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Related Concept Videos

Raman Spectroscopy: Overview01:20

Raman Spectroscopy: Overview

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The underlying principle of Raman spectroscopy is based on the interaction between light and matter, specifically molecules' inelastic scattering of photons. When a monochromatic beam of light, typically from a laser source, interacts with a sample, most scattered light has the same frequency as the incident light. This is known as Rayleigh scattering.
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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
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Freeze-drying-induced mutarotation of lactose detected by Raman spectroscopy.

Julia Monola1, Elle Koivunotko1, Jacopo Zini2

  • 1Drug Research Program, Division of Pharmaceutical Biosciences, Faculty of Pharmacy, University of Helsinki, 00790 Helsinki, Finland.

European Journal of Pharmaceutics and Biopharmaceutics : Official Journal of Arbeitsgemeinschaft Fur Pharmazeutische Verfahrenstechnik E.V
|October 20, 2024
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Summary

Freeze-drying protects sensitive biomaterials, but excipients are needed. Combining nanofibrillated cellulose with lactose and glycine successfully preserved material properties after freeze-drying and reconstitution.

Keywords:
BiomaterialsFreeze-dryingMolecular dynamics simulationsMutarotationNanofibrillated cellulose hydrogelRaman spectroscopy

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Area of Science:

  • Materials Science
  • Biotechnology
  • Pharmaceutical Sciences

Background:

  • Freeze-drying (lyophilization) is crucial for storing heat-sensitive biomaterials.
  • Physicochemical stresses during freeze-drying can compromise material integrity and function.
  • The protective mechanisms of excipients in freeze-drying are not fully understood.

Purpose of the Study:

  • To screen sugars and amino acids as excipients for plant-based nanofibrillated cellulose (NFC) hydrogels.
  • To develop a protective matrix system for freeze-drying pharmaceuticals and biologics.
  • To evaluate the efficacy of NFC-based formulations using computational and spectroscopic methods.

Main Methods:

  • Molecular dynamics simulations to screen excipient-NFC interactions.
  • Freeze-drying and reconstitution of NFC hydrogel formulations.
  • Non-invasive Timegate PicoRaman spectroscopy for molecular analysis.
  • Traditional characterization methods for physicochemical and rheological properties.

Main Results:

  • In silico screening identified lactose and glycine as having high attraction to NFC.
  • NFC hydrogel formulations with lactose and glycine enabled successful freeze-drying and reconstitution.
  • Preserved physicochemical and rheological properties were observed post-reconstitution.
  • Raman spectroscopy revealed molecular-level changes, including lactose mutarotation.

Conclusions:

  • Integrating in silico screening with non-invasive spectroscopy is effective for designing freeze-drying formulations.
  • NFC-based hydrogels with specific excipients offer a promising protective matrix system.
  • Understanding molecular interactions and orientational changes of excipients is vital for freeze-drying applications.