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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
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The quadrupole mass analyzer consists of four cylindrical metal rods arranged in a diamond carrying a DC voltage and a radio-frequency AC voltage. The motion of ions through the quadrupole depends on the field strength, causing only ions of a certain m/z to resonate successfully and strike the detector at a given field strength. Though the transmission rate for these analyzers is high, the exact elemental composition of the sample is not determined because of low resolution; however, they are...
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¹H NMR: Interpreting Distorted and Overlapping Signals01:02

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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.
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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

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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...
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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

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Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other...
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¹³C NMR: ¹H–¹³C Decoupling01:04

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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.
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Nuclear Magnetic Resonance Spectroscopy for the Identification of Multiple Phosphorylations of Intrinsically Disordered Proteins
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Batch-specific discrimination using nuclear quadrupole resonance spectroscopy.

Georgia Kyriakidou1, Andreas Jakobsson2, Kaspar Althoefer1

  • 1†Department of Informatics, King's College London, Strand, London WC2R 2LS, United Kingdom.

Analytical Chemistry
|February 27, 2015
PubMed
Summary
This summary is machine-generated.

Nitrogen-14 nuclear quadrupole resonance spectroscopy ((14)N NQR) successfully identified differences between paracetamol (acetaminophen) tablet batches. This technique shows promise for detecting counterfeit medicines by analyzing material integrity.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Pharmaceutical Analysis

Background:

  • Paracetamol (acetaminophen) is a widely used analgesic.
  • Ensuring the quality and authenticity of pharmaceutical products is crucial.
  • Variations in manufacturing or storage can affect drug integrity.

Purpose of the Study:

  • To investigate the use of nitrogen-14 nuclear quadrupole resonance spectroscopy ((14)N NQR) for differentiating paracetamol tablet batches.
  • To assess the sensitivity of (14)N NQR to variations in crystal structure and material integrity.

Main Methods:

  • Utilized (14)N NQR spectroscopy to analyze paracetamol tablet batches.
  • Applied multivariate analysis of variance (MANOVA) to assess within-batch variability.
  • Performed statistical analysis to compare different batches based on batch number and expiry date.

Main Results:

  • No significant variability was found within batches of paracetamol tablets.
  • Significant differences were detected between different batches of paracetamol tablets.
  • (14)N NQR signals indicated variations influenced by manufacturing, storage, or aging.

Conclusions:

  • The (14)N NQR technique is highly sensitive to subtle changes in paracetamol tablet batches.
  • NQR spectroscopy can serve as a valuable tool for quality control and authentication of pharmaceuticals.
  • This method holds potential for detecting counterfeit medicines.