Method of producing a vitamin product

• US 6,139,872 A
• Filed: 08/13/1997
• Issued: 10/31/2000
• Est. Priority Date: 08/14/1996
• Status: Expired due to Term

• Current Assignee: Cognis International GmbH (BASF SE)
• Original Assignee: Henkel Corporation (Henkel AG & Co KGaA)
• Inventors: Walsh, Leo
• Primary Examiner(s): Spear, James M.
• Application Number:
  US08/917,049
• Time in Patent Office: 1,175 Days
• Field of Search: 424/464, 424/465, 424/489, 424/195.1
• US Class Current: 424/464
• CPC Class Codes: A23L 33/10 using additives addition of substantially indigestible substances A23L33/21
• CPC Class Codes: A23L 33/105 Plant extracts, their artificial duplicates or their derivatives
• CPC Class Codes: A23P 10/25 Agglomeration or granulation by extrusion or by pressing, e.g. through small holes, through sieves or between surfaces
• CPC Class Codes: A23V 2002/00 Food compositions, function of food ingredients or processes for food or foodstuffs
• CPC Class Codes: A23V 2250/06 Amino acid
• CPC Class Codes: A23V 2250/156 Mineral combination undefined extract A23V2250/1638
• CPC Class Codes: A23V 2250/1882 Polyunsaturated fatty acids
• CPC Class Codes: A23V 2250/204 Animal extracts
• CPC Class Codes: A23V 2250/21 Plant extracts
• CPC Class Codes: A23V 2250/2136 Phytosterols, phytostanols
• CPC Class Codes: A23V 2250/21362 Campestanol
• CPC Class Codes: A23V 2250/21364 Campesterol
• CPC Class Codes: A23V 2250/21372 Sitosterol
• CPC Class Codes: A23V 2250/21374 Stigmastanol
• CPC Class Codes: A23V 2250/21376 Stigmasterol
• CPC Class Codes: A23V 2250/70 Vitamins
• CPC Class Codes: A23V 2250/702 Vitamin A
• CPC Class Codes: A23V 2250/704 Vitamin B
• CPC Class Codes: A23V 2250/712 Vitamin E
• CPC Class Codes: A61K 9/1688 resulting in pure drug agglomerate optionally containing up to 5% of excipient
• CPC Class Codes: A61P 3/02 : Nutrients, e.g. vitamins, minerals
• CPC Class Codes: C07D 311/72 : 3,4-Dihydro derivatives having in position 2 at least one methyl radical and in position 6 one oxygen atom, e.g. tocopherols

Abstract

A process for producing a nutrient supplement powder is provided. The process forms a powder into a plastic mass which is not completely molten. The plastic mass is then formed into an elongated shape and allowed to cool to set to a solid state. The solid is then comminuted to obtain a powder having a desirable particle size, e.g. not more than 5% by weight through a 120-mesh sieve and not more than 5% by weight retained on a 14-mesh sieve.

Claims

1. A process for producing a substantially physiologically inert binder free, particulate composition wherein the binder consists essentially of a plastic nutritional supplement which process comprises:

heating a mass of the plastic nutritional supplement to a temperature not above about 170°

C., effective to form a plastic but not completely molten, mass of material,

extruding the plastic mass of material into at least one elongated form;

cooling the elongated form for a sufficient Time for the elongated form to set to a solid form; and

comminuting the solid form.

3. The process of claim 1 wherein the heating is accomplished in an extrusion zone.

4. The process of claim 1 wherein the elongated form is a rope having a diameter of from about 0.1 mm to about 2 mm.

5. The process of claim 4 wherein the diameter is from about 0.4 mm to about 0.6 mm.

6. The process of claim 1 wherein the elongated form sets to a solid form within one hour of the beginning of the cooling of the elongated form.

7. The process of claim 1 wherein the elongated form sets to a solid form within about 30 minutes of the beginning of cooling the elongated form.

8. The process of claim 1 wherein the elongated form sets to a solid form within about 10 minutes of the beginning of cooling the elongated form.

9. The process of claim 1 wherein the elongated form sets to a solid form in less than about 30 seconds of the beginning of cooling the elongated form.

10. The process of claim 1 wherein the solid form is comminuted by impacting the solid form.

11. The process of claim 10 wherein the comminuting does not compact the particles.

12. The process of claim 1 wherein the solid form is comminuted in an impact zone where there is no contact of impacting members of the impact zone with an opposing surface of the impact zone.

13. The process of claim 1 wherein the comminuted product has a particle size distribution wherein not more than 5% by weight passes through a 120-mesh sieve.

14. The process of claim 1 wherein the comminuted product has a particle size distribution wherein less than 5% by weight is retained on a 14 mesh sieve.

