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Stability Group - Solid Form Characterization Eric Munson

National Institute for Pharmaceutical Technology and Education (NIPTE). Stability Group - Solid Form Characterization Eric Munson. Outline. Samples of Gabapentin Analyzed Gabapentin - multiple forms Gabapentin monohydrate/desolvate Interconversion of forms upon analysis

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Stability Group - Solid Form Characterization Eric Munson

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  1. National Institute for Pharmaceutical Technology and Education (NIPTE) Stability Group - Solid Form Characterization Eric Munson

  2. Outline • Samples of Gabapentin Analyzed • Gabapentin - multiple forms • Gabapentin monohydrate/desolvate • Interconversion of forms upon analysis • Identification - Form III in milled samples • Gabapentin Lactam (primary degradation product)

  3. Gabapentin as Received - SSNMR

  4. Gabapentin as Received - SSNMR O 8 9 2 1 7 3 OH NH2 6 5 4 1H T1 = 134 s Tentative NMR Assignments 3 7 (6,8) 2 (5,9) Not shown: Carbon 1 at 179.5 ppm 4

  5. SSNMR of Gabapentin Forms

  6. SSNMR of Gabapentin Forms - Effects of Recrystallization

  7. Lot D Intensity (arbitrary units) Lot C Lot B Lot A Two-Theta (deg) SSNMR of Gabapentin Forms - Effects of Recrystallization

  8. Lot D Intensity (arbitrary units) Lot C Lot B Lot A Two-Theta (deg) SSNMR of Gabapentin Forms - Effects of Recrystallization

  9. SSNMR of Gabapentin Forms - Effects of Recrystallization Lot A, 20x Lot B, 20x Lot C, 10x Lot D, 20x

  10. SSNMR of Gabapentin Forms

  11. SSNMR of Gabapentin Forms - Monohydrate

  12. SSNMR of Gabapentin Forms - Milled Samples

  13. SSNMR of Gabapentin Forms - Milled Samples

  14. SSNMR of Gabapentin Forms - Milled Samples

  15. Effect of Grinding on Forms • Particles of bulk lactose monohydrate before processing • Lactose monohydrate cryoground for 60 minutes Crystalline Amorphous Crystalline

  16. Lactose 1H T1 Relaxation Data - SSNMR Lubach, J. W.; Xu, D.; Segmuller, B. E., Munson, E. J. In Press J. Pharm. Sci. 2006.

  17. Lactose 1H T1 Relaxation Data - SSNMR Lubach, J. W.; Xu, D.; Segmuller, B. E., Munson, E. J. In Press J. Pharm. Sci. 2006.

  18. Gabapentin Relaxation Times Stability - High, Medium, Low

  19. Degradation of Gabapentin Forms - Milled Samples

  20. Gabapentin Relaxation Times

  21. Degradation of Gabapentin Forms - Milled Samples

  22. Summary

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