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Side Chain Assignment生物大分子波谱学原理
吴季辉
(H)C(CO)NH-TOCSY: Side Chain C chemical shifts
H(CC)(CO)NH-TOCSY: Side chain H chemical shifts
HCCH-COSY: adjacent C-C correlation
HCCH-TOCSY: long range C-C correlation within one residue
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CCONH-TOCSY生物大分子波谱学原理
吴季辉
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HCONH-TOCSY生物大分子波谱学原理
吴季辉
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13C - 13C 相关谱
生物大分子波谱学原理吴季辉
碳-碳相关谱HCCH-COSY ( 1H-13C-13C-1H correlation spectroscopy )
及 HCCH-TOCSY ( 1H-13C-13C-1H total correlation spectroscopy )用于证认 13C 标记蛋白质的脂肪链 1H 及 13C ,信号传递是从 1H 开始,经过单键 J 偶合到 13C ,再通过类似同核 COSY 及 TOCSY 的机制传递到其他 13C ,最后通过单键 J偶合回传到 1H 。所以这类实验可以看作 1H 同核 COSY 及TOCSY 在 13C 上的推广。除了可以获得 13C 的信息,也可得到1H 的信息,对于大蛋白质而言,效果比 1H 同核 COSY 及TOCSY 更好,因为在 1H 同核 COSY 及 TOCSY 中起作用的是比较小的 1H 同核 J 偶合(一般小于 10Hz ),而这里虽有三步传递,却均是比较大的 J 偶合,其中 JHC 约 140Hz , JCC 约35Hz 。因此这类实验对于大蛋白质的侧链 1H , 13C 的证认非常重要。
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13C - 13C 相关谱
生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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生物大分子波谱学原理吴季辉
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7.3 13C - 13C 相关谱生物大分子波谱学原理
吴季辉
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7.3 13C - 13C 相关谱
生物大分子波谱学原理吴季辉
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7.3 13C - 13C 相关谱
生物大分子波谱学原理吴季辉
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7.3 13C - 13C 相关谱生物大分子波谱学原理
吴季辉
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7.3 13C - 13C 相关谱生物大分子波谱学原理
吴季辉
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Conventional implementation: 1H magnetization is transferred in a refocused INEPT to 13C in-phase magnetization. After C,C-TOCSY mixing, the back-transfer is achieved in an analogous manner. The incrementation of delays required for shared-time evolution in t1 is also indicated. Note that the C' 180 pulse during the t1 evolution period is not absolutely required, because 2JH,C' couplings are small.
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Doubly sensitivity-enhanced 3D H(C)CH-TOCSY experiment with hetero-nuclear gradient echo for solvent suppression. The heteronuclear in-phase transfer is implemented with a yxz-ICOS-CT sequence. Four different combination of gradients and and of phase settings and (corresponding to echo/antiecho pathways for both indirect dimensions) have to be recorded and stored in different memory locations. Modifications required for a semi-constant-time evolution during t1 are indicated. The operator F is the sum of I operators denoting the proton spins
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