Free to Read
How the 1D-NOESY suppresses solvent signal in metabonomics NMR spectroscopy: An examination of the pulse sequence components and evolution
Ryan T. Mckay,
Corresponding Author
Ryan T. Mckay
National High Field NMR Centre (NANUC), University of Alberta, Edmonton, Alberta, Canada T6G 2E1
National High Field NMR Centre (NANUC), University of Alberta, Edmonton, Alberta, Canada T6G 2E1Search for more papers by this authorRyan T. Mckay,
Corresponding Author
Ryan T. Mckay
National High Field NMR Centre (NANUC), University of Alberta, Edmonton, Alberta, Canada T6G 2E1
National High Field NMR Centre (NANUC), University of Alberta, Edmonton, Alberta, Canada T6G 2E1Search for more papers by this authorAbstract
Metabonomics has become an increasingly shared pursuit in international research. Presently the two most common techniques are mass spectrometry and nuclear magnetic resonance (NMR) spectrometry either in isolation or in conjunction. The 1D-1H-NOESY is the most utilized (Beckonert et al., Nat Protoc 2007;2:2692–2703) NMR pulse sequence for the collection of metabonomics NMR data from biological samples such as blood plasma, serum, urine, cerebrospinal fluid, sputum, or homogenized tissue extracts. While the 1D version of the 2D-1H,1H-NOESY pulse sequence has become widely used in metabonomics studies, the understanding of the mechanism of solvent suppression has not kept pace. This article will examine the mechanisms by which the 1D-NOESY suppresses solvent signals and detail the pulse sequence's components in terms of function, phase cycle, and performance. © 2011 Wiley Periodicals, Inc. Concepts Magn Reson Part A 38: 197–220, 2011.
REFERENCES
- 1 Kovacs H,Moskau D,Spraul M. 2005. Cryogenically cooled probes—a leap in NMR technology. Progr NMR Spectrosc 46: 131–155.
- 2 Foxall PJ,Spraul M,Farrant RD,Lindon LC,Neild GH,Nicholson JK. 1993. 750 MHz 1H-NMR spectroscopy of human blood plasma. J Pharm Biomed Anal 11: 267–276.
- 3 Daviss B. 2005. Growing pains for metabolomics. Scientist 19: 25–28.
- 4 Altieri A,Miller K,Byrd A. 1996. A comparison of water suppression techniques using pulsed field gradients for high-resolution NMR of biomolecules. Magn Reson Rev 17: 27–82.
- 5 Freeman R. 1998. Spin Choreography: Basic Steps in High Resolution NMR. Oxford, UK: Oxford University Press. 391 p.
- 6 Gueron M,Plateau P,Decops M. 1991. Solvent signal suppression in NMR. Progr NMR Spectrosc 23: 135–209.
- 7 Hore PJ. 1983. Solvent suppression in fourier transform nuclear magnetic resonance. J Magn Reson 55: 283–300.
- 8 Hore PJ. 1989. Nuclear magnetic resonance. Solvent suppression. Methods Enzymol 176: 64–77.
- 9 Liu M,Mao X-A. 1999. Solvent suppression methods in NMR spectroscopy. In: JC Lindon, GE Tranter, JL Holmes, eds. Encylopedia of Spectroscopy and Spectrometry. Vols. 1 and 2. Academic Press. pp 2145–2152.
- 10 Price WS. 1999. Water signal suppression in NMR spectroscopy. Annu Rep NMR Spectrosc 38: 289–354.
- 11 McKay RT. 2009. Recent advances in solvent suppression for solution NMR: a practical reference. In: G Webb, ed. Vol. 66, Elsevier, pp 33–74.
- 12 Zheng G,Price WS. 2010. Solvent signal suppression in NMR. Prog Nucl Magn Reson Spectrosc 56: 267–288.
- 13 Kauzmann W. 1959. Some factors in the interpretation of protein denaturation. Adv Protein Chem 14: 1–63.
- 14 Edsall JT,McKenzie HA. 1978. Water and proteins. I. The significance and structure of water; its interaction with electrolytes and non-electrolytes. Adv Biophys 10: 137–207.
- 15 Edsall JT,McKenzie HA. 1983. Water and proteins. II. The location and dynamics of water in protein systems and its relation to their stability and properties. Adv Biophys 16: 53–183.
- 16 Patt SL,Sykes BD. 1972. Water eliminated Fourier transform NMR spectroscopy. J Chem Phys 56: 3182–3184.
- 17 Liu M,Tang H,Nicholson JK,Lindon JC. 2001. Recovery of underwater resonances by magnetization transferred NMR spectroscopy (RECUR-NMR). J Magn Reson 153: 133–137.
