Cross polarization stability in multidimensional NMR spectroscopy of biological solids.
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| Title: | Cross polarization stability in multidimensional NMR spectroscopy of biological solids. |
|---|---|
| Authors: | Harding, Benjamin D.1,2 (AUTHOR), Barclay, Alexander M.1,3 (AUTHOR), Piehl, Dennis W.4 (AUTHOR), Hiett, Ashley1,2 (AUTHOR), Warmuth, Owen A.1,2 (AUTHOR), Han, Ruixian5 (AUTHOR), Henzler-Wildman, Katherine2,6 (AUTHOR), Rienstra, Chad M.1,2,3,4,5,6,7,8 (AUTHOR) crienstra@wisc.edu |
| Source: | Journal of Magnetic Resonance. Aug2024, Vol. 365, pN.PAG-N.PAG. 1p. |
| Subjects: | Magic angle spinning, Nuclear magnetic resonance, Magnetic flux density, Quaternary structure, Tertiary structure |
| Abstract: | [Display omitted] • Demonstration of temperature impact on cross polarization stability. • Use of thermopad attenuators to reduce the effect of temperature drift. • Influence of tangent ramp parameters on cross polarization efficiency and stability. • Application to microcrystalline, membrane, and fibrous proteins. Magic-angle spinning (MAS) solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful and versatile technique for probing structure and dynamics in large, insoluble biological systems at atomic resolution. With many recent advances in instrumentation and polarization methods, technology development in SSNMR remains an active area of research and presents opportunities to further improve data collection, processing, and analysis of samples with low sensitivity and complex tertiary and quaternary structures. SSNMR spectra are often collected as multidimensional data, requiring stable experimental conditions to minimize signal fluctuations (t 1 noise). In this work, we examine the factors adversely affecting signal stability as well as strategies used to mitigate them, considering laboratory environmental requirements, configuration of amplifiers, and pulse sequence parameter selection. We show that Thermopad® temperature variable attenuators (TVAs) can partially compensate for the changes in amplifier output power as a function of temperature and thereby ameliorate one significant source of instability for some spectrometers and pulse sequences. We also consider the selection of tangent ramped cross polarization (CP) waveform shapes, to balance the requirements of sensitivity and instrumental stability. These findings collectively enable improved stability and overall performance for CP-based multidimensional spectra of microcrystalline, membrane, and fibrous proteins performed at multiple magnetic field strengths. [ABSTRACT FROM AUTHOR] |
| Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) | |
| Database: | Engineering Source |
| FullText | Text: Availability: 0 |
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| Header | DbId: egs DbLabel: Engineering Source An: 178975983 AccessLevel: 6 PubType: Academic Journal PubTypeId: academicJournal PreciseRelevancyScore: 0 |
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| Items | – Name: Title Label: Title Group: Ti Data: Cross polarization stability in multidimensional NMR spectroscopy of biological solids. – Name: Author Label: Authors Group: Au Data: <searchLink fieldCode="AR" term="%22Harding%2C+Benjamin+D%2E%22">Harding, Benjamin D.</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Barclay%2C+Alexander+M%2E%22">Barclay, Alexander M.</searchLink><relatesTo>1,3</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Piehl%2C+Dennis+W%2E%22">Piehl, Dennis W.</searchLink><relatesTo>4</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Hiett%2C+Ashley%22">Hiett, Ashley</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Warmuth%2C+Owen+A%2E%22">Warmuth, Owen A.</searchLink><relatesTo>1,2</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Han%2C+Ruixian%22">Han, Ruixian</searchLink><relatesTo>5</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Henzler-Wildman%2C+Katherine%22">Henzler-Wildman, Katherine</searchLink><relatesTo>2,6</relatesTo> (AUTHOR)<br /><searchLink fieldCode="AR" term="%22Rienstra%2C+Chad+M%2E%22">Rienstra, Chad M.