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Side Chain Assignment

生物大分子波谱学原理 吴季辉. Side Chain Assignment. (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. 生物大分子波谱学原理 吴季辉. CCONH-TOCSY. 生物大分子波谱学原理 吴季辉. HCONH-TOCSY.

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Side Chain Assignment

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  1. 生物大分子波谱学原理 吴季辉 Side Chain Assignment (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

  2. 生物大分子波谱学原理 吴季辉 CCONH-TOCSY

  3. 生物大分子波谱学原理 吴季辉 HCONH-TOCSY

  4. 生物大分子波谱学原理 吴季辉 13C－13C相关谱 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。

  5. 生物大分子波谱学原理 吴季辉 13C－13C相关谱

  6. 生物大分子波谱学原理 吴季辉

  7. 生物大分子波谱学原理 吴季辉

  8. 生物大分子波谱学原理 吴季辉

  9. 生物大分子波谱学原理 吴季辉

  10. 生物大分子波谱学原理 吴季辉

  11. 生物大分子波谱学原理 吴季辉

  12. 生物大分子波谱学原理 吴季辉

  13. 生物大分子波谱学原理 吴季辉

  14. 生物大分子波谱学原理 吴季辉 7.3 13C－13C相关谱

  15. 生物大分子波谱学原理 吴季辉 7.3 13C－13C相关谱

  16. 生物大分子波谱学原理 吴季辉 7.3 13C－13C相关谱

  17. 生物大分子波谱学原理 吴季辉 7.3 13C－13C相关谱

  18. 生物大分子波谱学原理 吴季辉 7.3 13C－13C相关谱

  19. 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.

  20. 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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