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The preparation of pituitary tissue for bioassay commonly involves fractionation and lyophilization to reduce the bulk of material. It is of practical importance to know if losses of hormonal activity are associated with such procedures.

To examine this point, pituitary glands were collected from four aged crossbred ewes and frozen within 1 hr. of slaughter. The pooled anterior lobes, average weight 0·940 g., were homogenized in 20 ml. 0·15 M-NH₄HCO₃ buffer, pH 7·2, containing 1% n-butanol and the homogenate was divided into four aliquots. One aliquot was frozen directly and a second was treated with acetone for 36 hr. at 2° by the method of Parlow, Anderson & Melampy (1964), the resulting powder being weighed and stored 48 hr. in a desiccator. The remaining homogenate samples were stirred for approximately 8 hr. and then centrifuged. The supernatants were made up to 5 ml. with buffer