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. Author manuscript; available in PMC: 2014 Oct 1.
Published in final edited form as: Eur J Pharm Biopharm. 2013 Apr 20;85(2):189–196. doi: 10.1016/j.ejpb.2013.04.003

Table 2.

Freeze drying parameters used for the series of formulations in this study.

Formulation Fill volume (vial size) Target product temperature Chamber pressure Freezing temperature (ramp rate) Primary drying Secondary drying

Shelf temperature (ramp rate) Drying Time Shelf temperature (ramp rate) Drying time
HES + disaccharide (i.e. Formulation A) 1 mL (5 cc) –40 °C 70 mTorr –45 °C (1 °C/min) –20 °C (1.3 °C/min) ~12 h +33 °C (0.3 °C/min) 2 h
Samples with sorbitol in formulation B, C and D 2 mL (5 cc) –31 °C 100 mTorr –40 °C (1 °C/min) –18 °C (0.2 °C/min) ~43 h +40 °C (0.1 °C/min) 6 h
Samples with glycerol in formulation B, C and D 2 mL (5 cc) –40 °C 60 mTorr –45 °C (1 °C/min) –34 °C (0.2 °C/min) ~88 h +40 °C (0.1 °C/min) 5 h
HES 0.75% + trehalose:glycerol (i.e. Formulation E) 5 mL (20 cc) –40 °C 70 mTorr –45 °C (1 °C/min) –34 °C (0.2 °C/min) ~72 h +40 °C (0.1 °C/min) 6 h