- 18 Barjat H,Mattiello DL,Freeman R. 1999. Suppression of radiation damping in high-resolution NMR. J Magn Reson 136: 114–117.
- 19 Bloembergen N,Pound RV. 1954. Radiation damping in magnetic resonance experiments. Phys Rev 95: 8–12.
- 20 Böckmann A,Guittet E. 1996. Suppression of radiation damping during selective excitation of the water signal: the WANTED sequence. J Biomol NMR 8: 87–92.
- 21 Cutting B,Chen JH,Moskau D,Bodenhausen G. 2000. Radiation damping compensation of selective pulses in water-protein exchange spectroscopy. J Biomol NMR 17: 323–330.
- 22 Mao X,Chen J. 1996. Radiation damping effects in solvent preirradiation experiments in NMR. Chem Phys 202: 357–366.
- 23 Price WS,Hayamizu K,Arata Y. 1997. Optimization of the water-PRESS pulse sequence and its integration into pulse sequences for studying biological macromolecules. J Magn Reson 126: 256–265.
- 24 Sweeting LM. 1982. The recovery-preparation time in pulsed FT NMR experiment. J Magn Reson 48: 311–313.
- 25 Grzesiek S,Bax A. 1993. The importance of not saturating H2O in protein NMR. Application to sensitivity enhancement and NOE measurements. J Am Chem Soc 115: 12593–12594.
- 26 Lauridsen M,Maher AD,Keun H,Lindon JC,Nicholson JK,Nyberg NT,Hansen SH,Cornett C,Jaroszewski JW. 2008. Application of the FLIPSY pulse sequence for increased sensitivity in 1H NMR-based metabolic profiling studies. Anal Chem 80: 3365–3371.
- 27 Inubushi T,Becker ED. 1983. Efficient detection of paramagnetically shifted NMR resonances by optimizing the WEFT pulse sequence. J Magn Reson 51: 128–133.
- 28 Mirau PA. 1987. Selective water attenuation by T2 and T1 relaxation in one- and two-dimensional NMR. J Magn Reson 73: 123–133.
- 29 Beckonert O,Keun HC,Ebbels TM,Bundy J,Holmes E,Lindon JC,Nicholson JK. 2007. Metabolic profiling, metabolomic and metabonomic procedures for NMR spectroscopy of urine, plasma, serum and tissue extracts. Nat Protoc 2: 2692–2703.
- 30 Reynolds WF,Enriquez RG. 2002. Choosing the best pulse sequences, acquisition parameters, postacquisition processing strategies, and probes for natural product structure elucidation by NMR spectroscopy. J Nat Prod 65: 221–244.
- 31 Wishart DS,Bigam CG,Yao J,Abildgaard F,Dyson HJ,Oldfield E,Markley JL,Sykes BD. 1995. 1H, 13C and 15N chemical shift referencing in biomolecular NMR. J Biomol NMR 6: 135–140.
- 32 Markley JL,Bax A,Arata Y,Hilbers CW,Kaptein R,Sykes BD,Wright PE,Wuthrich K. 1998. Recommendations for the presentation of NMR structures of proteins and nucleic acids. IUPAC-IUBMB-IUPAB inter-union task group on the standardization of data bases of protein and nucleic acid structures determined by NMR spectroscopy. J Biomol NMR 12: 1–23.
- 33 Evans JNS. 1995. Biomolecular NMR Spectroscopy. Oxford, UK: Oxford University Press.
- 34 Cavanagh J,Fairbrother WJ,Palmer AGIII,Skelton NJ. 2006. Protein NMR Spectroscopy: Principles and Practice, 2nd ed. Elsevier Academic Press. 885 p.
- 35 Homans SW. 1995. A dictionary of concepts in NMR. In: RA Dwek, editor. Biophysical Techniques Series. Oxford, UK:Oxford University Press.
- 36 Keifer PA. 1999. 90° pulse width calibrations: how to read a pulse width array. Concept Magn Reson 11: 165–180.
- 37 Levitt MH. 1996. Composite pulses. In: DMG Harris, ARK, eds. Encyclopedia of Nuclear Magnetic Resonance, Wiley. pp 1396–1410.
- 38 Wu PS,Otting G. 2005. Rapid pulse length determination in high-resolution NMR. J Magn Reson 176: 115–119.
- 39 Augustine M,Zilm K. 1996. Observation of bulk susceptibility effects in high-resolution nuclear magnetic resonance. J Magn Reson A123: 145–156.
- 40 Dalvit C,Pevarello P,Tato M,Veronesi M,Vulpetti A,Sundstrom M. 2000. Identification of compounds with binding affinity to proteins via magnetization transfer from bulk water. J Biomol NMR 18: 65–68.
