Removing acoustic ringing baseline curvature in 13C NMR spectra for quantitative analyses

IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
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
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引用次数: 0

Abstract

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.

用于定量分析的13C NMR谱中消除声学振铃基线曲率
13C核磁共振(NMR)传统上被认为是一种不灵敏的技术,需要很长的采集时间来测量大聚合物上的稀释官能团。随着冷冻探针和更好的电子设备的引入,灵敏度得到了提高,使测量所需的时间比以前减少了1/20。不幸的是,冷冻探针的高Q因子会产生与声学振铃相关的基线曲率,从而影响定量NMR分析。手动基线校正通常用于补偿基线滚动,但这是一个耗时的过程。手动基线校正的结果可能因处理参数而异,尤其是对于复杂的光谱。此外,区分宽峰值和基线滚动可能具有挑战性。先前报道了一种新的反环脉冲序列(zgig_isp),以改进现有的单脉冲实验(zgig)。最初的报告提供了有限的与13C NMR的比较数据,但在考虑更广泛的实施之前,需要进行彻底的验证。在这项工作中,我们报告了zgig_isp和zgig脉冲序列的循环测试和比较。在测试阶段,我们发现对于所检查的大多数积分,zgig_disp实际上相当于zgig到±2%。此外,短宽带反转脉冲(BIP)被证明是最初报道的绝热CHIRP形状脉冲的替代方案。对Bruker光谱仪的zgig_ isp脉冲序列编码也进行了简化。
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来源期刊
CiteScore
4.70
自引率
10.00%
发文量
99
审稿时长
1 months
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.
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