Method: Igc Sea Technical Note 804
Method: Igc Sea Technical Note 804
Method: Igc Sea Technical Note 804
In this study the effect of the sample mass on the surface and free energy of different pharmaceutical
ingredients has been investigated.
Introduction Method
Paracetamol (Sigma Aldrich, UK with a purity of
Inverse Gas Chromatography (IGC) is typically minimum 99.0%) and microcrystalline cellulose
carried out at infinite dilution (low concentration Prosolv 50 (Penwest Co., USA) have been used as
of vapour). In this regime only few vapour probe model substances for an active pharmaceutical
molecules interact with the high energy sites on ingredient and an excipient, respectively.
the surface of the solid material under Different masses of each powder were packed
investigation. If the concentration (partial into a silanised standard column (SMS standard
pressure) of the vapour probe is increased (“finite columns, 2mm ID for Paracetamol and 4 mm ID
dilution”) less active sites on the surface are also for microcrystalline cellulose) using the SMS
involved in the interaction and energetic sample-packing device. All columns were
parameters measured usually decrease in prepared using the same frequency and duration
comparison to infinite dilution conditions. of tapping during packing.
Whether a pulse experiment is carried out at Five columns containing different sample masses
infinite or finite concentration depends on the (ranging between 80 mg and 480 mg) of
ratio between amount of sample (= mass) and paracetamol and six columns of microcrystalline
amount of probe vapour (= concentration cellulose (between 8 mg and 271 mg) were
/volume) due to its discontinuous nature. packed and analysed. All analyses were carried
Given the above, it becomes obvious that the out using the SMS-iGC SEA instrument and the
results of an IGC-SEA pulse experiment are SMS-iGC v1.3 analysis suite of macros. All
dependent on the concentration regime and columns were initially conditioned at 30oC for 2h
conditions must therefore be carefully controlled. and 0% relative humidity (RH) and experiments
were carried out at 30°C and 0% RH with
injections of 0.03 P/P0 elutant vapour
concentrations for all elutants. A flame ionisation
detector was used to record the chromatogram
and resulting retention times.
References
[1]Frank Thielmann, David Butler, Determination of the dispersive surface
energy of Paracetamol by iGC at infinite dilution, SMS Application Note
202 (2000).
[2]Simone B. Reutenauer Reproducibility of the Dispersive Component of
Surface Energy measured by Inverse Gas Chromatography. Part I: Low
Energetic Materials, SMS Technical Note 801 (2003).
[3]Simone B. Reutenauer Reproducibility of the Dispersive Component of
Surface Energy measured by Inverse Gas Chromatography. Part II: Highly
Energetic Materials, SMS Technical Note 802 (2003).
[4]Frank Thielmann, Ingo Florian, The Measurement of Isotherms by Pulse
IGC, SMS Application Note 208 (2002).
[5]Frank Thielmann, Daniel Burnett, Isotherm Types and Adsorption
Mechanisms of Solvents on Pharmaceutical Excipients, SMS Application
Note 26 (2004).
[6]
Surface Energetic Heterogeneity Profiles by iGC Surface Energy Analyzer,
SMS Application Note 224.