IP Library Granted Patent US 7,495,098
Granted Patent B2
US 7,495,098 · App. 11/578,627 · Granted Feb 24, 2009

Extraction of alkaloids from opium

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Quick Facts
Patent No.
US 7,495,098
App. No.
11/578,627
Granted
Feb 24, 2009
Kind
B2
Abstract

A method for extracting at least one alkaloid from opium that includes dissolving opium in a solvent, heating the dissolved opium solution, cooling the dissolved opium solution, adjusting the pH of the dissolved opium solution with at least one first weak acid, filtering the dissolved opium solution to recover a filtrate; and then separating and purifying at least one alkaloid in the filtrate. Preferably, this includes an additional step of chilling the opium solution after adjusting the pH of the dissolved opium solution with at least one first acid. The preferred method for separating and purifying at least one alkaloid in the filtrate includes utilizing preparative liquid chromatography, however, solvent extraction and filtration can also be utilized.

Claims (29)

1. A method for extracting at least one alkaloid from opium comprising:

dissolving opium in a solvent;

heating the dissolved opium solution to a temperature from about 70° Celsius to about 105° Celsius;

cooling the dissolved opium solution;

adjusting the pH of the dissolved opium solution with at least one weak acid;

filtering the dissolved opium solution to recover a filtrate, and

separating and purifying the at least one alkaloid in the filtrate.

2. The method for extracting at least one alkaloid from opium as set forth in claim 1 , further comprising chilling the opium solution after the adjusting the pH of the dissolved opium solution with at least one first acid.

3. The method for extracting at least one alkaloid from opium as set forth in claim 2 , wherein the step of chilling the opium solution is at a temperature from about 0° Celsius to about 30° Celsius.

4. The method for extracting at least one alkaloid from opium as set forth in claim 2 , wherein the step of chilling the opium solution is at a temperature from about 0° Celsius to about 25° Celsius.

5. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the solvent includes water.

6. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step of heating the dissolved opium solution is at a temperature from about 95° Celsius to about 105° Celsius.

7. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step of cooling the dissolved opium solution is at a temperature from about 25° Celsius to about 70° celsius.

8. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step of cooling the dissolved opium solution is at a temperature from about 40° Celsius to about 60° Celsius.

9. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step adjusting the pH of the dissolved opium solution is in a range from about 2 pH to about 4 pH.

10. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step adjusting the pH of the dissolved opium solution is in a range from about 2.5 pH to about 3.5 pH.

11. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein at least one weak acid includes acetic acid and formic acid.

12. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the at least one weak acid is selected from the group consisting of acetic acid, formic acid, carbonic acid, citric acid, propionic acid, trichloroacetic acid, nicotinic acid, pyruvic acid and conjugate acids of weak bases.

13. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein after the step of adjusting the pH of the dissolved opium solution further comprises the step of stirring the dissolved opium solution from about 60 minutes to about 720 minutes at a temperature from about 25° Celsius to about 70° Celsius.

14. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein after the step of adjusting the pH of the dissolved opium solution further comprises the step of stirring the dissolved opium solution from about 120 minutes to about 240 minutes at a temperature from about 40° Celsius to about 60° Celsius.

15. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein after the step of stirring the dissolved opium solution further comprises the step of adding filter aids to the opium solution.

16. The method for extracting at least one alkaloid from opium as set forth in claim 15 , wherein the filter aids are selected from the group consisting of diatomite, perlite, dicalite, vegetable grain, diatomaceous earth, calcium silicate, magnesium silicate, amorphous silicas and cellulose.

17. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the filtering of dissolved opium solution to recover a filtrate is under a vacuum.

18. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the filtering of the dissolved opium solution to recover a filtrate is done with a horizontal belt filter.

19. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the filtering of the dissolved opium solution to recover a filtrate includes forming a filter cake and washing the filter cake with an acidified solvent.

20. The method for extracting at least one alkaloid from opium as set forth in claim 19 , wherein the step of washing the filter cake with an acidified solvent is under a vacuum.

