Chinese Journal of Magnetic Resonance >
Heating of Biological Samples in Studies of MAS Solid-State NMR
Received date: 2014-04-17
Revised date: 2015-01-11
Online published: 2015-03-05
Supported by
国家自然科学基金资助项目(21075133, 21173259).
Magic-angle-spinning (MAS) solid-state NMR studies of biomolecules involve application of rapid sample rotation and radiofrequency pulsing, both of which can increase the sample temperature significantly, causing distorted spectra, sample dehydration and even sample degradation. In this review, the mechanisms leading to bio-sample heating in MAS solid-state NMR experiments are first introduced. The importance of sample temperature monitoring is then emphasized. Finally, we present the methods that can be used to to alleviate the problem, including optimization of sample preparation, selecting
optimal NMR parameters, and improving NMR spectrometer hardware such as the probes.
Key words: solid-state NMR; sample heating; magic angle spinning; radiofrequency
TANG Xin-qi1 , 2 , ZHANG Zheng-feng1 , YANG Jun1* . Heating of Biological Samples in Studies of MAS Solid-State NMR[J]. Chinese Journal of Magnetic Resonance, 2015 , 32(1) : 123 -140 . DOI: 10.11938/cjmr20150114
[1] ZHANG Zhen-feng(张正逢), Yang Jun(杨俊). Solid-state NMR studies on amyloid fibrils: recent progresses(固体核磁共振研究淀粉样蛋白纤维的进展)[J]. Chinese J Magn Reson(波谱学杂志), 2013, 30(2): 157-174.
[2] Fu Ri-qiang(傅日强). High-resolution solid-state NMR spectroscopy of membrane bound proteins and peptides aligned in hydrated lipids(水化磷脂层中蛋白质和多肽的高分辨固体核磁共振波谱学)[J]. Chinese J Magn Reson(波谱学杂志). 2009, 26(4): 437-456.
[3] Ladizhansky V, Vega S. Polarization transfer dynamics in Lee–Goldburg cross polarization nuclear magnetic resonance experiments on rotating solids[J]. J Chem Phys, 2000, 112(16): 7 158-7 168.
[
4] Dvinskikh S V, Zimmermann H, Maliniak A, et al. Heteronuclear dipolar recoupling in liquid crystals and solids by PISEMA-type pulse sequences[J]. J Magn Reson, 2003, 164(1): 165-170.
[5] Oldfield E, Meadows M, Rice D, et al. Spectroscopic studies of specifically deuterium labeled membrane systems. Nuclear magnetic resonance investigation of the effects of cholesterol in model systems[J]. Biochemistry, 1978, 17(14): 2 727-2 740.
[6] Stringer J A, Bronnimann C E, Mullen C G, et al. Reduction of RF-induced sample heating with a scroll coil resonator structure for solid-state NMR probes[J]. J Magn Reson, 2005, 173(1): 40-48.
[7] Wu Z, Ding S. Prevention of spinning induced sample deterioration during long time solid-state NMR experiments of quadrupolar spin systems[J]. Solid State Nucl Magn Reson, 2009, 35(4): 214-216.
[8] Wang A C, Bax A. Minimizing the effects of radio-frequency heating in multidimensional NMR experiments[J]. J Biomol NMR, 1993, 3(6): 715-720.
[9] Kugel H. Improving the signal-to-noise ratio of NMR signals by reduction of inductive losses[J]. J Magn Reson, 1991, 91(1): 179-185.
[10] Led J J, Petersen S B. Heating effects in 13C NMR spectroscopy on aqueous solutions caused by proton noise decoupling at high frequencies[J]. J Magn Reson, 1978, 32(1): 1-17.
[11] Brus, J. Heating of samples induced by fast magic-angle spinning[J]. Solid State Nucl Magn Reson, 2000, 16(3): 151-160.
[12] Thurber K R, Tycko R. Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder[J]. J Magn Reson, 2009, 196(1): 84-87.
