Drug solubilization mechanism of α-glucosyl stevia by NMR spectroscopy

Int J Pharm. 2014 Apr 25;465(1-2):255-61. doi: 10.1016/j.ijpharm.2014.01.035. Epub 2014 Feb 4.

Abstract

We investigated the drug solubilization mechanism of α-glucosyl stevia (Stevia-G) which was synthesized from stevia (rebaudioside-A) by transglycosylation. (1)H and (13)C NMR peaks of Stevia-G in water were assigned by two-dimensional (2D) NMR experiments including (1)H-(1)H correlation, (1)H-(13)C heteronuclear multiple bond correlation, and (1)H-(13)C heteronuclear multiple quantum coherence spectroscopies. The (1)H and (13)C peaks clearly showed the incorporation of two glucose units into rebaudioside-A to produce Stevia-G, supported by steviol glycoside and glucosyl residue assays. The concentration-dependent chemical shifts of Stevia-G protons correlated well with a mass-action law model, indicating the self-association of Stevia-G molecules in water. The critical micelle concentration (CMC) was 12.0 mg/mL at 37°C. The aggregation number was 2 below the CMC and 12 above the CMC. Dynamic light scattering and 2D (1)H-(1)H nuclear Overhauser effect spectroscopy (NOESY) NMR experiments demonstrated that Stevia-G self-associated into micelles of a few nanometers in size with a core-shell structure, containing a kaurane diterpenoid-based hydrophobic core and a glucose-based shell. 2D (1)H-(1)H NOESY NMR measurements also revealed that a poorly water-soluble drug, naringenin, was incorporated into the hydrophobic core of the Stevia-G micelle. The Stevia-G self-assembly behavior and micellar drug inclusion capacity can achieve significant enhancement in drug solubility.

Keywords: Aggregation number; Drug solubility improvement; Micelle; Nuclear Overhauser effect spectroscopy; Nuclear magnetic resonance; α-Glucosyl stevia.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbon-13 Magnetic Resonance Spectroscopy*
  • Diterpenes, Kaurane / chemical synthesis
  • Diterpenes, Kaurane / chemistry*
  • Excipients / chemistry*
  • Flavanones / chemistry*
  • Glucosides / chemical synthesis
  • Glucosides / chemistry*
  • Micelles
  • Nanoparticles
  • Particle Size
  • Proton Magnetic Resonance Spectroscopy*
  • Solubility
  • Technology, Pharmaceutical / methods*
  • Water / chemistry*

Substances

  • Diterpenes, Kaurane
  • Excipients
  • Flavanones
  • Glucosides
  • Micelles
  • Water
  • naringenin