TOCSY

1
TOCSY
?????????? ???
????TOCSY(total correlation spectroscopy)??HOHAHA
(homonuclear Hartmann-Hahn spectroscopy),?????????
?????
2
TOCSY
?????????? ???
3
TOCSY
MLEV-17
Spin Lock
Product Operator
Positive and absorptive diagonal cross peaks
for Z-filtered anisotropic TOCSY
4
TOCSY
?????????? ???
5
TOCSY
?????????? ???
?TOCSY????????????,?WALTZ-16,MLEV-17,DIPSI-2,
DIPSI-3?,???isotropic mixing sequence?????,???????
?? ?????????ROE??,????TOCSY???????????????,?
?????????ROE??,??NOE??,??????????ROE-2NOE,???????
???,???????????TOCSY????Clean-TOCSY?
6
TOCSY
?????????? ???

• C ?????
• ????COSY??????,??????????,??512????
• ?????????????????,??????,???????,??????20-30ms,???
  ?100ms???????????????????,??????????????????????,
  ?????????????????,??TOCSY??????????????
• ??TOCSY????,?????60-90????????

7
TOCSY
?????????? ???
8
TOCSY
?????????? ???
D ?? TOCSY????????????,?????,??????????
9
TOCSY-wagergate
?????????? ???
???, ??????90??(????)
10
TOCSY-doublewagergate
?????????? ???
d1?????????????,??WATERGATE?????
11
TOCSY-enhance mode
?????????? ???
180???
12
??? ????????
?????????? ???

• COSY???
• ????
• TOCSY
• NOESY
• ROESY

13
Selection of NOESY and ROESY
1000 3000
14
NOESY
?????????? ???
15
NOESY
?????????? ???
16
NOESY
Mixing time 80 of T1

17
NOESY
?????????? ???
18
NOESY
?????????? ???
19
NOESY
?????????? ???
20
NOESY
?????????? ???
C ????? ?TOCSY??,??????????,????NOESY?????,?
??????,???512-800???????????,???????????
??????????,?????????????,??????,?????,????,??????,
????????????????,???????,??????????????????(initia
l rate regime),??????????????????????????,????????
?????????6?????,??????????????????
???NOESY???????????????????????????,?????????????
??6????????,?????????????,?????????initial rate
regime???,????????????????????????????????,??????
???????????????????????,???????????,??????????????
?????????????????????????????,?????????????????
???????NOESY??????????????,???????,?????????,?
????100?ms?
21
NOESY
?????????? ???
?????????????????,???????,?????,?????????,???????
????????????????,??????????????,????????,?????????
????????????????????????????????,??????????m?????
?180???,??????????,?????????????180????????,?180??
?????t1????,????????? ??NOESY????,?????60-90?????
???
22
NOESY
?????????? ???
D ????? ???,????5??????????????NOE????NOESY??????
?,??????????????????????????,????????????,????????
?,?jump-and-return,??WATERGATE????????????
23
NOESY
?????????? ???
24
NOESY
?????????? ???
25
NOESY
?????????? ???
26
??? ????????
?????????? ???

• COSY???
• ????
• TOCSY
• NOESY
• ROESY

27
ROESY
?????????? ???
??????????????????????,??????,??????????????,?????
NOE????????????????????????????????ROESY???ROESY??
???????????????,?NOE??,ROE???????????,????NOE???,R
OE??????
28
ROESY
?????????? ???
29
ROESY
?????????? ???
30
ROESY
?????????? ???
31
ROESY
?????????? ???
32
ROESY
?????????? ???
C ????? ???????????TOCSY??????,?????????,???2-5kH
z,???????TOCSY??,?????????????????,??ROESY?????TOC
SY?? ?NOESY??,?????????,?ROE???NOE?????? ???????
??????NOESY???
33
ROESY
?????????? ???
D ?? ????????????,?????????????ROESY,??????ROESY?
???????,???ROESY??????????????,??????????????,????
??????,?????????????????????????????????? ?????,?
?????????????????
34
?????????
?????????? ???
???????????? (AX??) ??????????????????????4??
,??????DQF-COSY?????4????????????????2D?,???COSY,T
OCSY,NOESY?ROESY,???????,?4????????????? ??COSY???
???,?????????,????????????????,?????
35
?????????
?????????? ???
??COSY??????,?????????,????????????????,?????
????COSY?DQF-COSY,???????????????????????????
(??????)?,?????????????? ????????????????,???CO
SY,??COSY,DQF-COSY?????????????,???????,??????
36
?????????
?????????? ???
??TOCSY,NOESY?ROESY??????????????????????,??????
????? ???????????????,?TOCSY,NOESY?ROESY???????
????,??????????????
37
?????????
?????????? ???
??????????? ??COSY??256?FID, ??????1K?1K??????
??COSY??512?FID, ??????2K?2K?????? DQF-COSY??51
2?FID, ??????2K?2K?????? TOCSY ??256?FID,
??????1K?1K??????,?15ms?75ms NOESY ??256?FID,
??????1K?1K??????, ?150ms?250ms ROESY
??256?FID, ??????1K?1K??????,?150ms?250ms
????????????10000????????????,????COSY?DQF-COSY???
?????,????????,??????????
38
?????????
?????????? ???
?????2D???,?????? (receiver gain)
?????????????COSY??(??COSY,??COSY,DQF-COSY),?????F
ID?????????,?????FID??????,???FID(t10)???????????
????????????????????FID???,???????FID???,?????????
????????????????TOCSY,NOESY?ROESY??,?????FID????,?
????FID????????????????????????????FID???????
39
?????????
?????????? ???
????,NH-?H????????,??NH-?H??????????????????
1. ???????????????H??????????????NH-?H??????
??????????10?C, ????????,??H???????? 2.
??NH?H2O????,??????,??NH??????????????????????????
(?????),?????pH???????? 3.
????NH-?H????????????????????????????????????????
(????????????) ??????
40
?????
?????????? ???
????????????????,???????????????????????????? ???
??????????????????????????,??????,????????,??????
????,?????????J??????,?????????,????????????????
???????????????,?????????????????,??????????????,
?????????????????????????NOESY?TOCSY?????