[13] Dillmann B, Elbayed K, Zeiger H, et al. A novel low-E field coil to minimize heating of biological samples in solid-state multinuclear NMR experiments[J]. J Magn Reson, 2007, 187(1): 10-18.
[14] Neue G, Dybowski C. Determining temperature in a magic-angle spinning probe using the temperature dependence of the isotropic chemical shift of lead nitrate[J]. Solid State Nucl Magn Reson, 1997, 7(4): 333-336.
[15] Grimmer A R, Kretschmer A, Cajipe V B. Influence of magic angle spinning on sample temperature[J]. Magn Reson Chem, 1997, 35(2): 86-90.
[16] Dvinskikh S V, Castro V, Sandström D. Heating caused by radiofrequency irradiation and sample rotation in 13C magic angle spinning NMR studies of lipid membranes[J]. Magn Reson Chem, 2004, 42(10): 875-881.
[17] Mildner T, Ernst H, Freude D. 207Pb NMR detection of spinning-induced temperature gradients in MAS rotors[J]. Solid State Nucl Magn Reson, 1995, 5(3): 269-271.
[18] Langer B, Schnell I, Spiess H W, et al. Temperature calibration under ultrafast MAS conditions[J]. J Magn Reson, 1999, 138(1): 182-186.
[19] Fowler D J, Harris M J, Thompson L K. Heat management strategies for solid-state NMR of functional proteins[J]. J Magn Reson, 2012, 222: 112-118.
[20] Haw J F, Campbell G C, Crosby R C. Experimental considerations in variable-temperature solid-state nuclear magnetic resonance with cross polarization and magic-angle spinning[J]. Anal Chem, 1986, 58(14): 3 172-3 177.
[21] Chattah A K, Cucchietti F M, Hologne M, et al. Radiofrequency-induced temperature increase as a function of cross polarization contact time in 8CB[J]. Magn Reson Chem, 2002, 40(12): 772-776.
[22] Fung B. The effect of radiofrequency heating in 13C NMR studies of liquid crystals[J]. J Magn Reson, 1990, 86(1): 160-163.
[23] Shellock F G. Radiofrequency energy-induced heating during MR procedures: A Review[J]. J Magn Reson Imaging, 2000, 12(1): 30-36.
[24] d’Espinose de Lacaillerie J B, Jarry B, Pascui, et al. “Cooking the sample”: Radiofrequency induced heating during solid-state NMR experiments[J]. Solid State Nucl Magn Reson, 2005, 28(2): 225-232.
[25] Zhou Z, Sayer B G, Stark R E, et al. High-resolution magic-angle spinning 1H nuclear magnetic resonance studies of lipid dispersions using spherical glass ampoules[J]. Chem Phys Lipids, 1997, 90(1-2): 45-53.
[26] Nicholls A W, Mortishire-Smith R J. Temperature calibration of a high-resolution magic-angle spinning NMR probe for analysis of tissue samples[J]. Magn Reson Chem, 2001, 39(12): 773-776.
[27] Marassi F M, Crowell K J. Hydration-optimized oriented phospholipid bilayer samples for solid-state NMR structural studies of membrane proteins[J]. J Magn Reson, 2003, 161(1): 64-69.
[28] van Wüllen L, Schwering G, Naumann E, et al. MAS NMR at very high temperatures[J]. Solid State Nucl Magn Reson, 2004, 26(2): 84-86.
[29] Limbach H H, Hennig J, Kendrick R, et al. Proton-transfer kinetics in solids: tautomerism in free base porphines by nitrogen-15 CPMAS NMR[J]. J Am Chem Soc, 1984, 106(14): 4 059-4 060.
[30] Haw J F, Crook R A, Crosby R C. Solid-solid phase transitions for temperature calibration in magic-angle spinning[J]. J Magn Reson, 1986, 66(3): 551-554.
