The use of inverse phase gas chromatography to study the glass transition temperature of a powder surface.
OBJECTIVE
To measure the glass transition temperature (Tg) at the surface of a hydrophobic particle at different temperatures and humidities, on the hypothesis that the surface may be plasticized to a different extent to the bulk due to slow water sorption giving a concentration gradient of water through the particles.


METHODS
Amorphous indomethacin was exposed to a range of relative humidities (RH) and temperatures in an inverse gas chromatograph (IGC). The retention volumes of decane were calculated at all conditions using center of mass (Vcom) and peak height (Vmax) methods. The extent of water sorption was determined gravimetrically.


RESULTS
The Vcom retention volumes were found to deviate from Vmax results at certain critical humidities at each temperature. This was taken as a novel method for determining the Tg of the sample surface at different experimental conditions. Extrapolating the critical RH to lower the Tg to experimental temperature to 0% RH yeilded a Tg similar to literature values. Water sorption data provided valuable information on changes in mobility of the amorphous form as a function of temperature and RH.


CONCLUSIONS
It is possible to use IGC to determine the Tg of the surface of particles at defined conditions. This overcomes the problems of conventional methods of assessing Tg, relating to disruption of water sorption on heating. This helps in the understanding of the physical form of the surface of hydrophobic particles and how and when the surface will start to crystallize.
Buckton
Graham
G
Department of Pharmaceutics, School of Pharmacy, University of London, London WC1N 1AX, UK. Graham.buckton@ulsop.ac.uk
Ambarkhane
Ameet
A
Pincott
Kim
K
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000737:chemistry; D002849:Chromatography, Gas / Q000379:methods; D006813:Humidity; D057927:Hydrophobic and Hydrophilic Interactions; D007213:Indomethacin / Q000737:chemistry; D011208:Powders / Q000737:chemistry*; D013696:Temperature; D013816:Thermodynamics; D014867:Water / Q000737:chemistry
D000894:Anti-Inflammatory Agents, Non-Steroidal; D011208:Powders; D014867:Water; D007213:Indomethacin