IP Library Granted Patent US 8,748,449
Granted Patent B2
US 8,748,449 · App. 13/544,945 · Granted Jun 10, 2014

Use of polyols to obtain stable polymorphous forms of rifaximin

View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 8,748,449
App. No.
13/544,945
Granted
Jun 10, 2014
Kind
B2
Abstract

Polyols stabilize polymorphous form of rifaximin, in particular the β form. When polyols having at least two hydroxy groups are added to rifaximin powder, polymorph β is stable and remains stable in time independently from the environment humidity. In this invention a method to prepare formulations constituted by pure and stable polymorphous forms able to give a pharmaceutical product is described.

Claims (79)

1. A method of preparing rifaximin in polymorphous form β comprising:

i) contacting rifaximin in solid state with an aqueous solution of one or more polyols to obtain a mixture of rifaximin and polyols wherein the aqueous solution comprises one or more polyols at a concentration of 5% to 50% (w/w), and

ii) drying the mixture of rifaximin in solid state and polyols.

2. The method of claim 1 , wherein the one or more polyols are selected from the group of polyols comprising two to seven carbon atoms and two to seven hydroxy groups.

3. The method of claim 1 , wherein the one or more polyols are selected from the group consisting of monosaccharides, disaccharides, polysaccharides, xanthan gum, di-hydroxy acids and poly-hydroxy acids.

4. The method of claim 1 , wherein the one or more polyols are compounds of formula I:

H—[O—CH—(X)—CH 2 ] n —OH  (I)

wherein X is hydrogen or lower alkyl, and n is between 1 and 20.

5. The method of claim 1 , wherein the one or more polyols are compounds having the general formula H—[O—CH 2 —CH 2 ] n —OH, wherein n is between 2 and 14.

6. The method of claim 1 , wherein the polyol is 1,2,3-propanetriol or 1,2-propanediol.

7. The method of claim 1 , wherein the polyol is 1,2,3-propanetriol.

8. The method of claim 1 , wherein the polyol is 1,2-propanediol.

9. The method of claim 1 , wherein the contacting of said rifaximin in solid state with an aqueous solution of one or more polyols is at a temperature of between 20° C. and 90° C.

10. The method of claim 1 , wherein the contacting is for a period of time of between 1 and 24 hours.

11. The method of claim 1 , wherein the drying is at a temperature of between 40° C. and 80° C.

12. The method of claim 1 , wherein the drying is at ambient pressure or under vacuum.

13. The method of claim 1 , wherein the drying is for a period of time of between 2 and 72 hours.

14. The method of claim 1 , wherein the contacting step comprises spraying the polyol aqueous solution at concentrations of from 5 to 50% (w/w) on the rifaximin β in solid state in a fluid bed apparatus having an inlet temperature of between 20° C. and 90° C., and wherein the drying step comprises drying the mixture under an air flow at a temperature of between 30° C. and 90° C.

15. The method of claim 3 , wherein the polysaccharide is selected from the group consisting of starch, cellulose or derivatives thereof, dextrin and maltodextrin.

16. The method of claim 3 , wherein the one or more polyols are selected from the group consisting of fructose, dextrose and sucrose.

17. The method of claim 1 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of:

5.3°, 7.7° and 10.4°; or

5.3°, 7.7° and 17.7°; or

5.3°, 7.7° and 18.2°; or

5.3°, 10.4° and 17.7°; or

5.3°, 10.4° and 18.2°; or

7.7°, 10.4° and 17.7°; or

7.7°, 10.4° and 18.2°; or

8.9°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3° and 17.7°; or

5.3°, 7.7°, 12.3° and 18.2°; or

7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 6.7°, 7.7°, 8.9°, 10.4°, 17.7°, 18.2 and 20.7.

18. The method of claim 1 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of 5.3, 7.7 and 18.2.

19. The method of claim 1 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of 5.3, 6.7, 7.7, 8.9, 10.4, 12.3, 17.7, 18.2, 18.6 and 20.7.

