J. C. May1 , N. M. Etz1 , H. Wang1 , L. Rey2 , 1CBER, FDA, Rockville, MD, 2Conseiller Scientifique, Lausanne, Switzerland
Residual moisture specifications which are set by the US Food and Drug Administration must be met to ensure potency and stability of freeze-dried biological product throughout the product's licensed shelf life. Thermogravimetry, thermogravimetry/mass spectrometry, and Karl Fischer methodology and vapor pressure moisture measurements are used to provide moisture information for freeze-dried biological products. Residual moisture measurements are compared for a Pertussis Vaccine and other freeze-dried biological products. Residual moisture data for the freeze-dried cake and vapor pressure moisture determinations in the space above the freeze-dried cake in the final container are discussed in regard to stability. Residual moisture stability data are presented and results for biological products in glass vials with elastomeric container closures are studied and compared to freeze-dried products in flame-sealed glass ampoules. Near-infrared spectroscopy measurements in the OH combination bands region (near 1920 nm) for Pertussis Vaccine incubated at 22, 37 and 50o C indicate moisture migration within the flame-sealed glass ampoule.