Method for stabilizing compound DX-52-1 and lyophilized composit

Drug – bio-affecting and body treating compositions – Designated organic active ingredient containing – Heterocyclic carbon compounds containing a hetero ring...

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A61K 31495, A61K 3150

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active

059771097

DESCRIPTION:

BRIEF SUMMARY
TECHNICAL FIELD

The present invention relates to a method for stabilizing DX-52-1 and derivatives thereof.


BACKGROUND ART

DX-52-1 according to Formula (I-1) shown below and derivatives thereof are known to have antitumor activity as described in U.S. Pat. No. 4,650,869. ##STR2##
However, DX-52-1 and derivatives thereof (hereinafter, collectively referred to as "DX-52-1 derivatives") decompose easily in an aqueous solution. For example, while DX-52-1 is relatively stable in an aqueous solution under an alkaline condition of pH 7 or above, long-term preservability and stability of DX-52-1 is not sufficient. It is therefore necessary to develop a long-term preservable and stable preparation of DX-52-1.


DISCLOSURE OF THE INVENTION

It is an object of the present invention to overcome these shortcomings of the prior art.
In accordance with an aspect of the present invention, there is provided a method for stabilizing DX-52-1 derivatives represented by Formula (I): ##STR3## wherein R is hydrogen or lower alkyl, comprising the steps of preparing a solution containing the DX-52-1 derivative and at least one saccharide, and lyophilizing said solution, said solution having a pH of 7 to 12.
The present invention further relates to a desiccated composition comprising a DX-52-1 derivative according to Formula (I) and at least one saccharide.
The present invention relates to a process for attaining long-term stable compositions of DX-52-1 derivatives according to Formula (I). Preferably, lower alkyl is a straight-chain or branched alkyl group having 1 to 6 carbon atoms. Most preferably, lower alkyl is methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, tert-butyl, pentyl, or hexyl.
The DX-52-1 derivatives represented by Formula (I) can be prepared as disclosed in U.S. Pat. No. 4,650,869. The '869 Patent shows freeze-dried preparations of DX-52-1 which do not contain a saccharide in Example 1 hereinafter.
Suitable DX-52-1 derivatives for use in the present invention are exemplified in Table 1 below.


TABLE 1 ______________________________________ Compound .sup.13 C-NMR .delta. (ppm) ______________________________________ 1 183.7, 156.4, 138.1, 129.0, 122.4, 121.4, 119.4, 110.1, 70.8, 65.5, 65.2, 58.7, 58.4, 58.3, 56.3, 45.1, 41.8, 33.0, 30.0 (D.sub.2 O) - 2 175.91, 155.83, 136.19, 127.81, 122.05, 120.44, 117.82, 108.59, 70.45, 65.79, 64.70, 58.03, 57.84, 57.60, 55.32, 52.24, 42.77, 41.91, 32.96, 28.91 (CDCl.sub.3) ______________________________________
The present invention is illustrated in detail below.
The DX-52-1 derivative represented by Formula (I) and one or more saccharide are dissolved in a solvent. Preferably, the mixture solution is adjusted to a pH between 7 and 12, typically with an aqueous solution of hydrochloric acid and an aqueous solution of sodium hydroxide. The resulting solution is filtered under a sterile condition through a membrane filter, followed by lyophilization.
Representative examples of the saccharides are lactose, sucrose, raffinose, dextran, mannitol, inositol, galactose, ribose, xylose, mannose, cellobiose, maltose, maltotriose, maltotetraose, and trehalose. Preferably, lactose is used. The saccharide is used in a concentration of 0.005 to 1,000 mg/ml, preferably 1 to 500 mg/ml.
The solvent in which the DX-52-1 derivative and one or more saccharide are dissolved is not particularly limited. Preferable solvents maintain the pH in the range of 7 to 12 as such or permit addition of an aqueous solution of hydrochloric acid and an aqueous solution of sodium hydroxide. In addition to water, preferable examples of the solvents include buffer solutions, such as a citric acid/disodium hydrogenphosphate buffer, a phosphate buffer, a borate buffer, an acetate buffer, and a citrate buffer. These buffer solutions may desirably be used at a concentration of 0.001 to 0.5 M.
If desired, the preparation according to the present invention may also contain pharmaceutically acceptable additives, such as antioxidants, antiseptics, buffering agents, anesthetics, solubilizers, so

REFERENCES:
patent: 4650869 (1987-03-01), Hirata et al.

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