Joseph K. Vasquez, Zhe Zhou, Brian Clark, Ad J. Kimenai, Benjamin R. Reiner, Nathan J. Rau, Dan Baugh III, Donald V. Eldred, Manjiri Paradkar, Chen Zheng, Jim DeFelippis, Janece M. Potter, Xiao Hua Qiu, Xiaohong Zong, Wenshiue Owen Young, Thomas Fitzgibbons, Aitor Moreno, Christoph Freudenberger, Maksim Mayzel
{"title":"用于定量分析的13C NMR谱中消除声学振铃基线曲率","authors":"Joseph K. Vasquez, Zhe Zhou, Brian Clark, Ad J. Kimenai, Benjamin R. Reiner, Nathan J. Rau, Dan Baugh III, Donald V. Eldred, Manjiri Paradkar, Chen Zheng, Jim DeFelippis, Janece M. Potter, Xiao Hua Qiu, Xiaohong Zong, Wenshiue Owen Young, Thomas Fitzgibbons, Aitor Moreno, Christoph Freudenberger, Maksim Mayzel","doi":"10.1002/mrc.5384","DOIUrl":null,"url":null,"abstract":"<p><sup>13</sup>C nuclear magnetic resonance (NMR) is traditionally considered an insensitive technique, requiring long acquisition times to measure dilute functionalities on large polymers. With the introduction of cryoprobes and better electronics, sensitivity has improved in a way that allows measurements to take less than 1/20th the time that they previously did. Unfortunately, a high Q-factor with cryoprobes creates baseline curvature related to acoustic ringing that affects quantitative NMR analyses. Manual baseline correction is commonly used to compensate for the baseline roll, but it is a time-intensive process. The outcome of manual baseline correction can vary depending on processing parameters, especially for complicated spectra. Additionally, it can be challenging to distinguish between broad peaks and baseline rolls. A new anti-ring pulse sequence (zgig_pisp) was previously reported to improve on the incumbent single pulse experiment (zgig). The original report presented limited comparison data with <sup>13</sup>C NMR, but a thorough validation is needed before broader implementation can be considered. In this work, we report the round-robin testing and comparison of zgig_pisp and zgig pulse sequences. During the testing phase, we found that zgig_pisp is practically equivalent to zgig to ±2% for the majority of integrals examined. Additionally, a short broadband inversion pulse (BIP) was demonstrated as an alternative to the originally reported adiabatic CHIRP shaped pulse. The zgig_pisp pulse sequence code for Bruker spectrometers is also simplified.</p>","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":null,"pages":null},"PeriodicalIF":1.9000,"publicationDate":"2023-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Removing acoustic ringing baseline curvature in 13C NMR spectra for quantitative analyses\",\"authors\":\"Joseph K. Vasquez, Zhe Zhou, Brian Clark, Ad J. Kimenai, Benjamin R. Reiner, Nathan J. Rau, Dan Baugh III, Donald V. Eldred, Manjiri Paradkar, Chen Zheng, Jim DeFelippis, Janece M. Potter, Xiao Hua Qiu, Xiaohong Zong, Wenshiue Owen Young, Thomas Fitzgibbons, Aitor Moreno, Christoph Freudenberger, Maksim Mayzel\",\"doi\":\"10.1002/mrc.5384\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><sup>13</sup>C nuclear magnetic resonance (NMR) is traditionally considered an insensitive technique, requiring long acquisition times to measure dilute functionalities on large polymers. With the introduction of cryoprobes and better electronics, sensitivity has improved in a way that allows measurements to take less than 1/20th the time that they previously did. Unfortunately, a high Q-factor with cryoprobes creates baseline curvature related to acoustic ringing that affects quantitative NMR analyses. Manual baseline correction is commonly used to compensate for the baseline roll, but it is a time-intensive process. The outcome of manual baseline correction can vary depending on processing parameters, especially for complicated spectra. Additionally, it can be challenging to distinguish between broad peaks and baseline rolls. A new anti-ring pulse sequence (zgig_pisp) was previously reported to improve on the incumbent single pulse experiment (zgig). The original report presented limited comparison data with <sup>13</sup>C NMR, but a thorough validation is needed before broader implementation can be considered. In this work, we report the round-robin testing and comparison of zgig_pisp and zgig pulse sequences. During the testing phase, we found that zgig_pisp is practically equivalent to zgig to ±2% for the majority of integrals examined. Additionally, a short broadband inversion pulse (BIP) was demonstrated as an alternative to the originally reported adiabatic CHIRP shaped pulse. 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Removing acoustic ringing baseline curvature in 13C NMR spectra for quantitative analyses
13C nuclear magnetic resonance (NMR) is traditionally considered an insensitive technique, requiring long acquisition times to measure dilute functionalities on large polymers. With the introduction of cryoprobes and better electronics, sensitivity has improved in a way that allows measurements to take less than 1/20th the time that they previously did. Unfortunately, a high Q-factor with cryoprobes creates baseline curvature related to acoustic ringing that affects quantitative NMR analyses. Manual baseline correction is commonly used to compensate for the baseline roll, but it is a time-intensive process. The outcome of manual baseline correction can vary depending on processing parameters, especially for complicated spectra. Additionally, it can be challenging to distinguish between broad peaks and baseline rolls. A new anti-ring pulse sequence (zgig_pisp) was previously reported to improve on the incumbent single pulse experiment (zgig). The original report presented limited comparison data with 13C NMR, but a thorough validation is needed before broader implementation can be considered. In this work, we report the round-robin testing and comparison of zgig_pisp and zgig pulse sequences. During the testing phase, we found that zgig_pisp is practically equivalent to zgig to ±2% for the majority of integrals examined. Additionally, a short broadband inversion pulse (BIP) was demonstrated as an alternative to the originally reported adiabatic CHIRP shaped pulse. The zgig_pisp pulse sequence code for Bruker spectrometers is also simplified.
期刊介绍:
MRC is devoted to the rapid publication of papers which are concerned with the development of magnetic resonance techniques, or in which the application of such techniques plays a pivotal part. Contributions from scientists working in all areas of NMR, ESR and NQR are invited, and papers describing applications in all branches of chemistry, structural biology and materials chemistry are published.
The journal is of particular interest not only to scientists working in academic research, but also those working in commercial organisations who need to keep up-to-date with the latest practical applications of magnetic resonance techniques.