- 41 Jerschow A. 1999. Unwanted signal leakage in excitation sculpting with single axis gradients. J Magn Reson 137: 206–214.
- 42 Levitt MH. 1996. Demagnetization field efects in two-dimensional solution NMR. Concepts Magn Reson 8: 77–103.
- 43 Luo J,He X,d'Avignon DA,Ackerman JJ,Yablonskiy DA. 2010. Protein-induced water 1H MR frequency shifts: contributions from magnetic susceptibility and exchange effects. J Magn Reson 202: 102–108.
- 44 McKay RT,Mercier P,Sykes BD. 2009. Comparative analysis of solvent suppression techniques and improvements for high resolution 1H NMR metabonomics studies. Experimental Nuclear Magnetic Resonance Conference, Pacific Grove, CA, U.S.A, Poster 226.
- 45 Szantay C,Demeter A. 1999. Radiation damping diagnostics. Concepts Magn Reson 11: 121–145.
- 46 Donne DG,Gorenstein DG. 1997. A pictorial representation of product operator formalism: nonclassical vector diagrams for multidimensional NMR. Concepts Magn Reson 9: 95–111.
- 47 Abragam A. 1961. Principles of nuclear magnetism. Int Ser Monographs Phys 32: 599.
- 48 Levitt MH,Freeman R. 1981. Compensation for pulse imperfections in NMR spin-echo experiments. J Magn Reson 43: 65–80.
- 49 Sinha N,Schmidt-Rohr K,Hong M. 2004. Compensation for pulse imperfections in rotational-echo double-resonance NMR by composite pulses and EXORCYCLE. J Magn Reson 168: 358–365.
- 50 Kumar A,Ernst RR,Wuthrich K. 1980. A two-dimensional nuclear Overhauser enhancement (2D NOE) experiment for the elucidation of complete proton-proton cross-relaxation networks in biological macromolecules. Biochem Biophys Res Commun 95: 1–6.
- 51 Saude EJ,Slupsky CM,Sykes BD. 2006. Optimization of NMR analysis of biological fluids for quantitative accuracy. Metabolomics 2: 113–123.
- 52 Szantay C. 1998. Analysis and implications of transition-band signals in high-resolution NMR. J Magn Reson 135: 334–352.
- 53 Mo H,Raftery D. 2008. Improved residual water suppression: WET180. J Biomol NMR 41: 105–111.
- 54 Mo H,Raftery D. 2008. Pre-SAT180, a simple and effective method for residual water suppression. J Magn Reson 190: 1–6.
- 55 Altieri AS,Byrd RA. 1995. Randomization approach to water suppression in multidimensional NMR usingpulsed field gradients. J Magn Reson B 107: 260–266.
- 56 Canet D,Brondeau J,Mischler E,Humbert F. 1993. Solvent suppression by use of a DANTE train of B1-gradient pulses. J Magn Reson A105: 239–244.
- 57 Hwang T,Shaka A. 1995. Water supression that works. Excitation sculpting using arbitrary waveforms and pulsed field gradients. J Magn Reson 112A: 275–279.
- 58 Kay LE. 1995. Field gradient techniques in NMR spectroscopy. Curr Opin Struct Biol 5: 674–681.
- 59 Zheng G,Torres AM,Price WS. 2008. Solvent suppression using phase-modulated binomial-like sequences and applications to diffusion measurements. J Magn Reson 194: 108–114.
- 60 Thomas DJ,Mitschang L,Simon B,Oschkinat H. 1999. Signal selection in high-resolution NMR by pulsed field gradients. J Magn Reson 137: 10–24.
- 61 Keeler J. 2005. Understanding NMR Spectroscopy. Chichester: Wiley.
- 62 Bodenhausen G,Freeman R,Turner DL. 1977. Suppression of artifacts in two-dimensional j spectroscopy. J Magn Reson 27: 511–514.
- 63 Wu PS,Otting G. 2005. SWET for secure water suppression on probes with high quality factor. J Biomol NMR 32: 243–250.
- 64 Jahnke W,Kessler H. 1994. Enhanced sensitivity of rapidly exchanging amide protons by improved phase cycling and the constructive use of radiation damping. J Biomol NMR 4: 735–740.
- 65 Jahnke W,Baur M,Gemmecker G,Kessler H. 1995. Improved accuracy of NMR structures by a modifiedNOESY-HSQC experiment. J Magn Reson 106B: 86–88.
- 66 Gregory RM,Bain AD. 2009. The effects of finite rectangular pulses in NMR: phase and intensity distortions for a spin-1/2. Concept Magn Reson A 34A: 305–314.
- 67
Freeman DM,Hurd R.
1997.
