Process for freeze drying cyclophosphamide

Drug – bio-affecting and body treating compositions – Designated organic active ingredient containing – Carbohydrate doai

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514 23, 514 54, 514960, 536124, 536127, 536 182, 536 553, 536117, 536 171, A61K 3170, C07H 100

Patent

active

046596992

ABSTRACT:
A two-stage process for freeze-drying an aqueous solution of a dosage amount of cyclophosphamide to yield a hydrate of cyclophosphamide (referred to as "CPA" for brevity), comprises, in a first stage, freeze-drying a solution of CPA in combination with an excipient until the moisture content of the freeze-dried material is less than 2% by wt, based on the amount of anhydrous CPA present; and, in a second stage, rehydrating the freeze-dried material until the moisture content of the product is in the critical range of from about 2% to 7% by wt, based on the net wt of CPA product, it being essential for stability of the product that at least one sugar excipient be present. The process requires that a major amount by weight of the excipient(s) or all of it, be mannitol, optionally with an additional sugar and/or a carboxylic acid, and/or a buffer salt; and, the mannitol is present in an amount at least one-half (0.5 times) as mush as the CPA (anhyd) present. To produce a dosage form of a `plug` or `cake` which is free of flakes and granules, or bubbles on its surface, and/or voids within the product (or "plug"), any of which are individually no greater than 2 mm in equivalent diameter ("equiv. dia."), requires a unique combination of carefully controlled process steps. The preferred CPA product obtained by the process provides a dosage amount of stable freeze-dried and rehydrated CPA as a hydrate which includes at least an equivalent amount by weight, and up to 5 times as much, of mannitol. The dosage amount may include sodium chloride to adjust tonicity, and a buffer salt to maintain pH.

REFERENCES:
patent: 3018302 (1962-01-01), Arnold et al.
patent: 3356652 (1967-12-01), Ray-Chaudhuri
patent: 4157440 (1979-06-01), Reiner et al.
patent: 4404368 (1983-09-01), Alvardo-Urbina et al.
patent: 4537883 (1985-08-01), Alexander et al.

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