IP Library Granted Patent US 8,404,293
Granted Patent B2
US 8,404,293 · App. 12/889,109 · Granted Mar 26, 2013

Method for separating and concentrating bioactive phenolics

Inventors: Nirmal K. Sinha (Frankfort, MI); Meena Sinha (Frankfort, MI)
Assignee: Graceland Fruit, Inc.
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Quick Facts
Patent No.
US 8,404,293
App. No.
12/889,109
Granted
Mar 26, 2013
Kind
B2
Abstract

A method for physical separation and purification of bioactive phenolics from fruits, berries and vegetables by subjecting a fruit, berry or vegetable extract solution having a Brix of from about 1 to about 4 to ultrafiltration using an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F. This is followed by subjecting the resulting retentate to diafiltration-ultrafiltration with the addition of water, using an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F., and recovering the diafiltered retentate or the bioactive phenolic containing solids thereof.

Claims (30)

1. A method for physical separation and concentration of bioactive phenolics having molecular weights of less than 1,000 Daltons from fruits, berries and vegetables comprising: subjecting a fruit, berry or vegetable extract solution having a Brix of from about 1 to about 4 to ultrafiltration using an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F., followed by subjecting the resulting retentate to diafiltration-ultrafiltration with the co-injection of water, using an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F., and recovering the diafiltered retentate containing bioactive phenolics having molecular weights of less than 1,000 Daltons.

2. The method of claim 1 in which said ultrafiltration is conducted using an about 4,000-6,000 Dalton cutoff ultrafiltration membrane.

3. The method of claim 2 in which said ultrafiltration is conducted using an about 5,000 Dalton cutoff ultrafiltration membrane.

4. The method of claim 2 in which said diafiltration-ultrafiltration is conducted using the same ultrafiltration membrane as is used in said ultrafiltration.

5. The method of claim 2 in which said diafiltration-ultrafiltration is conducted using an about 2,000-4,000 Dalton cut-off ultrafiltration membrane.

6. The method of claim 5 in which said diafiltration-ultrafiltration is conducted using an about 3,000 Dalton cut-off ultrafiltration membrane.

7. The method of claim 2 in which both said ultrafiltration and said diafiltration are conducted at about 30-60 psi.

8. The method of claim 7 in which both said ultrafiltration and said diafiltration are conducted at about 45 psi.

9. The method of claim 2 in which both said ultrafiltration and said diafiltration are conducted at about 60-120 psi.

10. The method of claim 2 in which both said ultrafiltration and said diafiltration are conducted at about 100 psi.

11. The method of claim 5 in which the retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

12. The method of claim 2 in which retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

13. The method of claim 1 in which the retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

14. The method of claim 5 in which both said ultrafiltration and said diafiltration are conducted at about 100-110° F.

15. The method of claim 2 in which both said ultrafiltration and said diafiltration are conducted at about 100-110° F.

16. The method of claim 1 in which both said ultrafiltration and said diafiltration are conducted at about 100-110° F.

17. The method of claim 5 in which said ultrafiltration is discontinued when the flow rate through said ultra-filter drops to less than about 15 liters per minute.

18. The method of claim 2 in which said ultrafiltration is discontinued when the flow rate through said ultra-filter drops to less than about 15 liters per minute.

19. The method of claim 1 in which said ultrafiltration is discontinued when the flow rate through said ultra-filter drops to less than about 4 liters per square meter of membrane area per hour or 4.0 LMH.

20. A method for separating and concentrating bioactive phenolics having molecular weights of less than 1,000 Daltons from fruits, berries and vegetables comprising: subjecting a fruit, berry or vegetable extract solution having a Brix of from about 1 to about 4 to ultrafiltration, with recirculation of the retentate, using an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F.; discontinuing said ultrafiltration when the flow rate of said extract and said recycled retentate through said ultrafiltration membrane drops to less than about 4 liters per square meter of membrane area per hour or 4.0 LMH, thereby creating an ultrafiltered retentate; followed by subjecting the ultrafiltered retentate to diafiltration-ultrafiltration by recirculating said ultrafiltered retentate, with the addition of water at a rate of about one quarter to about one half liter of water per liter of retentate, through an about 2,000-6,000 Dalton cutoff ultrafiltration membrane under a pressure of about 30-120 psi, and a temperature of about 80-110° F., until the total added water used is about 1 and ½ to about 3 times the volume of the ultrafiltered retentate; and recovering the diafiltered retentate containing bioactive phenolics having molecular weights of less than 1,000 Daltons.

21. The method of claim 20 in which said ultrafiltration is conducted using an about 4,000-6,000 Dalton cutoff ultrafiltration membrane.

22. The method of claim 21 in which said diafiltration-ultrafiltration is conducted using the same ultrafiltration membrane as is used in said ultrafiltration.

23. The method of claim 21 in which said diafiltration-ultrafiltration is conducted using an about 2,000-4,000 Dalton cut-off ultrafiltration membrane.

24. The method of claim 23 in which both said ultrafiltration and said diafiltration are conducted at about 30-60 psi.

25. The method of claim 24 in which the retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

26. The method of claim 23 in which the retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

27. The method of claim 20 in which the retentates are recirculated both during said ultrafiltration and during said diafiltration-ultrafiltration.

28. The method of claim 24 in which both said ultrafiltration and said diafiltration are conducted at about 100-110° F.

29. The method of claim 23 in which both said ultrafiltration and diafiltration are conducted at about 100-110° F.

30. The method of claim 20 in which both said ultrafiltration and said diafiltration are conducted at about 100-110° F.

Assignments (4)
RELEASE OF SECURITY INTEREST Recorded Aug 12, 2022
From: THE HUNTINGTON NATIONAL BANK
To: GRACELAND FRUIT, INC.
Reel/Frame 060795/0579 →
SECURITY INTEREST Recorded Dec 19, 2017
From: GRACELAND FRUIT, INC.; GATEWAY PRODUCTS, INC.
To: PNC BANK, NATIONAL ASSOCIATION, AS AGENT
Reel/Frame 044437/0378 →
SECURITY AGREEMENT Recorded Jan 17, 2012
From: GRACELAND FRUIT, INC.
To: CITIZENS BANK
Reel/Frame 027544/0846 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 23, 2010
From: SINHA, NIRMAL K.; SINHA, MEENA
To: GRACELAND FRUIT, INC.
Reel/Frame 025071/0795 →
Continuity (1)
Related Publication 20120076904A1 · Mar 29, 2012