[31] Bjorholm T, Jakobsen H J. 31P MAS NMR of P4S3. Crystalline-to-plastic phase transition induced by MAS in a double air-bearing stator[J]. J Magn Reson, 1989, 84(1): 204-211.
[32] Anderson-Altmann K L, Grant D M. A solid-state 15N NMR study of the phase transitions in ammonium nitrate[J]. J Phys Chem, 1993, 97(42): 11 096-11 102.
[33] Klymachyov A N, Dalal N S. Squaric acid as an internal standard for temperature measurements in 13C MAS NMR[J]. Solid State Nucl Magn Reson, 1996, 7(2): 127-134.
[34] Bielecki A, Burum D P. Temperature dependence of 207Pb MAS spectra of solid lead nitrate. An accurate, sensitive thermometer for variable-temperature MAS[J]. J Magn Reson, 1995, 116(2): 215-220.
[35] Ferguson D B, Haw J F. Transient methods for in situ NMR of reactions on solid catalysts using temperature jumps[J]. Anal Chem, 1995, 67(18): 3 342-3 348.
[36] Aliev A E, Harris K D. Simple technique for temperature calibration of a MAS probe for solid‐state NMR spectroscopy[J]. Magn Reson Chem, 1994, 32(6): 366-369.
[37] Aliev A E, Harris K D M, Apperley D C. High-resolution solid-state 13C and 29Si NMR investigations of the dynamic properties of tetrakis (trimethylsilyl) silane[J]. J Chem Soc, Chem Commun, 1993, (3): 251-253.
[38] Campbell G C, Crosby R C, Haw J F. 13C Chemical shifts which obey the Curie Law in CP/MAS NMR spectra. The first CP/MAS NMR chemical-shift thermometer[J]. J Magn Reson, 1986, 69(1): 191-195.
[39] Grey C P, Cheetham A K, Dobson C M. Temperature-dependent solid-state 119Sn MAS NMR of Nd2Sn2O7, Sm2Sn2O7, and Y1.8Sm0.2Sn2O7. Three sensitive chemical-shift thermometers[J]. J Magn Reson, 1993, 101(3): 299-306.
[40] Vanmoorsel G J M P, Vaneck E R H, Grey C P. Pr2Sn2O7 and Sm2Sn2O7 as high-temperature shift thermometers in variable-temperature 119Sn MAS NMR[J]. J Magn Reson, 1995, 113(2): 159-163.
[41] Pan H, Gerstein B C. NMR of 31P in (VO)2P2O7 as an internal temperature standard in high-temperature NMR[J]. J Magn Reson, 1991, 92(3): 618-619.
[42] Massiot D, Bessada C, Echegut P, et al. High temperature NMR study of lithium sodium sulfate[J]. Solid State Ionics, 1990, 37(2-3): 223-229.
[43] Aliev A E, Harris K D M. Simple technique for temperature calibration of a MAS probe for solid-state NMR spectroscopy[J]. Magn Reson Chem, 1994, 32(6): 366-369.
[44] Li C G, Mo Y M, Hu J, et al. Analysis of RF heating and sample stability in aligned static solid-state NMR spectroscopy[J]. J Magn Reson, 2006, 180(1): 51-57.
[45] Chen Y, Zhang Z, Tang X, et al. Conformation and topology of diacylglycerol kinase in E. coli membranes revealed by solid-state NMR spectroscopy[J]. Angew Chem Int Edit, 2014, 53(22): 5 624-5 628.
[46] McDermott A, Polenova T, Bockmann A, et al. Partial NMR assignments for uniformly (13C, 15N)-enriched BPTI in the solid state[J]. J Biomol NMR, 2000, 16(3): 209-219.
[47] Mehring M. High Resolution NMR in Solids[M]. Springer, 1976.
[48] Detken A, Hardy E H, Ernst M, et al. Simple and efficient decoupling in magic-angle spinning solid-state NMR: the XiX scheme[J]. Chem Phys Lett, 2002, 356(3-4): 298-304.
