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Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

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Page 1: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Protein in solution

Radio waves

1H 800 MHz13C 200 MHz15N 80 MHz

Spectra

Principles of NMR Protein Spectroscopy

Bo 18.79 T

Frequencies and Spectra

Page 2: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

How would the 1H NMR spectrum appear?

H

HH

H

H

NH

O

O

HN

H

H

CH3

HH

Ala Phe

10 9 8 7 6 5 4 3 2 1 0 ppm

Page 3: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

- NMR is very sensitive to environment

H

HH

H

H

NH

O

O

HN

H

H

CH3

HH

Ala Phe

electronic, bonding

small differences in for each nucleus in molecule

B0

2(Hz)

s = B0

2

ActualGeneral = B0

2(Hz)

is shielding constantcan or of nucleus

-same for 13C, 15N

Chemical Shift

Page 4: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

B0

2(Hz) - resonance condition (field + local)

s = B0

2

Chemical Shift

B=Bo(1-) = B0

2recall

=d +p +m +r +e +s

d = e2

3me

re dr0

8

Page 5: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

each nucleus has unique chemical shift

H

HH

H

H

NH

O

O

HN

H

H

CH3

HH

Ala Phe

10 9 8 7 6 5 4 3 2 1 0 ppm

similar for 13C, 15N

1H spectrum

Page 6: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

Chemical Shift

4.80 ppm

= 106 sample - ref ppmref

ref = internal standard (0 ppm)

1H @ 14.09T sample= 599.2933272 MHzDSS DSS = 599.2904502 MHz

= 4.80 ppmFactors out B0 - is same at any B

DSS - dimethyl-silapentane-sulphonate

2877

Page 7: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Principles of NMR Protein Spectroscopy

Chemical Shift

DSS 1H @ 14.09T, DSS= 599.2904502 MHz

010

070

13C @ 14.09T ref = 13C * DSS 1H

=150.6913020

Page 8: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Chemical Shifts of Proteins

1H spectrum

In generalnuclei found in “ranges” of chemical shift

10 9 8 7 6 5 4 3 2 1 0 ppm

NH

Aromatics

HH

CH3

100 90 80 70 60 50 40 30 20 10 0 ppm

C C CH3

13C spectrum C

Principles of NMR Protein Spectroscopy

Page 9: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Protein Database

BioMagResBank

http://www.bmrb.wisc.edu/ Reference

Reference Information Chemical Shift Statistics Derived from the BMRB Database for: Restricted Set of Protein Chemical Shifts Full Set of Protein Chemical Shifts Restricted Set of DNA Chemical Shifts Full Set of DNA Chemical Shifts Restricted Set of RNA Chemical Shifts Full Set of RNA Chemical Shifts

Principles of NMR Protein Spectroscopy

http://www.bmrb.wisc.edu/ref_info/statful.htm
Page 10: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

BioMagResBank

actual chemical shifts for each amino acid are differentdependence on placement in sequence and secondary structure

Example

H

HH

H

H

NH

O

O

HN

H

H

CH3

HH

Ala Phe

8.19

7.03-7.11

4.61

4.261.37 8.39

2.97, 3.00

Principles of NMR Protein Spectroscopy

Page 11: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Spin-spin Coupling

Principles of NMR Protein Spectroscopy

A ABAB

= B0

2B0

2+J

J

Page 12: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Spin-spin Coupling

Principles of NMR Protein Spectroscopy

1H(15N)

1H-1H 0-20 Hz1H-13C 125-160 Hz1H-15N ~ 93 Hz

2nI +1 lines

13C(1H)

93 Hz 143 Hz

-CH3-NH

Page 13: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Spin-spin Coupling

Principles of NMR Protein Spectroscopy

1H-1H 0-20 Hz

H

HH

H

H

NH

O

O

HN

H

H

CH3

HH

3J

3J = 6.98cos2 - 1.38cos +1.72

= - 60˚

Page 14: Protein in solution Radio waves 1 H 800 MHz 13 C 200 MHz 15 N 80 MHz Spectra Principles of NMR Protein Spectroscopy B o 18.79 T Frequencies and Spectra

Other Coupling

Principles of NMR Protein Spectroscopy

D = || (3cos2 - 1)

Dipolar Interaction

2

|| = - 12h

42r3

Bo r12


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