20. A stabilized polymorphous rifaximin β in solid state obtained by the method of claim 1 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of:

5.3°, 7.7° and 10.4°; or

5.3°, 7.7° and 17.7°; or

5.3°, 7.7° and 18.2°; or

5.3°, 10.4° and 17.7°; or

5.3°, 10.4° and 18.2°; or

7.7°, 10.4° and 17.7°; or

7.7°, 10.4° and 18.2°; or

8.9°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3° and 17.7°; or

5.3°, 7.7°, 12.3° and 18.2°; or

7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 6.7°, 7.7°, 8.9°, 10.4°, 17.7°, 18.2 and 20.7.

21. A stabilized polymorphous β form of rifaximin in solid state comprising one or more polyols wherein the polyol is selected from the group consisting of a compound having the general formula H—[O—CH 2 —CH 2 ] n —OH, wherein n is between 2 and 16.

22. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the one or more polyols are selected form the group consisting of 1,2,3-propanetriol, and 1,2-propanediol.

23. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the one or more polyols are selected from the group consisting of polyols comprising two to seven carbon atoms and two to seven hydroxy groups.

24. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the one or more polyols are selected from the group consisting of monosaccharides, disaccharides, polysaccharides, xanthan gum, di-hydroxy acids and poly-hydroxy acids.

25. The stabilized polymorphous β form of rifaximin of claim 24 , wherein the polyols are selected from the group consisting of fructose, dextrose, sucrose, starch, cellulose and derivatives thereof, maltodextrin and dextrin.

26. The stabilized polymorphous β form of rifaximin of claim 21 , wherein n is between 2 and 10.

27. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the polyol is 1,2,3-propanetriol.

28. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the polyol is 1,2-propanediol.

29. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of:

5.3°, 7.7° and 10.4°; or

5.3°, 7.7° and 17.7°; or

5.3°, 7.7° and 18.2°; or

5.3°, 10.4° and 17.7°; or

5.3°, 10.4° and 18.2°; or

7.7°, 10.4° and 17.7°; or

7.7°, 10.4° and 18.2°; or

8.9°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3° and 17.7°; or

5.3°, 7.7°, 12.3° and 18.2°; or

7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 7.7°, 12.3°, 17.7° and 18.2°; or

5.3°, 6.7°, 7.7°, 8.9°, 10.4°, 17.7°, 18.2 and 20.7.

30. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of 5.3, 7.7 and 18.2.

31. The stabilized polymorphous β form of rifaximin of claim 21 , wherein the polymorphous form β is characterized by peaks at the values of the diffraction angles 2θ of 5.3, 6.7, 7.7, 8.9, 10.4, 12.3, 17.7, 18.2, 18.6 and 20.7.

32. A pharmaceutical composition for the treatment of pathologies that need antibiotic therapy, said composition comprising the stabilized polymorphous β form of rifaximin of claim 24 and an excipient.

33. The pharmaceutical composition of claim 32 , wherein the rifaximin is in the form of gastroresistant microgranules.

34. The pharmaceutical composition of claim 33 , wherein the composition is in thermo-welded bags.

35. The pharmaceutical composition of claim 32 , wherein the composition is in tablet form.

36. The pharmaceutical composition of claim 32 , wherein the excipient is selected from the group consisting of diluents, ligands, lubricants, disintegrants, dyes, flavors and sweeteners.

Assignments (3)
CHANGE OF ADDRESS Recorded Oct 15, 2019
From: ALFASIGMA S.P.A.
To: ALFASIGMA S.P.A.
Reel/Frame 050727/0652 →
MERGER Recorded Nov 14, 2017
From: ALFA WASSERMANN S.P.A.
To: ALFASIGMA S.P.A.
Reel/Frame 045061/0645 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 12, 2016
From: MAFFEI, PAOLA; BACHETTI, MILENA; BOTTONI, GIUSEPPE; VISCOMI, GIUSEPPE CLAUDIO
To: ALFA WASSERMANN S.P.A.
Reel/Frame 039138/0805 →