06.12.2012 Views

th  - 1987 - 51st ENC Conference

th  - 1987 - 51st ENC Conference

th  - 1987 - 51st ENC Conference

SHOW MORE
SHOW LESS

Create successful ePaper yourself

Turn your PDF publications into a flip-book with our unique Google optimized e-Paper software.

MK23<br />

MATER SUPPRESSION TECHNIQUES FOR THE GENERATION OF PURE PHASE<br />

TWO-DIMENSIONALNMR SPECTRA<br />

Vladlmlr Sklenar* and Ad Bax*<br />

Laboratory of Chemical Physics, Natlonal Institute of Diabetes<br />

Digestive and Kidney Diseases, National Institutes of Heal<strong>th</strong><br />

Be<strong>th</strong>esda,MD.20892<br />

A number of different approaches has been proposed for suppression of<br />

<strong>th</strong>e intense H20 resonance in 2D NMR spectra of biological compounds. Most<br />

commonly one employs presaturatlon of <strong>th</strong>e H~O resonance using a low power<br />

irradiation prior to <strong>th</strong>e observation pulse. The main disadvantage of <strong>th</strong>is<br />

me<strong>th</strong>od is <strong>th</strong>at resonances of exchangeable protons may also be saturated.<br />

Selective excitation using pulse sequences which have a null at <strong>th</strong>e water<br />

resonance avoids <strong>th</strong>is problem. A large variety of different excitation<br />

schemes has been designed in recent years. However, all but <strong>th</strong>e slmplest<br />

90x-T-90_x sequence yield spectra <strong>th</strong>at require a large linear phase<br />

correction. The baseline roll <strong>th</strong>at result from such a phase correction can<br />

lead to intense artifacts in phase sensitive 2D NMR spectra.<br />

A new approach is described for water suppression in one- and<br />

two-dlmensional NMRwhlch generates pure absorptive spectra <strong>th</strong>at are free<br />

of baseline dlstorslons. This me<strong>th</strong>od involves <strong>th</strong>e use of a 90x-~-90_x<br />

hard pulse as a read pulse followed by a 90~-k~-90.~ refocusing pulse<br />

which is phase cycled for obtaining <strong>th</strong>e highest possible water<br />

suppression. Incorporation into several of <strong>th</strong>e most popular 2D NHR<br />

experiments (NOESY, HOHAHA, ROESY, HMQC and COSY) is discussed in detail.<br />

Examples of <strong>th</strong>is approach for selective water suppression are demonstrated<br />

by recording <strong>th</strong>e 2D spectra of <strong>th</strong>e decapeptide LH-RH and <strong>th</strong>e Dickerson<br />

dodecamer in 90% H20.

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!