Abstract
The aim of this work was to assess the effect of different crystalline polymorphism on surface energetics of D-mannitol using finite dilution inverse gas chromatography (FD-IGC). Pure α, β and δ polymorphs were prepared via solution crystallisation and characterised by powder X-ray diffraction (P-XRD). The dispersive surface energies were found to range from 43 to 34 mJ/m2, 50 to 41 mJ/m2, and 48 to 38 mJ/m2 , for α, β, and δ, respectively, for surface coverage ranging from 0.006 to 0.095. A deconvolution modelling approach was employed to establish their energy sites. The primary sites corresponded to maxima in the dispersive surface energy of 37.1 and 33.5; 43.3 and 39.5; and 38.6, 38.4 and 33.0; for α, β, and δ, respectively. This methodology was also extended to an α-β polymorph mixture to estimate the amount of the constituent α and β components present in the sample. The dispersive surface energies of the α-β mixture were found to be in the range of 48 to 37 mJ/m2 with 40.0, 42.4, 38.4 and 33.1 mJ/m2 sites. The deconvolution modelling method extracted the energy contribution of each of the polymorphs from data for the polymorphic mixture. The mixture was found to have a β-polymorph surface content of ∼19%. This work shows the influence of polymorphism on surface energetics and demonstrates that FD-IGC coupled with a simple modelling approach to be a powerful tool for assessing the specific nature of this energetic distribution including the quantification of polymorphic content on the surface.
Similar content being viewed by others
References
Aguiar AJ, Krc J, Kinkel AW, Samyn JC. J Pharm Sci. 1967;56(7):847–53.
Borka L, Haleblian JK. Acta Pharm Jugosl. 1990;40:71–94.
Burger A, Ramberger R. Microchim Acta. 1979;72(3–4):259–71.
Navrotsky A. Geochem Trans. 2003;4(6):34.
Li Q, Rudolph V, Weigl B, Earl A. Int J Pharm. 2004;280(1–2):77–93.
Shah UV, Olusanmi D, Narang AS, Hussain MA, Tobyn MJ, Heng JYY. Int J Pharm. 2014;475(1–2):592–6.
Shah UV, Olusanmi D, Narang AS, Hussain MA, Tobyn MJ, Hinder SJ, et al. Pharm Res 2014: 1–12.
Das SC, Zhou Q, Morton DAV, Larson I, Stewart PJ. Eur J Pharm Sci. 2011;43(4):325–33.
Fichtner F, Mahlin D, Welch K, Gaisford S, Alderborn G. Pharm Res. 2008;25(12):2750–9.
Szekely J, Stanek V. Chem Eng Sci. 1969;24(1):11–24.
Heng JYY, Bismarck A, Lee AF, Wilson K, Williams DR. J Pharm Sci. 2007;96(8):2134–44.
Heng JYY, Bismarck A, Lee AF, Wilson K, Williams DR. Langmuir. 2006;22(6):2760–9.
Ho R, Hinder SJ, Watts JF, Dilworth SE, Williams DR, Heng JYY. Int J Pharm. 2010;387(1–2):79–86.
Shah UV, Olusanmi D, Narang AS, Hussain MA, Gamble JF, Tobyn MJ, et al. Int J Pharm. 2014;472(1–2):140–7.
Chemburkar SR, Bauer J, Deming K, Spiwek H, Patel K, Morris J, et al. Org Process Res Dev. 2000;4(5):413–7.
Cares-Pacheco MG, Vaca-Medina G, Calvet R, Espitalier F, Letourneau JJ, Rouilly A, et al. Int J Pharm. 2014;475(1–2):69–81.
Lee AY, Erdemir D, Myerson AS. Annu Rev Chem Biomol Eng. 2011;2(1):259–80.
Chattoraj S, Shi L, Sun CC. CrystEngComm. 2010;12(8):2466–72.
Yoshinari T, Forbes RT, York P, Kawashima Y. Int J Pharm. 2002;247(1–2):69–77.
Fowkes FM. Dispersion force contributions to surface and interfacial tensions, contact angles, and heats of immersion. Contact Angle, Wettability, and Adhesion. Advances in Chemistry. 43: American Chemical Society, 1964. p. 99–111.
Wu S. Macromol Sci C. 1974;10(1):1–73.
Schultz J, Lavielle L, Martin C. J Adhes. 1987;23(1):45–60.
Dorris GM, Gray DG. J Colloid Interface Sci. 1980;77(2):353–62.
Shi B, Wang Y, Jia L. J Chromatogr A. 2011;1218(6):860–2.
Buckton G, Gill H. Adv Drug Deliv Rev. 2007;59(14):1474–9.
Rudzinski W, Everett DH. Adsorption of gases on heterogeneous surfaces. London: Academic; 1992. p. 529–51.
Harris LB. Surf Sci. 1968;10(2):129–45.
Brunauer S, Emmett PH, Teller E. J Am Chem Soc. 1938;60(2):309–19.
Thielmann F, Burnett DJ, Heng JYY. Drug Dev Ind Pharm. 2007;33(11):1240–53.
Jefferson AE, Williams DR, Heng JYY. J J Adhes Sci Technol. 2011;25(4–5):339–55.
Smith RR, Williams DR, Burnett DJ, Heng JYY. Langmuir. 2014;30(27):8029–35.
Aubrey-Medendorp C. Atomic force microscopy method development for surface energy analysis [Doctoral Thesis]. Lexington, KY, United States: University of Kentucky; 2011.
Poornachary SK, Parambil JV, Chow PS, Tan RBH, Heng JYY. Cryst Growth Des. 2013;13(3):1180–6.
Gamble JF, Leane M, Olusanmi D, Tobyn M, Šupuk E, Khoo J, et al. Int J Pharm. 2012;422(1–2):238–44.
Ylä-Mäihäniemi PP, Heng JYY, Thielmann F, Williams DR. Langmuir. 2008;24(17):9551–7.
Stephenson GA, Forbes RA, Reutzel-Edens SM. Adv Drug Deliv Rev. 2001;48(1):67–90.
Shah B, Kakumanu VK, Bansal AK. J Pharm Sci. 2006;95(8):1641–65.
Acknowledgments
The PhD studentship, supported by the Engineering and Physical Science Research Council and Surface Measurement Systems for Robert Smith, is gratefully acknowledged.
Author information
Authors and Affiliations
Corresponding author
Additional information
Responsible editors: Otilia M. Koo, Panayiotis P. Constantinides, Lavinia M. Lewis, and Joseph Reo
Rights and permissions
About this article
Cite this article
Smith, R.R., Shah, U.V., Parambil, J.V. et al. The Effect of Polymorphism on Surface Energetics of D-Mannitol Polymorphs. AAPS J 19, 103–109 (2017). https://doi.org/10.1208/s12248-016-9978-y
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1208/s12248-016-9978-y