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Related Concept Videos

Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

833
In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
833
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

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The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
1.7K
Other Nuclides: 31P, 19F, 15N NMR01:16

Other Nuclides: 31P, 19F, 15N NMR

475
Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a...
475
NMR Spectroscopy of Aromatic Compounds01:14

NMR Spectroscopy of Aromatic Compounds

5.1K
Aromatic compounds can be identified or analyzed using proton NMR and carbon‐13 NMR. Typically, aromatic hydrogens or hydrogens directly bonded to the aromatic rings are strongly deshielded by the aromatic ring current. Therefore, they absorb in the range of 6.5–8.0 ppm in proton NMR spectra. For instance, aromatic hydrogens directly bonded to the benzene ring absorb at 7.3 ppm. However, aromatic hydrogens of larger rings absorb farther upfield or downfield than the ideal range.
5.1K
NMR Spectroscopy Of Amines01:19

NMR Spectroscopy Of Amines

9.4K
In proton NMR spectroscopy, primary amines and secondary amines showcase their N–H protons as a broad signal in the chemical shift range between δ 0.5 and 5 ppm. The exact position in this range depends on several factors, including sample concentration, hydrogen bonding, and the type of solvent used. Since amine protons undergo fast proton exchange in solution, the protons are labile and therefore do not participate in any splitting with adjacent protons. Thus, the observed peak is...
9.4K
NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

1.3K
NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
1.3K

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Related Experiment Video

Updated: Sep 20, 2025

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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19F Solid-state NMR characterization of pharmaceutical solids.

Yong Du1, Yongchao Su2

  • 1Analytical Research and Development, Merck & Co., Inc., Rahway, NJ, 07065, United States.

Solid State Nuclear Magnetic Resonance
|June 10, 2022
PubMed
Summary

Fluorine-19 solid-state NMR enhances drug analysis sensitivity. This review covers advanced 19F magic angle spinning NMR methods for drug research, development, and quality control.

Keywords:
(19)F NMRAmorphous solid dispersionDrug productsDrug substancesPharmaceuticalsPolymorphismQuantificationSolid-state analysis

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A Package of Established Analytical Tools to Investigate the Solid-State Alteration of Lipid-Based Excipients
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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products

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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products

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Area of Science:

  • Analytical Chemistry
  • Pharmaceutical Sciences
  • Spectroscopy

Background:

  • Solid-state NMR is a powerful tool for characterizing pharmaceutical materials.
  • Low sensitivity is a major challenge in analyzing low-concentration or complex drug systems.
  • Fluorinated drugs offer a unique opportunity for enhanced NMR analysis.

Purpose of the Study:

  • To review recent advancements in fluorine-19 (19F) magic angle spinning NMR methods for drug research and development.
  • To highlight the utility of 19F NMR in overcoming sensitivity limitations in pharmaceutical analysis.
  • To discuss applications of 19F NMR in various stages of drug development.

Main Methods:

  • Review of recent literature on 19F magic angle spinning NMR techniques.
  • Focus on methods applicable to drug substances and products.
  • Discussion of sensitivity enhancement strategies using fluorine as a probe.

Main Results:

  • 19F NMR provides high sensitivity for analyzing fluorinated pharmaceuticals.
  • Advanced 19F MAS NMR enables polymorph screening at micromolar levels.
  • Applications include structural elucidation and investigation of molecular interactions in drug delivery and stability.

Conclusions:

  • 19F MAS NMR is a valuable and sensitive technique for modern drug research and development.
  • It offers significant advantages for quality control and understanding drug behavior.
  • Fluorine-19 NMR is crucial for characterizing complex pharmaceutical systems.