Laura Casta ña r Acedo Small Molecule NMR Conference September 11 th 14 th 2016 La Jolla California USA NMR Methodology group The University of Manchester 1 Simplified NMR spectra ID: 1012390
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1. PSYCHE pure shift NMR:spectral simplification and its applicationsLaura Castañar AcedoSmall Molecule NMR ConferenceSeptember 11th -14th, 2016La Jolla, California, USA. NMR Methodology groupThe University of Manchester
2. 1Simplified NMR spectraEnhanced signal resolutionPROBLEM Signal overlap &poor spectral resolutionSOLUTION1H Broadband homodecoupled spectrumCollapsing of typical JHH coupling multiplicity to singletsIntroduction Pure shift NMR
3. 2BroadbandSensitivity1.1%0.5-5%100%10-20%J-refocusing elementIntroduction Pure shift NMR
4. Selective pulses > 20 msPSYCHEIntroduction Pure Shift NMR3Acquisition modet << 1/JHHInterferogram Real timet ≡ 1/SW11/SW1 << 1/JHH
5. Introduction PSYCHE4M. Foroozandeh, R. W. Adams, N. J. Meharry, D. Jeannerat, M. Nilsson, G. A. Morris, Angew. Chem. Int. Ed. 2014, 53, 6990.1H NMR1D PSYCHEZSEstradiolPure Shift Yielded by CHirp Excitation (PSYCHE)Selective inversion element
6. 5Results and discussion Implementing PSYCHE in 1D & 2D experimentsOneshot-PSYCHE DOSYSelective 1D TOCSY-PSYCHEF1-PSYCHE-CLIP-COSYSpectral simplificationHigher signal resolutionPractical applicationsAnalysis of mixturesStructure determination of complex moleculesF1-PSYCHEF2-PSYCHE [interferogram]
7. Mixture analysis: Oneshot DOSYMisleading peaks!!Signal overlap6Results and discussion Oneshot-PSYCHE DOSYM. D. Pelta, G. A. Morris, M. J. Stchedroff, S. J. Hammond, Magn. Reson. Chem. 2002, 40, S147.
8. 7Mixture analysis: Oneshot-PSYCHE DOSYResults and discussion Oneshot-PSYCHE DOSYSpectral simplificationHigher signal resolutionUnpublished
9. 7Mixture analysis: Oneshot-PSYCHE DOSYResults and discussion Oneshot-PSYCHE DOSYUnpublishedCorrect diffusion coefficients
10. 8Results and discussion Selective 1D TOCSY-PSYCHEMixture analysis: peppermint oil
11. ???Mixture analysis: selective 1D TOCSY9Results and discussion Selective 1D TOCSY-PSYCHESelective excitationM. J. Thrippleton, J. Keeler, Angew. Chem. Int. Ed. 2003, 42, 3938.
12. 10Mixture analysis: selective 1D TOCSY-PSYCHEConventionalPure shiftResults and discussion Selective 1D TOCSY-PSYCHEUnpublished
13. 11CLean In-Phase COSYM. R. M. Koos, G. Kummerlöwe, L. Kaltschnee, C. M. Thiele, B. Luy, Angew. Chem. Int. Ed. 2016, 55, 765.D=10-15msCOSY (mc)DQF-COSY (ph)CLIP-COSY (ph)Results and discussion F1-PSYCHE-CLIP-COSY
14. 12PSYCHE-CLIP-COSYF2-CLIP-COSY-PSYCHEResults and discussion F1-PSYCHE-CLIP-COSYM. R. M. Koos, G. Kummerlöwe, L. Kaltschnee, C. M. Thiele, B. Luy, Angew. Chem. Int. Ed. 2016, 55, 765.F1-PSYCHE-CLIP-COSYUnpublished
15. 13F1-PSYCHE-CLIP-COSYCLIP-COSYF1-PSYCHE-CLIP-COSYF1-PSYCHE-CLIP-COSY+ CovarianceResults and discussion F1-PSYCHE-CLIP-COSYEstradiolUnpublished
16. 14Results and discussion F1-PSYCHE-CLIP-COSYUnpublishedF1-PSYCHE-CLIP-COSY[n=1]F1-PSYCHE-CLIP-COSY & RELAYEstradiol
17. 14Results and discussion F1-PSYCHE-CLIP-COSYEstradiolUnpublishedF1-PSYCHE-CLIP-COSY & RELAYF1-PSYCHE-CLIP-COSY[n=1]F1-PSYCHE-RELAY[n=2]
18. Summary & ConclusionsPSYCHE pure shift NMR Spectral simplification Higher signal resolution Reduced signal overlapPure shift spectra of individual components in intact complex mixturesMixture analysis Structure determinationOneshot-PSYCHE DOSY Selective 1D PSYCHE-TOCSY F1-PSYCHE-CLIP-COSY & RELAYCombination with covariance processingUltra-high resolution phase-sensitive COSYMinimises misleading peaksCorrect diffusion coefficients15
19. AcknowledgmentsProf. Gareth. A. Morris Dr. Mathias NilssonManchester NMR Methodology Grouphttp://nmr.chemistry.manchester.ac.uk/Dr. Mohammadali Foroozandeh Guilherme Dal PoggettoDr. Ralph W. AdamsDr. Peter KiralyPinelopi MoutzouriAaron Hernandez-Cid
20. Thank you very much for your attention