A LOW-E MAGIC ANGLE SPINNING PROBE FOR BIOLOGICAL SOLID STATE NMR AT 750 MHz
Identifieur interne : 000338 ( Pmc/Corpus ); précédent : 000337; suivant : 000339A LOW-E MAGIC ANGLE SPINNING PROBE FOR BIOLOGICAL SOLID STATE NMR AT 750 MHz
Auteurs : Seth A. Mcneill ; Peter L. Gor Ov ; Kiran Shetty ; William W. Brey ; Joanna R. LongSource :
- Journal of magnetic resonance (San Diego, Calif. : 1997) [ 1090-7807 ] ; 2008.
Abstract
Crossed-coil NMR probes are a useful tool for reducing sample heating for biological solid state NMR. In a crossed-coil probe, the higher frequency 1H field, which is the primary source of sample heating in conventional probes, is produced by a separate low-inductance resonator. Because a smaller driving voltage is required, the electric field across the sample and the resultant heating is reduced. In this work we describe the development of a magic angle spinning (MAS) solid state NMR probe utilizing a dual resonator. This dual resonator approach, referred to as “Low-E,” was originally developed to reduce heating in samples of mechanically aligned membranes. The study of inherently dilute systems, such as proteins in lipid bilayers, via MAS techniques requires large sample volumes at high field to obtain spectra with adequate signal-to-noise ratio under physiologically relevant conditions. With the Low-E approach, we are able to obtain homogeneous and sufficiently strong radiofrequency fields for both 1H and 13C frequencies in a 4 mm probe with a 1H frequency of 750 MHz. The performance of the probe using windowless dipolar recoupling sequences is demonstrated on model compounds as well as membrane embedded peptides.
Url:
DOI: 10.1016/j.jmr.2008.12.008
PubMed: 19138870
PubMed Central: 2659328
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PMC:2659328Le document en format XML
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<author><name sortKey="Gor Ov, Peter L" sort="Gor Ov, Peter L" uniqKey="Gor Ov P" first="Peter L." last="Gor Ov">Peter L. Gor Ov</name>
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<author><name sortKey="Shetty, Kiran" sort="Shetty, Kiran" uniqKey="Shetty K" first="Kiran" last="Shetty">Kiran Shetty</name>
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<author><name sortKey="Brey, William W" sort="Brey, William W" uniqKey="Brey W" first="William W." last="Brey">William W. Brey</name>
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<author><name sortKey="Long, Joanna R" sort="Long, Joanna R" uniqKey="Long J" first="Joanna R." last="Long">Joanna R. Long</name>
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<front><div type="abstract" xml:lang="en"><p id="P1">Crossed-coil NMR probes are a useful tool for reducing sample heating for biological solid state NMR. In a crossed-coil probe, the higher frequency <sup>1</sup>
H field, which is the primary source of sample heating in conventional probes, is produced by a separate low-inductance resonator. Because a smaller driving voltage is required, the electric field across the sample and the resultant heating is reduced. In this work we describe the development of a magic angle spinning (MAS) solid state NMR probe utilizing a dual resonator. This dual resonator approach, referred to as “Low-E,” was originally developed to reduce heating in samples of mechanically aligned membranes. The study of inherently dilute systems, such as proteins in lipid bilayers, via MAS techniques requires large sample volumes at high field to obtain spectra with adequate signal-to-noise ratio under physiologically relevant conditions. With the Low-E approach, we are able to obtain homogeneous and sufficiently strong radiofrequency fields for both <sup>1</sup>
H and <sup>13</sup>
C frequencies in a 4 mm probe with a <sup>1</sup>
H frequency of 750 MHz. The performance of the probe using windowless dipolar recoupling sequences is demonstrated on model compounds as well as membrane embedded peptides.</p>
</div>
</front>
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<pmc article-type="research-article"><pmc-comment>The publisher of this article does not allow downloading of the full text in XML form.</pmc-comment>
<pmc-dir>properties manuscript</pmc-dir>
<front><journal-meta><journal-id journal-id-type="nlm-journal-id">9707935</journal-id>
<journal-id journal-id-type="pubmed-jr-id">20597</journal-id>
<journal-id journal-id-type="nlm-ta">J Magn Reson</journal-id>
<journal-id journal-id-type="iso-abbrev">J. Magn. Reson.</journal-id>
<journal-title-group><journal-title>Journal of magnetic resonance (San Diego, Calif. : 1997)</journal-title>
