( n is a mixture of Carbamezipine stable ...)Practical Applications of HyperDSC in a Pharmaceutical Laboratory

n is a mixture of Carbamezipine stable form I and metastable form III. Figure 6 shows an experiment carried out at 500 C/min in which a very weak endotherm was detected for the melting of Carbamazepine form III, a polymorph making up only 1% of the sample content.

Analysis of a weak glass transition (Tg)

The detection of a glass transition in an amorphous material is also improved by HyperDSC (Figure 7). With HyperDSC detection limits < 1% (w/w) can be reached in order to quantify the amorphous material in pharmaceutical compounds [1].

At such heating rates, thermal gradients within the sample can have an impact, widening the signals detected and superimposing thermal phenomena inside the material. One way to limit this thermal gradient is to perform analyses on samples of very small mass, less than a milligram [2].

Application of HyperDSC to several Sanofi-Aventis samples

Polymorphism

This active ingredient comprises a mixture of physical forms (phases α + ).

A DSC measurement under standard conditions at 10 C/min causes form α to transform into form , which prevents the two crystalline forms from being quantified by comparing melting enthalpies.

In this case, HyperDSC inhibits phase transformation, and the melting endotherms of the two forms can thus be used to quantify the mixture. Figure 8 shows an experiment at 100 C/min, carried out on a reconstituted mixture of form α / form at 95 / 5%.

Transition separation by HyperDSC

Glass transition and evaporation

This amorphous active ingredient has a high water content (about 10%) whose evaporation conceals glass transition during a DSC analysis under conventional conditions (5 C/min). An experiment at
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