[49] Bennett A E, Rienstra C M, Auger M, et al. Heteronuclear decoupling in rotating solids[J]. J Chem Phys, 1995, 103(16): 6 951-6 958.
[50] Fung B M, Khitrin A K, Ermolaev K. An improved broadband decoupling sequence for liquidcrystals and solids[J]. J Magn Reson, 2000, 142(1): 97-101.
[51] Meier B H. Cross polarization under fast magic angle spinning: thermodynamical considerations[J]. Chem Phys Lett, 1992, 188(3-4): 201-207.
[52] Laage S, Marchetti A, Sein J, et al. Band-selective 1H-13C cross-polarization in fast magic angle spinning solid-state NMR spectroscopy[J]. J Am Chem Soc, 2008, 130(51): 17 216-17 217.
[53] Ernst M, Samoson A, Meier B H. Low-power decoupling in fast magic-angle spinning NMR[J]. Chem Phys Lett, 2001, 348(3-4): 293-302.
[54] Laage S, Sachleben J R, Steuernagel S, et al. Fast acquisition of multi-dimensional spectra in solid-state NMR enabled by ultra-fast MAS[J]. J Magn Reson, 2009, 196(2): 133-141.
[55] Nielsen A B, Straasø L A, Nieuwkoop A J, et al. Broadband heteronuclear solid-state NMR experiments by exponentially modulated dipolar recoupling without decoupling[J]. J Phys Chem Lett, 2010, 1(13): 1 952-1 956.
[56] Jaroniec C P, Filip C, Griffin R G. 3D TEDOR NMR experiments for the simultaneous measurement of multiple carbonnitrogen distances in uniformly 13C, 15N-labeled solids[J]. J Am Chem Soc, 2002, 124(36): 10 728-10 742.
[57] Lewandowski J R, De Paëpe G, Griffin R G. Proton assisted insensitive nuclei cross polarization[J]. J Am Chem Soc, 2007, 129(4): 728-729.
[58] Gor’kov P L, Chekmenev E Y, Li C, et al. Using Low-E resonators to reduce RF heating in biological samples for static solid-state NMR up to 900 MHz [J]. J Magn Reson, 2007, 185(1): 77-93.
[59] Gor’kov P L, Witter R, Chekmenev E Y, et al. Low-E probe for 19F-1H NMR of dilute biological solids[J]. J Magn Reson, 2007, 189(2): 182-189.
[60] Froncisz W, Hyde J S. The loop-gap resonator: a new microwave lumped circuit ESR sample structure[J]. J Magn Reson, 1982, 47(3): 515-521.
[61] Alecci M, Nicholson I, Lurie D J. A novel multiple-tuned radiofrequency loop–gap resonator for use in PEDRI[J]. J Magn Reson, 1996, 110(1): 82-86.
[62] Cory D G, Lewandowski J T, Maas W E. INMR Probe for CP2: USA, 5, 539, 315[P]. 1996.
[63] Tang M, Comellas G, Mueller L, et al. High resolution 13C-detected solid-state NMR spectroscopy of a deuterated protein[J]. J Biomol NMR, 2010, 48(2): 103-111.
[64] Nadaud P S, Helmus J J, Kall S L, et al. Paramagnetic ions enable tuning of nuclear relaxation rates and provide long-range structural restraints in solid-state NMR of proteins[J]. J Am Chem Soc, 2009, 131(23): 8 108-8 120.
[65] Lopez J J, Kaiser C, Asami S, et al. Higher sensitivity through selective 13C excitation in solid-state NMR spectroscopy[J]. J Am Chem Soc, 2009, 131(44): 15 970-15 971.
[66] Thurber K R, Yau W M, Tycko R. Low-temperature dynamic nuclear polarization at 9.4 T with a 30 mW microwave source[J]. J Magn Reson, 2010, 204(2): 303-313.
/
| 〈 |
|
〉 |