IP Library Granted Patent US 8,703,187
Granted Patent B2
US 8,703,187 · App. 12/148,987 · Granted Apr 22, 2014

Vitamin D content uniformity in pharmaceutical dosage forms

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Quick Facts
Patent No.
US 8,703,187
App. No.
12/148,987
Granted
Apr 22, 2014
Kind
B2
Abstract

New dosage forms of vitamin D and calcium carbonate having improved content uniformity are described. The improvements are realized through modifications to the formulation, the raw material specifications, and the process of manufacture.

Claims (29)

1. A method of manufacturing calcium carbonate/vitamin D tablets comprising:

forming a premix comprising a mixture of vitamin D granulation and silicon dioxide;

adding a calcium carbonate granulation to said premix to form a first vitamin D/calcium carbonate granulation mixture, wherein the calcium carbonate granulation has a median particle size within ±40% of the vitamin D granulation;

mixing and sieving the first vitamin D/calcium carbonate granulation mixture to form a sieved first vitamin D/calcium carbonate granulation mixture;

blending the first vitamin D/calcium carbonate granulation mixture in a V blender to form a blended first vitamin D/calcium carbonate granulation mixture;

dividing the blended first vitamin D/calcium carbonate granulation mixture into four equal portions and adding calcium carbonate to each portion to form a second vitamin D/calcium carbonate granulation mixture;

blending the second vitamin D/calcium carbonate granulation mixture in a V blender; and,

forming tablets from a composition comprising the second vitamin D/calcium carbonate granulation mixture.

2. The method of claim 1 , wherein said premix of vitamin D and silicon dioxide is in a mass ratio of about 25:9 vitamin D:silicon dioxide.

3. The method of claim 1 , wherein said first mixture is in a mass ratio of about 1000:25:9 calcium carbonate:vitamin D:silicon dioxide.

4. The method of claim 1 , wherein said step of mixing and sieving comprises sieving through a US 20 Mesh sieve.

5. The method of claim 1 , wherein said step of blending the second mixture in a V blender comprises blending for about 2 minutes.

6. The method of claim 1 , wherein said step of dividing the first mixture into four equal portions and adding calcium carbonate comprises adding 2.0 kg of calcium carbonate.

7. The method of claim 1 , further comprising the step of milling and sieving said calcium carbonate granulation and said vitamin D granulation to produce said calcium carbonate and vitamin D granulations having median particle sizes within ±40% of one another.

8. The method of claim 7 , wherein said median particle sizes are within ±25% of one another.

9. The method of claim 7 , wherein said median particle sizes are within ±15% of one another.

10. The method of claim 1 , further comprising the step of milling and sieving said calcium carbonate granulation to have a D 20 value of less than 110 microns.

11. The method of claim 1 , further comprising the step of milling and sieving said calcium carbonate granulation to have a D 16 value of less than 95 microns.

12. A method of manufacturing calcium carbonate/vitamin D tablets comprising:

forming a premix comprising a layer of calcium carbonate, a layer of vitamin D/silicon dioxide and another layer of calcium carbonate, wherein the calcium carbonate has a median particle size within ±40% of the vitamin D;

sieving and blending the premix to form a first vitamin D/calcium carbonate granulation mixture;

adding calcium carbonate to said first vitamin D/calcium carbonate granulation mixture such that there is a layer of calcium carbonate granulation, a layer of said first granulation mixture, and another layer of calcium carbonate, to form a second vitamin D/calcium carbonate granulation mixture;

sieving and blending the second vitamin D/calcium carbonate granulation mixture; and,

forming tablets from a composition comprising the second vitamin D/calcium carbonate granulation mixture.

13. The method of claim 12 , wherein one or both of said steps of sieving and blending the premix and sieving and blending the second vitamin D/calcium carbonate granulation mixture comprises blending with a V blender.

14. The method of claim 13 , wherein said step of sieving and blending the premix comprises blending with a V blender comprises blending for about 8 minutes.

15. The method of claim 13 , wherein said step of sieving and blending the second vitamin D/calcium carbonate granulation mixture comprises blending with a V blender comprises blending for about 50 minutes.

16. The method of claim 12 , wherein said step of forming a premix comprising a layer of calcium carbonate, a layer of vitamin D/silicon dioxide and another layer of calcium carbonate comprises adding two layers of about 500 kg each of calcium carbonate.

17. The method of claim 12 , wherein said first mixture is in a mass ratio of about 1600:20:7 calcium carbonate:vitamin D:silicon dioxide.

Assignments (5)
CORRECTIVE ASSIGNMENT TO CORRECT THE US PATENT NO. 8,050,873 PREVIOUSLY RECORDED ON REEL 040183 FRAME 0129. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Feb 22, 2018
From: WARNER CHILCOTT COMPANY, LLC
To: ALLERGAN PHARMACEUTICALS INTERNATIONAL LIMITED
Reel/Frame 045417/0593 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 29, 2016
From: WARNER CHILCOTT COMPANY, LLC
To: ALLERGAN PHARMACEUTICALS INTERNATIONAL LIMITED
Reel/Frame 040183/0129 →
RELEASE OF SECURITY INTEREST Recorded Oct 31, 2013
From: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
To: WARNER CHILCOTT COMPANY, LLC
Reel/Frame 031531/0538 →
RELEASE - REEL 023456, FRAME 0052 Recorded Mar 29, 2011
From: CREDIT SUISSSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT
To: WARNER CHILCOTT COMPANY LLC
Reel/Frame 026042/0046 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 8, 2010
From: PROCTER & GAMBLE COMPANY, THE
To: WARNER CHILCOTT COMPANY, LLC
Reel/Frame 023796/0417 →