Evaluation of Pharmaceutical Small Molecule Crystallization Processes Using eXalt™ Technology

Evaporative crystallization studies can be carried out efficiently using eXalt technology and provide researchers with a high degree of control. eXalt can crystallize various small molecule actives from different solvents simultaneously under the same conditions and rate.

Instrumentation and Experimental Procedure

eXalt includes a sample holder for securely placing 4ml vials (Figure 1). A ‘tower’ with baffles is built into the holder to control the individual evaporation rate. After placing the assembled holders into a Genevac HT evaporator, the preferred evaporation time is selected.

L to R: eXalt baffles and tower assembly, loading vials and towers to holders, completed holder assembly

Figure 1. L to R: eXalt baffles and tower assembly, loading vials and towers to holders, completed holder assembly. Image credit: SP Scientific

Initial Studies

Recrystallization of Carbamazepine, Caffeine, and Ibuprofen were carried out from various solvents for 24 and above 66 hours, to

explore the possibility of formation of different polymorphs. The results for Carbamazepine are illustrated in Figure 2.

Carbamazepine Polymorphism XRPD (L) and DSC (R) Analysis

Figure 2. Carbamazepine Polymorphism XRPD (L) and DSC (R) Analysis. Image credit: SP Scientific

Conclusion

Eight compounds were crystallized using eXalt. Small 5mg sample volumes per vial were adequate, only 50mg was needed for the full screening process. eXalt produced crystals suitable for SCXR, DSC, and XPRD analyses. Seed crystals were also produced for further process development. The non-destructive nature allows for full recovery of all amorphous test material and poor quality crystals.

eXalt technology is accessible to all researchers involved in late stage research projects. Amorphous compounds previously uncrystallized were successfully crystallized.

Acknowledgements

Produced from materials authored by Rob Darrington from Genevac Ltd, Ipswich, UK.

This information has been sourced, reviewed and adapted from materials provided by Genevac.

For more information on this source, please visit Genevac.

 

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