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<issn pub-type="ppub">1090-7807</issn>
<issn pub-type="epub">1096-0856</issn>
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<article-id pub-id-type="pmc">2659328</article-id>
<article-id pub-id-type="doi">10.1016/j.jmr.2008.12.008</article-id>
<article-id pub-id-type="manuscript">NIHMS84540</article-id>
<article-categories><subj-group subj-group-type="heading"><subject>Article</subject>
</subj-group>
</article-categories>
<title-group><article-title>A LOW-E MAGIC ANGLE SPINNING PROBE FOR BIOLOGICAL SOLID STATE NMR AT 750 MHz</article-title>
</title-group>
<contrib-group><contrib contrib-type="author"><name><surname>McNeill</surname>
<given-names>Seth A.</given-names>
</name>
<xref ref-type="aff" rid="A2">#</xref>
</contrib>
<contrib contrib-type="author"><name><surname>Gor’kov</surname>
<given-names>Peter L.</given-names>
</name>
<xref ref-type="aff" rid="A3">+</xref>
</contrib>
<contrib contrib-type="author"><name><surname>Shetty</surname>
<given-names>Kiran</given-names>
</name>
<xref ref-type="aff" rid="A3">+</xref>
</contrib>
<contrib contrib-type="author"><name><surname>Brey</surname>
<given-names>William W.</given-names>
</name>
<xref ref-type="aff" rid="A3">+</xref>
</contrib>
<contrib contrib-type="author"><name><surname>Long</surname>
<given-names>Joanna R.</given-names>
</name>
<xref ref-type="aff" rid="A1">@</xref>
<xref rid="FN1" ref-type="author-notes">*</xref>
</contrib>
</contrib-group>
<aff id="A1"><label>@</label>
Department of Biochemistry and Molecular Biology and McKnight Brain Institute, University of Florida, Gainesville, Florida 32610</aff>
<aff id="A2"><label>#</label>
Department of Electrical and Computer Engineering, University of Florida, 32611</aff>
<aff id="A3"><label>+</label>
National High Magnetic Field Laboratory, Tallahassee, FL 32310</aff>
<author-notes><corresp id="FN1">Correspondence: email: <email>jrlong@mbi.ufl.edu</email>
telephone :(352)846-1506 fax :(352)392-3422</corresp>
</author-notes>
<pub-date pub-type="nihms-submitted"><day>12</day>
<month>1</month>
<year>2009</year>
</pub-date>
<pub-date pub-type="epub"><day>14</day>
<month>12</month>
<year>2008</year>
</pub-date>
<pub-date pub-type="ppub"><month>4</month>
<year>2009</year>
</pub-date>
<pub-date pub-type="pmc-release"><day>01</day>
<month>4</month>
<year>2010</year>
</pub-date>
<volume>197</volume>
<issue>2</issue>
<fpage>135</fpage>
<lpage>144</lpage>
<abstract><p id="P1">Crossed-coil NMR probes are a useful tool for reducing sample heating for biological solid state NMR. In a crossed-coil probe, the higher frequency <sup>1</sup>
H field, which is the primary source of sample heating in conventional probes, is produced by a separate low-inductance resonator. Because a smaller driving voltage is required, the electric field across the sample and the resultant heating is reduced. In this work we describe the development of a magic angle spinning (MAS) solid state NMR probe utilizing a dual resonator. This dual resonator approach, referred to as “Low-E,” was originally developed to reduce heating in samples of mechanically aligned membranes. The study of inherently dilute systems, such as proteins in lipid bilayers, via MAS techniques requires large sample volumes at high field to obtain spectra with adequate signal-to-noise ratio under physiologically relevant conditions. With the Low-E approach, we are able to obtain homogeneous and sufficiently strong radiofrequency fields for both <sup>1</sup>
H and <sup>13</sup>
C frequencies in a 4 mm probe with a <sup>1</sup>
H frequency of 750 MHz. The performance of the probe using windowless dipolar recoupling sequences is demonstrated on model compounds as well as membrane embedded peptides.</p>
</abstract>
<kwd-group><kwd>solid state NMR</kwd>
<kwd>magic angle spinning</kwd>
<kwd>membrane proteins</kwd>
<kwd>probe design</kwd>
<kwd>loop gap resonator</kwd>
<kwd>low-E</kwd>
<kwd>rf heating</kwd>
</kwd-group>
<funding-group><award-group><funding-source country="United States">National Heart, Lung, and Blood Institute : NHLBI</funding-source>
<award-id>R01 HL076586-04 || HL</award-id>
</award-group>
<award-group><funding-source country="United States">National Heart, Lung, and Blood Institute : NHLBI</funding-source>
<award-id>R01 HL076586-03 || HL</award-id>
</award-group>
<award-group><funding-source country="United States">National Heart, Lung, and Blood Institute : NHLBI</funding-source>
<award-id>R01 HL076586-01A1 || HL</award-id>
</award-group>
</funding-group>
</article-meta>
</front>
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