21. The method for extracting at least one alkaloid from opium as set forth in claim 20 , wherein the acidified solvent includes a solvent, which includes water and the acid is selected from the group consisting of acetic acid, formic acid, carbonic acid, citric acid, propionic acid, trichloroacetic acid, nicotinic acid, pyruvic acid and conjugate acids of weak bases.

22. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step of separating and purifying at least one alkaloid in the filtrate includes utilizing preparative liquid chromatography.

23. The method for extracting at least one alkaloid from opium as set forth in claim 1 , wherein the step of separating and purifying the at least one alkaloid in the filtrate includes utilizing solvent extraction and filtration.

Assignments (3)
RELEASE OF PATENT SECURITY INTERESTS RECORDED AT REEL 032480, FRAME 0001 Recorded Nov 16, 2023
From: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
To: THERAKOS, INC.; MALLINCKRODT INTERNATIONAL FINANCE S.A.; MALLINCKRODT CB LLC; MALLINCKRODT FINANCE GMBH; MALLINCKRODT US HOLDINGS LLC (F/K/A MALLINCKRODT US HOLDINGS INC.); MALLINCKRODT CARRIBEAN, INC.; MALLINCKRODT US POOL LLC; MNK 2011 LLC (F/K/A MALLINCKRODT INC.); LUDLOW LLC (F/K/A LUDLOW CORPORATION); CNS THERAPEUTICS, INC.; MALLINCKRODT ENTERPRISES HOLDINGS LLC (F/K/A MALLINCKRODT ENTERPRISES HOLDINGS, INC.); MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; LAFAYETTE PHARMACEUTICALS LLC; LIEBEL-FLARSHEIM COMPANY LLC; MALLINCKRODT BRAND PHARMACEUTICALS LLC (F/K/A MALLINCKRODT BRAND PHARMACEUTICALS, INC.); MALLINCKRODT VETERINARY, INC.; MALLINCKRODT US HOLDINGS LLC; IMC EXPLORATION COMPANY; MEH, INC.; MALLINCKRODT HOSPITAL PRODUCTS IP UNLIMITED COMPANY (F/K/A MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED); MALLINCKRODT ARD IP UNLIMITED COMPANY (F/K/A MALLINCKRODT ARD IP LIMITED); OCERA THERAPEUTICS LLC (F/K/A OCERA THERAPEUTICS, INC.); SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC (F/K/A VTESSE INC.); MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY (F/K/A MALLINCKRODT PHARMA IP TRADING D.A.C.); INFACARE PHARMACEUTICAL CORPORATION; ST SHARED SERVICES LLC; IKARIA THERAPEUTICS LLC; INO THERAPEUTICS LLC
Reel/Frame 065609/0322 →
SECURITY INTEREST Recorded Mar 19, 2014
From: MALLINCKRODT INTERNATIONAL FINANCE S.A.; MALLINCKRODT CB LLC; MALLINCKRODT FINANCE GMBH; MALLINCKRODT US HOLDINGS INC.; MALLINCKRODT CARIBBEAN, INC.; MALLINCKRODT US POOL LLC; MALLINCKRODT INC.; LUDLOW CORPORATION; CNS THERAPEUTICS, INC.; ENTERPRISES HOLDINGS, INC.; MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; LAFAYETTE PHARMACEUTICALS LLC; LIEBEL-FLARSHEIM COMPANY LLC; MALLINCKRODT BRAND PHARMACEUTICALS, INC; MALLINCKRODT VETERINARY, INC.; MALLINCKRODT US HOLDINGS LLC; IMC EXPLORATION COMPANY; MEH, INC; MALLINCKRODT ENTERPRISES HOLDINGS, INC.
To: DEUTSCHE BANK AG NEW YORK BRANCH
Reel/Frame 032480/0001 →
CHANGE OF LEGAL ENTITY Recorded Aug 16, 2011
From: MALLINCKRODT INC.
To: MALLINCKRODT LLC
Reel/Frame 026754/0001 →