Isolation of polyphenolic compounds from fruits or vegetables utilizing sub-critical water extraction

• US 7,208,181 B1
• Filed: 06/12/2002
• Issued: 04/24/2007
• Est. Priority Date: 06/12/2002
• Status: Expired due to Fees

• Current Assignee: The United States of America As Represented By The Secretary of Agriculture
• Original Assignee: United States Department Of Agriculture
• Inventors: King, Jerry W., Grabiel, Richard D.
• Primary Examiner(s): FLOOD, MICHELE C
• Application Number:
  US10/171,258
• Time in Patent Office: 1,777 Days
• Field of Search: 424/725, 424/777, 424/735, 424/732, 424/736, 424/757, 424/765, 424/750, 424/776, 424/779, 426/425, 426/431, 426/489
• US Class Current: 424/725
• CPC Class Codes: A23L 33/105 Plant extracts, their artificial duplicates or their derivatives
• CPC Class Codes: A23L 5/43 using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
• CPC Class Codes: A23V 2002/00 Food compositions, function of food ingredients or processes for food or foodstuffs
• CPC Class Codes: A23V 2250/2104 Anthocyanins
• CPC Class Codes: C09B 61/00 Dyes of natural origin prepared from natural sources , e.g. vegetable sources

Abstract

Anthocyanins, other flavonoids and related polyphenolic compounds are extracted from fruits or highly pigmented garden vegetables and their by-products using subcritical water with or without a secondary cosolvent. This method has the advantages of being relatively inexpensive, minimizes or totally avoids the use of objectionable solvents, and provides a facile means for supplying an ample source of concentrated phytochemicals for use in food formulation, dietary supplements and phyto-pharmaceutical applications.

Claims

1. A method for extracting an anthocyanin compound in its substantially native, chemically unaltered state from a fruit or vegetable material, wherein said fruit material is obtained from a source species selected from the group consisting of Aronia, Citrus, Empetrum, Fragaria, Hylocereus, Malus, Morus, Prunus, Punica, Pyrus, Ribes, Rubus, Sambucus, Solanum and blueberry species of Vaccinium, and said vegetable material is obtained from a source species selected from the group consisting of Beta, Brassica, Daucus, Ipomoea, Rhapanus, Solanum, and Zea, comprising:

a. treating said fruit or vegetable material with a continuous flow of aqueous solvent system through said material under subcritical conditions sufficient to dissolve said anthocyanin compound into the aqueous solvent system to obtain an aqueous solvent system having a dissolved anthocyanin compound, wherein said subcritical conditions comprise a temperature in a range of 75–

200°

C., an extraction pressure of 10–

50 Bar, a pH less than 5.0, and a superficial velocity of at least 0.1 cm/sec;

b. rapidly cooling said aqueous solvent system having said dissolved anthocyanin compound; and

c. recovering an extract comprising the aqueous solvent system and said dissolved anthocyanin compound in its native, chemically unaltered state.

2. The method of claim 1, wherein said fruit or vegetable material is selected from the group consisting of whole fruits or vegetables, partial fruits or vegetables, processed fruits or vegetables, and fruit- or vegetable-derived substrates.

3. The method of claim 2, wherein said fruit- or vegetable-derived substrate is selected from the group consisting of seeds, stems, skins, fiber and pomace.

4. The method of claim 1, wherein said material is a fruit material obtained from a source selected from the group consisting of elderberry, blueberry, bilberry, chokeberry, raspberry, blackberry, red currant, black currant, strawberry, mulberry, lingonberry, pear, apple, peach, plum, cherry, and pomegranate.

5. The method of claim 1, wherein said material is a fruit material obtained from a source selected from the group consisting of elderberry, chokeberry, blueberry, bilberry and raspberry.

6. The method of claim 1, wherein water is the principal component of the aqueous solvent system comprising water and a lesser amount of a cosolvent other than water.

7. The method of claim 6, wherein said cosolvent is ethanol.

8. The method of claim 6, wherein said cosolvent is present in said solvent system at a level of less than 45% (v/v).

9. The method of claim 6, wherein said cosolvent is present in said solvent system at a level of less than 30% (v/v).

10. The method of claim 6, wherein said cosolvent is present in said solvent system at a level of less than 20% (v/v).

11. The method of claim 1, wherein water is the sole component of the aqueous solvent system.

12. The method of claim 11, wherein said water is acidified.

13. The method of claim 1, wherein one of said subcritical conditions is a pH of less than 2.0.

14. The method of claim 1, wherein said subcritical conditions comprise a temperature in a range of 100–

150°

C. and a pH between 1 and less than 5.0.

15. A method for extracting an anthocyanin compound in its substantially native, chemically unaltered state from a fruit or vegetable material, wherein said fruit material is obtained from a source species selected from the group consisting of Aronia, Citrus, Empetrum, Fragaria, Hylocereus, Malus, Morus, Prunus, Punica, Pyrus, Ribes, Rubus, Sambucus, Solanum and blueberry species of Vaccinium, and said vegetable material is obtained from a source species selected from the group consisting of Beta, Brassica, Daucus, Ipomoea, Rhapanus, Solanum, and Zea, comprising:

b. treating said fruit or vegetable material with a continuous flow of solvent consisting essentially of water through said material under subcritical conditions sufficient to dissolve said compound into the solvent, wherein said subcritical conditions comprise a temperature in a range of 100–

200°

C., an extraction pressure of 10–

50 Bar, a pH less than 5.0, and a superficial velocity of at least 0.1 cm/sec;

b. rapidly cooling said solvent having said dissolved compound; and

c. recovering an extract comprising the solvent and said dissolved anthocyanin compound in its native, chemically unaltered state.

16. The method of claim 15, wherein said fruit or vegetable material is selected from the group consisting of whole fruits or vegetables, partial fruits or vegetables, processed fruits or vegetables, and fruit- or vegetable-derived substrates.

17. The method of claim 16, wherein said fruit- or vegetable-derived substrate is selected from the group consisting of seeds, stems, skins, fiber and pomace.

18. The method of claim 15, wherein said material is a fruit material obtained from a source selected from the group consisting of elderberry, blueberry, bilberry, chokeberry, raspberry, blackberry, red currant, black currant, strawberry, mulberry, lingonberry, pear, apple, peach, plum, cherry, and pomegranate.

19. The method of claim 15, wherein said material is a fruit material obtained from a source selected from the group consisting of elderberry, chokeberry, blueberry, bilberry and raspberry.