Skip to main content
Log in

Quantification of Surface Amorphous Content Using Dispersive Surface Energy: the Concept of Effective Amorphous Surface Area

  • Research Article
  • Published:
AAPS PharmSciTech Aims and scope Submit manuscript

Abstract

We investigate the use of dispersive surface energy in quantifying surface amorphous content, and the concept of effective amorphous surface area is introduced. An equation is introduced employing the linear combination of surface area normalized square root dispersive surface energy terms. This equation is effective in generating calibration curves when crystalline and amorphous references are used. Inverse gas chromatography is used to generate dispersive surface energy values. Two systems are investigated, and in both cases surface energy data collected for physical mixture samples comprised of amorphous and crystalline references fits the predicted response with good accuracy. Surface amorphous content of processed lactose samples is quantified using the calibration curve, and interpreted within the context of effective amorphous surface area. Data for bulk amorphous content is also utilized to generate a thorough picture of how disorder is distributed throughout the particle. An approach to quantifying surface amorphous content using dispersive surface energy is presented. Quantification is achieved by equating results to an effective amorphous surface area based on reference crystalline, and amorphous materials.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

REFERENCES

  1. Buckton G, Dove J, Davies P. Isothermal microcalorimetry and inverse phase gas chromatography to study small changes in powder surface properties. Int J Pharm. 1999;193:13–9.

    Article  PubMed  CAS  Google Scholar 

  2. Buckton G, Ambarkhane A, Pincott K. The use of inverse gas chromatography to study the glass transition temperature of a powder surface. Pharm Res. 2004;9:1554–7.

    Article  Google Scholar 

  3. Adamska K, Voelkel A. Inverse gas chromatographic determination of solubility parameters of excipients. Int J Pharm. 2005;304:11–7.

    Article  PubMed  CAS  Google Scholar 

  4. Adamska K, Voelkel A, Heberger H. Selection of solubility parameters for characterization of pharmaceutical excipients. J Chromatogr A. 2007;1171:90–7.

    Article  PubMed  CAS  Google Scholar 

  5. Newell H, Buckton G, Butler D, Thielmann F, Williams D. The use of inverse phase gas chromatography to study the change in surface energy of amorphous lactose as a function of relative humidity and the process of collapse and crystallization. Int J Pharm. 2001;217:45–56.

    Article  PubMed  CAS  Google Scholar 

  6. Planinsek O, Buckton G. Invergas chromatography: considerations about appropriate use for amorphous and crystalline powders. J Pharm Sci. 2003;92:1286–94.

    Article  PubMed  CAS  Google Scholar 

  7. Newell H, Buckton G. Inverse gas chromatography: investigating whether the techniques preferentially probes high energuy sites for mixtures crystalline and amorphous lactose. Pharm Res. 2004;8:1440–4.

    Article  Google Scholar 

  8. Adamson A, Gast AP. Physical chemistry of surfaces. 6th ed. New York: Wiley; 1997.

    Google Scholar 

  9. Sun C, Berg J. The effective surface energy of heterogeneous solids measured by inverse gas chromatography at infinite dilution. J Colloid Interface Sci. 2003;260:443–8.

    Article  PubMed  CAS  Google Scholar 

  10. van Oss C, Good R. Surface tension and solubility of polymers and biopolymers: the role of polar and apolar interfacial free energies. Journal of Macromolecular. Science. Chemistry. 1989;26:1183–203.

    Google Scholar 

  11. Schultz J, Lavielle L. Inverse gas chromatograophy: characterization of polymers and other materials. In: Lloyd D, Ward T, Schreiber H, editors. ACS Symposium Series 391. Washington DC: American Chemical Soceity; 1989.

    Google Scholar 

  12. Hogan S, Buckton G. The quantification of small degrees of disorder in lactose using solution calorimetry. Int J Pharm. 2000;207:57–64.

    Article  PubMed  CAS  Google Scholar 

  13. Ho R, Wilson D, Heng J. Crystal habits and the variation in surface energy heterogeneity. Cryst Growth and Des. 2009;9:4907–11.

    Article  CAS  Google Scholar 

Download references

ACKNOWLEDGMENTS

The authors would like to thank Dr. Rachel Forcino, and Ms. Maria Barnett for supplying the samples of Drug Substance A, and amorphous lactose respectively. We also thank the reviewers for constructive comments.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Jeffrey Brum.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Brum, J., Burnett, D. Quantification of Surface Amorphous Content Using Dispersive Surface Energy: the Concept of Effective Amorphous Surface Area. AAPS PharmSciTech 12, 887–892 (2011). https://doi.org/10.1208/s12249-011-9655-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1208/s12249-011-9655-5

KEY WORDS

Navigation