C8953 NMR strukturní analýza seminář
TOCSY & ROESY
Jan Novotný
17 6003@is.muni.cz
April 3, 2019
TOCSY (TOtal Correlation Spectroscopy)
spin lock - isotropic mixing
► series of short 180° pulses
► "lock-in" of spins in transversal plane
► higher power in case of TOCSY, offset set into the middle (on resonance)
► smaller power in case of ROESY, offset set into the edge (off resonance)
► crosstalk (ROE transfer in TOCSY, J-coupling in ROESY)
TOCSY (TOtal Correlation Spectroscopy)
correlation based on J
► mutual correlation of all protons in one spin system
► rmix « 20 - 120ms
► crosspeak intensity depends on rmix a J value
u   Jabj I I    Jbc - -    Jcq - -
NAD+:TOCSY (40ms)
82 - 1H (ppm)
NAD+: TOCSY (40ms), detail of aromatics
9.0 8.5 82 - 1H (ppm)
NAD+: TOCSY (40ms), detail of aliphatics
6.5
4.5-
E 5.0-
Cl
CL
5.5-
6.0-
6.5
6.0
6.0
5.5
5.0
5.5 5.0 52 - 1H (ppm)
4.0
■4.5
0-Nic
4
5 ^^3.
*NH2
8
o       31I2'
■5.0
OH OH
10
NH2
Ade 0=P-0
L O
ľ     c    16
■5.5
4'
97 N
ľ
3| |2-OH OH
■6.0
0 »
4.5
4.0
□ ť3? - =
NOESY - Palmatine
ROESY - Glutathione
CL CL
to 6
6 4 82 - 1H (ppm)
Next session:
Heteronuclear correlations