Spontaneous gelation of a novel histamine H4 receptor antagonist in aqueous solution

Pharm Res. 2011 Oct;28(10):2556-66. doi: 10.1007/s11095-011-0483-9. Epub 2011 Jun 3.

Abstract

Purpose: Low molecular weight hydrogelators typically require a stimulus such as heat, antisolvent, or pH adjustment to produce a gel. This study examines gelation of a novel histamine H4 receptor antagonist that forms hydrogels spontaneously at room temperature.

Methods: To elucidate the mechanism and structural moieties responsible for this unusual gelation, hydrogels were characterized by rheology, optical microscopy, and XRD. SEM was performed on xerogels; NMR measurements were conducted in gelator solutions in the presence of a gel-breaker. The influence of temperature, concentration, pH, and ionic strength on elastic and viscous moduli of the hydrogels was evaluated; gel points were established via thorough rheological criteria.

Results: The observed are "true" gels with a fibrillar texture and lamellar microstructure. On a molecular level, the gels are composed of aggregates of partially ionized species stabilized by hydrophobic interactions of aromatic moieties. The gel-to-sol transition occurs at physiologically relevant temperatures and is concentration-, pH-, and ionic strength-dependent.

Conclusions: We hypothesize that this spontaneous gelation is due to the so-called "spring" effect, a high energy salt form that transiently increases aqueous solubility above its equilibrium limit. Upon equilibration, this supersaturated system undergoes aggregation that avoids crystallization and produces a hydrogel.

MeSH terms

  • Attention
  • Histamine Antagonists / chemistry*
  • Hydrogels / chemistry*
  • Hydrogen-Ion Concentration
  • Hydrophobic and Hydrophilic Interactions
  • Osmolar Concentration
  • Phase Transition
  • Receptors, G-Protein-Coupled / antagonists & inhibitors*
  • Receptors, Histamine
  • Receptors, Histamine H4
  • Rheology / methods
  • Salts / chemistry
  • Solutions / chemistry
  • Temperature
  • Water / chemistry*

Substances

  • HRH4 protein, human
  • Histamine Antagonists
  • Hydrogels
  • Receptors, G-Protein-Coupled
  • Receptors, Histamine
  • Receptors, Histamine H4
  • Salts
  • Solutions
  • Water