Gradient submicro inverse detection: rapid acquisition of inverse-detected heteronuclear chemical shift correlation data on submicromole quantities of material

✍ Scribed by Gary E. Martin; Ronald C. Crouch; Albert P. Zens

• Publisher: John Wiley and Sons
• Year: 1998
• Tongue: English
• Weight: 240 KB
• Volume: 36
• Category: Article
• ISSN: 0749-1581
• DOI: 10.1002/(sici)1097-458x(199807)36:7<551::aid-omr332>3.0.co;2-f

✦ Synopsis

Micro NMR probes require substantially reduced quantities of sample for spectral characterization relative to traditional 5 mm probes. In addition, 3 mm micro probes have also made it feasible to routinely acquire inverse-detected heteronuclear shift correlation data on submicromole quantities. This paper reports the development and initial testing of a 1.7 mm submicro gradient inverse-detection probe. The further reductions in the sample volume required relative even to the combination of 3 mm micro probes and Shigemi micro NMR sample cells make it feasible to acquire heteronuclear shift correlation data on submicromole quantities of material in very short periods of time. Results obtained using a 0.55 lmol sample of the model alkaloid cryptolepine dissolved in 25 ll of solvent are described. Using submicro probe technology, GHSQC data were acquired on the 0.55 lmol sample of cryptolepine dissolved in 25 ll as rapidly as 12 min and GHMBC data were recorded in 1.1 h. 1998 ( John Wiley & Sons, Ltd.