15. The process of claim 1 wherein the comminuted product has a particle size distribution wherein at least about 25% by weight of the comminuted product passes through a 25 mesh sieve and is retained on a 60-mesh sieve.

16. The process of claim 1 wherein the plastic nutritional supplement is selected from the group consisting of tocopheryl succinate, phytosterols and mixtures thereof.

17. The process of claim 16 wherein the phytosterols are selected from the group consisting of sterols, sterol esters, stanols, stanol esters and mixtures thereof.

18. The process of claim 17 wherein the sterols are selected from the group consisting of alpha-sitosterol, beta-sitosterol, gamma-sitosterol, campesterol, stigmasterol, brassicasterol and mixtures thereof.

19. The process of claim 17 wherein the stanols are selected from the group consisting of stigmastanol, ergostanol, campestanol and mixtures thereof.

20. The process of claim 17 wherein the phytosterols comprise:

beta-sitosterol;

campesterol;

stigmasterol; and

brassicasterol.

21. The process of claim 17 wherein the phytosterols comprise:

about 43 to about 53 wt. % beta-sitosterol;

about 22 to about 26 wt. % campesterol;

about 17 to about 19 wt. % stigmasterol; and

about 2 wt. % brassicasterol, wherein wt % is based on the total plant extract.

22. The product of the process of claim 1, wherein said product comprises phytosterols.

2. A process of producing a substantially binder free particulate composition comprising a plastic nutritional supplement which comprises:

heating a mass of the plastic nutritional supplement to an elevated temperature effective to form a plastic, but not completely molten, mass of material;

extruding the plastic mass of material into an atomizer head; and

atomizing the plastic mass of material into particles.

33. The particles of the process of claim 2, wherein said particles comprise phytosterols.

34. The process of claim 2 wherein the elevated temperature is not above about 170°

C.

35. The process of claim 2 wherein the heating is accomplished in an extrusion zone.

36. The process of claim 2 wherein the plastic nutritional supplement is selected from the group consisting of tocopheryl succinate, phytosterols and mixtures thereof.

37. The process of claim 36 wherein the phytosterols are selected from the group consisting of sterols, sterol esters, stanols, stanol esters and mixtures thereof.

38. The process of claim 37 wherein the sterols are selected from the group consisting of alpha-sitosterol, beta-sitosterol, gamma-sitosterol, campesterol, stigmasterol, brassicasterol and mixtures thereof.

39. The process of claim 37 wherein the stanols are selected from the group consisting of stigmastanol, ergostanol, campesterol and mixtures thereof.

40. The process of claim 37 wherein the phytosterols comprise:

beta-sitosterol;

campesterol;

stigmasterol; and

brassicasterol.

41. The process of claim 37 wherein the phytosterols comprise:

about 43 to about 53 wt. % beta-sitosterol;

about 22 to about 26 wt. % campesterol;

about 17 to about 19 wt. % stigmasterol; and

about 2 wt. % brassicasterol, wherein the wt. % is based on the total plant extract.

23. A process of producing a substantially physiologically inert binder free, particulate composition wherein the binder consists essentially of a plastic nutritional supplement which comprises:

heating a mass of the plastic nutritional supplement to an elevated temperature effective to form a plastic, but not completely molten, mass of material;

extruding the plastic mass of material into an injection molding head; and

molding tablets of said plastic nutritional supplement.

24. The process of claim 23 wherein the elevated temperature is not above about 170°

C.

25. The process of claim 23 wherein the heating is accomplished in an extrusion zone.

26. The process of claim 23 wherein the plastic nutritional supplement is selected from the group consisting of tocopheryl succinate, phytosterols and mixtures thereof.

27. The process of claim 26 wherein the phytosterols are selected from the group consisting of sterols, sterol esters, stanols, stanol esters and mixtures thereof.

28. The process of claim 27 wherein the sterols are selected from the group consisting of alpha-sitosterol, beta-sitosterol, gamma-sitosterol, campesterol, stigmasterol, brassicasterol and mixtures thereof.

29. The process of claim 27 wherein the stanols are selected from the group consisting of stigmastanol, campestanol, ergostanol and mixtures thereof.

30. The process of claim 26 wherein the phytosterols comprise:

beta-sitosterol;

campesterol;

stigmasterol; and

brassicasterol.

31. The process of claim 26 wherein the phytosterols comprise:

about 43 to about 53 wt. % beta-sitosterol;

about 22 to about 26 wt. % campesterol;

about 17 to about 19 wt. % stigmasterol; and

about 2 wt. % brassicasterol, wherein wt. % is based on the total plant extract.

32. The tablets of the process of claim 23.