Decoupling: theory and practice. II. State of the art: in vivo applications of decoupling.
NMR Biomed
10:
381–393.
10.1002/(SICI)1099-1492(199712)10:8<381::AID-NBM495>3.0.CO;2-7 CAS PubMed Web of Science® Google Scholar
- 68 Levitt MH. 1982. Broadband heternuclear decoupling. J Magn Reson 47: 328–330.
- 69 Levitt MH. 1982. Symmetrical composite pulse sequences for NMR population inversion. I. compensation of radiofrequency field inhomogeneity. J Magn Reson 48: 234–264.
- 70 Levitt MH. 1986. Composite pulses. Prog Nucl Magn Reson Spectrosc 18: 61–122.
- 71 Levitt MH. 1982. Symmetrical composite pulse sequences for NMR population inversion. II. Compensation of resonance offset. J Magn Reson 50: 95–110.
- 72 Botana A,Aguilar JA,Nilsson M,Morris GA. 2011. J-Modulation effects in DOSY experiments and their suppression: the Oneshot45 experiment. J Magn Reson 208: 270–278.
- 73 Cotts RM,Hoch MJR,Sun T,Markert JT. 1989. Pulsed field gradient stimulated echo methods for improved NMR diffusion measurements in heterogeneous systems. J Magn Reson 83: 252–266.
- 74 Jerschow A,Muller N. 1997. Suppression of convection artifacts in stimulated-echo diffusion experiments. Double-stimulated-echo experiments. J Magn Reson 125: 372–375.
- 75 Johnson CS. 1999. Diffusion ordered nuclear magnetic resonance spectroscopy: principles and applications. Progr NMR Spectrosc 34: 203–256.
- 76 Karlicek RF. 1980. A modified pulsed gradient technique for measuring diffusion in the presence of large background gradients* 1. J Magn Reson 37: 75–91.
- 77 Momot KI,Kuchel PW. 2004. Convection-compensating PGSE experiment incorporating excitation-sculpting water suppression (CONVEX). J Magn Reson 169: 92–101.
- 78 Price WS. 1997. Pulsed-field gradient nuclear magnetic resonance as a tool for studying translational diffusion: part 1. Basic theory. Concepts Magn Reson 9: 299–336.
- 79 Price WS,Stilbs P,Jonsson B,Soderman O. 2001. Macroscopic background gradient and radiation damping effects on high-field PGSE NMR diffusion measurements. J Magn Reson 150: 49–56.
- 80 Sarkar R,Moskau D,Ferrage F,Vasos PR,Bodenhausen G. 2008. Single or triple gradients? J Magn Reson 193: 110–118.
- 81 Simorellis AK,Flynn PF. 2004. A PFG NMR experiment for translational diffusion measurements in low-viscosity solvents containing multiple resonances. J Magn Reson 170: 322–328.
- 82 Stilbs P. 1987. Fourier transform pulsed-gradient spin-echo studies of molecular diffusion. Prog NMR Spectrosc 19: 1–45.
- 83 Sun PZ,Seland JG,Cory D. 2003. Background gradient suppression in pulsed gradient stimulated echo measurements. J Magn Reson 161: 168–173.
- 84 Torres AM,Zheng G,Price WS. 2010. J-compensated PGSE: an improved NMR diffusion experiment with fewer phase distortions. Magn Reson Chem 48: 129–133.
- 85 Zheng G,Price WS. 2009. Simultaneous convection compensation and solvent suppression in biomolecular NMR diffusion experiments. J Biomol NMR 45: 295–299.
- 86 Zheng G,Stait-Gardner T,Anil Kumar PG,Torres AM,Price WS. 2008. PGSTE-WATERGATE: an STE-based PGSE NMR sequence with excellent solvent suppression. J Magn Reson 191: 159–163.
- 87 Zheng G,Price WS. 2007. Suppression of background gradients in (Bo gradient based) NMR diffusion experiments. Concept Magn Reson 30A: 261–277.
- 88 Lam B,Simpson AJ. 2008. Direct (1)H NMR spectroscopy of dissolved organic matter in natural waters. Analyst 133: 263–269.
- 89 Wu D,Chen A,Johnson CS. 1995. An improved diffusion-ordered spectroscopy experiment incorporating bipolari-gradient pulses. J Magn Reson 115A: 260–264.
- 90 Simpson AJ,Brown SA. 2005. Purge NMR: effective and easy solvent suppression. J Magn Reson 175: 340–346.
- 91 Nguyen BD,Meng X,Donovan KJ,Shaka AJ. 2007. SOGGY: solvent-optimized double gradient spectroscopy for water suppression. A comparison with some existing techniques. J Magn Reson 184: 263–274.
