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¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse.
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

A pulse is a short burst of radio waves distributed over a range of frequencies that simultaneously excites all the nuclei in the sample. Upon passing a radio frequency pulse along the x-axis, the nuclei absorb energy corresponding to their Larmor frequencies and achieve resonance. This shifts the net magnetization vector from the z-axis toward the transverse plane. This angle of rotation of the magnetization vector, or the flip angle, is proportional to the duration and intensity of the pulse.
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...

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関連する実験動画

Updated: Jul 13, 2026

Nuclear Magnetic Resonance Spectroscopy for the Identification of Multiple Phosphorylations of Intrinsically Disordered Proteins
12:47

Nuclear Magnetic Resonance Spectroscopy for the Identification of Multiple Phosphorylations of Intrinsically Disordered Proteins

Published on: December 27, 2016

サブミリモラー濃度でのサブ秒2DNMRスペクトロスコーピーは,サブミリモラー濃度で使用されます.

Boaz Shapira1, Erel Morris, Karol A Muszkat

  • 1Department of Chemical Physics, Weizmann Institute of Science, 76100 Rehovot, Israel.

Journal of the American Chemical Society
|September 24, 2004
PubMed
まとめ

この研究は,2D NMR (核磁気共鳴) とレーザー駆動動的ダイナミック核極化 (DNP) を組み合わせて,高品質のスペクトルを得ています. これにより,低濃度でペプチドとタンパク質のより速く,より敏感なNMRスペクトロスコピーを可能にします.

科学分野:

  • 生物物理化学 生物物理化学
  • スペクトル顕微鏡検査です.
  • 構造生物学 構造生物学とは

背景:

  • 二次元核磁気共鳴 (2D NMR) は,分子構造の決定のための強力な技術です.
  • 伝統的な2D NMRは,かなりの取得時間と高濃度の分析物質を必要とします.
  • ダイナミック・ニュクレア・ポラライゼーション (DNP) は,核スピン磁化を増やすことにより,NMR信号の感受性を高めます.

研究 の 目的:

  • レーザー駆動化学的に誘発されたダイナミックな核極化 (CIDNP) と新しいシングルスキャンの2D NMRプロトコルの組み合わせを調査する.
  • この統合的アプローチを使用してペプチドとタンパク質の高品質の2D NMRスペクトルを取得する可能性を評価する.
  • NMRスペクトロスコピーの取得時間を大幅に短縮し,感度を改善する可能性を評価する.

主な方法:

  • 最近提案された単回スキャン2D NMR取得プロトコルの実装.
  • レーザー駆動化学誘導ダイナミック核偏振 (CIDNP) の応用により,核スピン磁化が強化される.
  • ペプチドとタンパク質のサンプルに対する2D NMR 1H 相関スペクトルの記録.

主要な成果:

  • 質の高い2D NMRデータセットの取得が,数秒以内に成功していることが実証されています.

さらに関連する動画

Measuring Interactions of Globular and Filamentous Proteins by Nuclear Magnetic Resonance Spectroscopy (NMR) and Microscale Thermophoresis (MST)
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Measuring Interactions of Globular and Filamentous Proteins by Nuclear Magnetic Resonance Spectroscopy (NMR) and Microscale Thermophoresis (MST)

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NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins
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NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins

Published on: November 1, 2024

関連する実験動画

Last Updated: Jul 13, 2026

Nuclear Magnetic Resonance Spectroscopy for the Identification of Multiple Phosphorylations of Intrinsically Disordered Proteins
12:47

Nuclear Magnetic Resonance Spectroscopy for the Identification of Multiple Phosphorylations of Intrinsically Disordered Proteins

Published on: December 27, 2016

Measuring Interactions of Globular and Filamentous Proteins by Nuclear Magnetic Resonance Spectroscopy (NMR) and Microscale Thermophoresis (MST)
10:28

Measuring Interactions of Globular and Filamentous Proteins by Nuclear Magnetic Resonance Spectroscopy (NMR) and Microscale Thermophoresis (MST)

Published on: November 2, 2018

NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins
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NMR 15N Relaxation Experiments for the Investigation of Picosecond to Nanoseconds Structural Dynamics of Proteins

Published on: November 1, 2024

  • NMRとCIDNPの組み合わせによる速度と感度の大幅な改善を達成しました.
  • 分析剤濃度が1mM未満で得られたスペクトルで,高感度を示しています.

    • 結論:

    • シングルスキャンの2D NMRとレーザー駆動のCIDNPの組み合わせは,迅速かつ敏感なバイオ分子スペクトロスコピーの強力なアプローチを提供します.
    • この技術は,生物学的に重要な低濃度でのペプチドおよびタンパク質の研究を可能にします.
    • 速度と感度が向上したことで,バイオ分子に関する構造的および動的研究に新たな道が開かれます.