Heteronuclear single-quantum correlation enhancements

Furthermore, the allohimachalane (see Section 13.11.9.1) <1999T14623> as well as boletunones A and B, highly functionalized sesquiterpenes from the fruit body of the mushroom Boletus calopus <20040L823>, have been characterized by 2D-NMR (heteronuclear single quantum correlation (HSQC), HMBC, and 111-COSY). The structure of a drimen-ll,12-acetonide, isolated from Maya s herb, was deduced by means of 111 and 13C NMR, distortionless enhancement by polarization transfer (DEPT), COSY, NOESY, HSQC, and HMBC analyses <2005MRC339>. 

Figure 2. Heteronuclear Single Quantum Correlation Spectra of I N-rCRALBP with and without 11-c/s-retinaldehyde. Results are shown from a gradient-enhanced sensitivity-enhanced heteronuclear single quantum correlation (GESE-HSQC) NMR experiment. The experiment correlates directly bonded pairs in rCRALBP. The correlation map for rCRALBP (29 mg/ml) with bound 11-c/s-retinaidehyde (heavy lines)...

L. Kay, P. Keifer, T. Saarinen, Pure absorption gradient enhanced heteronuclear single quantum correlation spectroscopy with improved sensitivity, J. Am. Chem. Soc. 114 (1992) 10663-10665. 

The vast literature associated with flavanoid chemistry precludes a discussion here but two valuable reviews have been published. The first reviews a number of spectroscopic techniques used for flavonoid analysis, with a strong emphasis on NMR spectroscopy (plus also mass spectrometry, vibrational spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, X-ray crystallography, and circular dichrosim (CD)) . The second review deals with NMR methods that have been successful in the characterization of phenolic acids and flavonoids from plant extracts that have not been separated or isolated as single components. The emphasis of the article is 2-D NMR methodology and a variety of experiments such as total correlated spectroscopy (TOCSY), COSY, nuclear Overhauser enhancement spectroscopy (NOESY) and heteronuclear multiple quantum correlation (HMQC) are discussed . 

Other strategies that show great promise in reducing NMR acquisition time utilise methods to obtain multiple sets of data from one experiment through a concept known as time-shared evolution. An example of this process that should find utility in natural products elucidation was demonstrated by a pulse sequence called CN-HMBC.93 Traditionally, a separate 13C-HMBC and 15N-HMBC were acquired independently. However, the CN-HMBC allows both 13C- and 15N-HMBC spectra to be obtained simultaneously. By acquiring both data sets simultaneously, an effective 50% time reduction can be achieved.93 This approach has also been demonstrated for a sensitivity-enhanced 2D HSQC-TOCSY (heteronuclear multiple bond correlation total correlation spectroscopy) and HSQMBC (heteronuclear single quantum... 

Heteronuclear multiple-quantum correlation Experiment for tailored correlation spectroscopy of H and H resonances in peptides and proteins Homonuclear Hartmann-Hahn spectroscopy Heteronuclear quadruple-quantum coherence Heteronuelear triple-quantum coherence Heteronuclear single-quantum coherence TOCSY sequences developed at the Indian Institute of Chemical Technology Insensitive nucleus enhancement by polarization transfer... 

More recently, a gradient-enhanced heteronuclear single quantum multiple bond correlation (HSQMBC) experiment and its variants34,47,60-62 have been proposed for the measurement of heteronuclear coupling... 

FIGURE 8.2. Flowchart for structure elucidation of purified compounds. DEPT Distortionless Enhancement by Polarization Transfer, HMBC Heteronuclear Multiple Bond Correlation, HSQC Heteronuclear Single Quantum Coherence, HMQC Heteronuclear Multiple Quantum Correlation, DQF-CQSY Double Quantum Filtered Correlated Spectroscopy and NOSEY Nuclear Overhauser effect spectroscopy. 

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