</searchLink><relatesTo>1,2,3,4,5,6,7,8</relatesTo> (AUTHOR)<i> crienstra@wisc.edu</i> – Name: TitleSource Label: Source Group: Src Data: <searchLink fieldCode="JN" term="%22Journal+of+Magnetic+Resonance%22">Journal of Magnetic Resonance</searchLink>. Aug2024, Vol. 365, pN.PAG-N.PAG. 1p. – Name: Subject Label: Subjects Group: Su Data: <searchLink fieldCode="DE" term="%22Magic+angle+spinning%22">Magic angle spinning</searchLink><br /><searchLink fieldCode="DE" term="%22Nuclear+magnetic+resonance%22">Nuclear magnetic resonance</searchLink><br /><searchLink fieldCode="DE" term="%22Magnetic+flux+density%22">Magnetic flux density</searchLink><br /><searchLink fieldCode="DE" term="%22Quaternary+structure%22">Quaternary structure</searchLink><br /><searchLink fieldCode="DE" term="%22Tertiary+structure%22">Tertiary structure</searchLink> – Name: Abstract Label: Abstract Group: Ab Data: [Display omitted] • Demonstration of temperature impact on cross polarization stability. • Use of thermopad attenuators to reduce the effect of temperature drift. • Influence of tangent ramp parameters on cross polarization efficiency and stability. • Application to microcrystalline, membrane, and fibrous proteins. Magic-angle spinning (MAS) solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful and versatile technique for probing structure and dynamics in large, insoluble biological systems at atomic resolution. With many recent advances in instrumentation and polarization methods, technology development in SSNMR remains an active area of research and presents opportunities to further improve data collection, processing, and analysis of samples with low sensitivity and complex tertiary and quaternary structures. SSNMR spectra are often collected as multidimensional data, requiring stable experimental conditions to minimize signal fluctuations (t 1 noise). In this work, we examine the factors adversely affecting signal stability as well as strategies used to mitigate them, considering laboratory environmental requirements, configuration of amplifiers, and pulse sequence parameter selection. We show that Thermopad® temperature variable attenuators (TVAs) can partially compensate for the changes in amplifier output power as a function of temperature and thereby ameliorate one significant source of instability for some spectrometers and pulse sequences. We also consider the selection of tangent ramped cross polarization (CP) waveform shapes, to balance the requirements of sensitivity and instrumental stability. These findings collectively enable improved stability and overall performance for CP-based multidimensional spectra of microcrystalline, membrane, and fibrous proteins performed at multiple magnetic field strengths. [ABSTRACT FROM AUTHOR] – Name: AbstractSuppliedCopyright Label: Group: Ab Data: <i>Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.) |
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| RecordInfo | BibRecord: BibEntity: Identifiers: – Type: doi Value: 10.1016/j.jmr.2024.107724 Languages: – Code: eng Text: English PhysicalDescription: Pagination: PageCount: 1 StartPage: N.PAG Subjects: – SubjectFull: Magic angle spinning Type: general – SubjectFull: Nuclear magnetic resonance Type: general – SubjectFull: Magnetic flux density Type: general – SubjectFull: Quaternary structure Type: general – SubjectFull: Tertiary structure Type: general Titles: – TitleFull: Cross polarization stability in multidimensional NMR spectroscopy of biological solids. Type: main BibRelationships: HasContributorRelationships: – PersonEntity: Name: NameFull: Harding, Benjamin D. – PersonEntity: Name: NameFull: Barclay, Alexander M. – PersonEntity: Name: NameFull: Piehl, Dennis W. – PersonEntity: Name: NameFull: Hiett, Ashley – PersonEntity: Name: NameFull: Warmuth, Owen A. – PersonEntity: Name: NameFull: Han, Ruixian – PersonEntity: Name: NameFull: Henzler-Wildman, Katherine – PersonEntity: Name: NameFull: Rienstra, Chad M. IsPartOfRelationships: – BibEntity: Dates: – D: 01 M: 08 Text: Aug2024 Type: published Y: 2024 Identifiers: – Type: issn-print Value: 10907807 Numbering: – Type: volume Value: 365 Titles: – TitleFull: Journal of Magnetic Resonance Type: main |
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