：
16.6
作者：
Dai D;Wang X;Liu Y;Yang XL;Glaubitz C;Denysenkov V;He X;Prisner T;Mao J
通讯作者：
Mao J
影响因子：
2.2
作者：
Hürlimann, MD;Venkataramanan, L
通讯作者：
Venkataramanan, L
DOI：
10.1002/anie.202011642
发表时间：
2021-01-11
期刊：
Angewandte Chemie (International ed. in English)
影响因子：
--
作者：
Kiraly P;Kern N;Plesniak MP;Nilsson M;Procter DJ;Morris GA;Adams RW
通讯作者：
Adams RW
影响因子：
15
作者：
Larsen, FH;Skibsted, J;Nielsen, NC
通讯作者：
Nielsen, NC