th - 1987 - 51st ENC Conference
th - 1987 - 51st ENC Conference
th - 1987 - 51st ENC Conference
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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.