Sensitivity enhancement by sequential data acquisition for 13C-direct detection NMR

نویسندگان

چکیده

13C-direct detection NMR has several advantages compared to proton detection, including a tendency relax slower and wider chemical shift range. However, the sensitivity of is much lower than that because its gyromagnetic ratio. In addition, virtual decoupling procedure often performed remove peak splitting in axis, which further reduces 1/√2. this study, enhance experiments, we developed HCACO-type new pulse sequence anti-phase (AP) in-phase (IP) signals are acquired sequentially single scan. The experiment was tested on an amino acid (valine) two proteins (streptococcal protein G B1 domain (GB1) α-synuclein). AP IP spectra were successfully obtained all cases. Using these spectra, IPAP performed, removed. increased by 1.43, 1.26 times for valine, GB1 α-synuclein, respectively, conventional HCACO experiment. another sequence, where simultaneously FID. 1.40 1.35 valine GB1, respectively. These methods potentially applicable other experiments measure one-bond correlations will extend utility method, especially structural analyses intrinsically disordered proteins.

برای دانلود باید عضویت طلایی داشته باشید

برای دانلود متن کامل این مقاله و بیش از 32 میلیون مقاله دیگر ابتدا ثبت نام کنید

اگر عضو سایت هستید لطفا وارد حساب کاربری خود شوید

منابع مشابه

Optimization of 13C direct detection NMR methods.

(13)C-detected experiments are still limited by their inherently lower sensitivity, as compared to the equivalent (1)H-detected experiments. Improving the sensitivity of (13)C detection methods remains a significant area of NMR research that may provide better means for studying large macromolecular systems by NMR. In this communication, we show that (13)C-detected experiments are less sensitiv...

متن کامل

13C-direct detected NMR experiments for the sequential J-based resonance assignment of RNA oligonucleotides

We present here a set of (13)C-direct detected NMR experiments to facilitate the resonance assignment of RNA oligonucleotides. Three experiments have been developed: (1) the (H)CC-TOCSY-experiment utilizing a virtual decoupling scheme to assign the intraresidual ribose (13)C-spins, (2) the (H)CPC-experiment that correlates each phosphorus with the C4' nuclei of adjacent nucleotides via J(C,P) c...

متن کامل

Sensitivity enhancement in multiple-quantum NMR experiments with CPMG detection.

We present a modified multiple-quantum (MQ) experiment, which implements the Carr-Purcell-Meiboom-Gill (CPMG) detection scheme in the static MQ NMR experiment proposed by W. S. Warren et al. (1980, J. Chem. Phys.73, 2084-2099) and exploited further by O. N. Antzutkin and R. Tycko (1999, J. Chem. Phys.110, 2749-2752). It is demonstrated that a significant enhancement in the sensitivity can be ac...

متن کامل

Detection of human muscle glycogen by natural abundance 13C NMR.

Natural abundance 13C nuclear magnetic resonance spectroscopy was used to detect signals from glycogen in the human gastrocnemius muscle. The reproducibility of the measurement was demonstrated, and the ability to detect dynamic changes was confirmed by measuring a decrease in muscle glycogen levels after exercise and its subsequent repletion. Single frequency gated 1H decoupling was used to ob...

متن کامل

Supramolecular interactions probed by 13C-13C solid-state NMR spectroscopy.

We present a robust solid-state NMR approach for the accurate determination of molecular interfaces in insoluble and noncrystalline protein-protein complexes. The method relies on the measurement of intermolecular (13)C-(13)C distances in mixtures of [1-(13)C]glucose- and [2-(13)C]glucose-labeled proteins. We have applied this method to Parkinson's disease-associated α-synuclein fibrils and fou...

متن کامل

ذخیره در منابع من


  با ذخیره ی این منبع در منابع من، دسترسی به آن را برای استفاده های بعدی آسان تر کنید

ژورنال

عنوان ژورنال: Journal of Magnetic Resonance

سال: 2021

ISSN: ['1096-0856', '1090-7807']

DOI: https://doi.org/10.1016/j.jmr.2020.106878