Removing Polyphenol Contaminants from Feedstock-based Polyphenols

Abstract

A method of producing a mixture of pure feedstock-based native polyphenols from a feedstock. Contaminant polyphenols are first removed from an enzyme solution for converting feedstock to a product to produce a polyphenol reduced enzyme solution. The polyphenol reduced enzyme solution is combined with the feedstock and the feedstock is converted to a product and by-product. Heretofore, there has been no process available to reduce or remove the contaminant phenols introduced to the feedstock by commercial enzyme solutions. This method allows for the removal of contaminant phenols prior to introduction to the processing stream and subsequent harvesting of pure feedstock—based native polyphenols. The pure feedstock-based polyphenols are removed from the product or by-product to produce a pure mixture of feedstock-based polyphenols.

Claims

1. A method of producing a pure mixture of native feedstock-based polyphenols from a feedstock for making alcohols or sugars, comprising the steps of: prior to enzymatic processing of the feedstock removing contaminating polyphenols from an enzyme solution for converting feedstock to an alcohol or sugar to produce a polyphenol removed enzyme solution; combining the polyphenol removed enzyme solution with the feedstock; enzymatic processing of the feedstock without contaminating phenols being present by converting the feedstock to at least one of alcohol or sugar, wherein contaminating polyphenols are phenols or polyphenols not sourced from the feedstock; and producing the pure mixture of native feedstock-based polyphenols from the feedstock free of the contaminating polyphenols from the enzyme solution by separating native feedstock-based polyphenols from at least one of the alcohol, the sugar, or a by-product of the conversion of the feedstock to the sugar or the alcohol, wherein a native composition of the feedstock-based polyphenols is preserved in the pure mixture of native feedstock-based polyphenols and the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols is suitable for consumption.

2. The method of claim 1, wherein the feedstock comprises a grain.

3. The method of claim 2, wherein the grain comprises at least one of wheat, corn, barley, sorghum, oats, rye, soybean or canola.

4. The method of claim 1, wherein the by-product comprises an oil.

5. The method of claim 1, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols has beneficial human health effects.

6. The method of claim 5, wherein the beneficial health effect is digestive health.

7. The method of claim 1, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols is suitable for use as a food additive.

8. The method of claim 7, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols prevents oxidation of food.

9. The method of claim 1, wherein the feedstock comprises at least one of sugarcane, sugarbeets, woody biomass, grasses, algae, beans, fruits, and legumes.

10. The method of claim 1, wherein the feedstock is an edible biomass.

11. A method of producing a pure mixture of native feedstock-based polyphenols from a feedstock comprising a renewable biological material, comprising the steps of: prior to enzymatic processing of the feedstock, removing contaminating polyphenols from an enzyme solution for converting the feedstock to a product to produce a polyphenol removed enzyme solution; combining the polyphenol removed enzyme solution with the feedstock; an-GI enzymatic processing of the feedstock without contaminating phenols being present by converting the feedstock to the product, wherein contaminating polyphenols are phenols or polyphenols not sourced from the feedstock; and producing the pure mixture of native feedstock-based polyphenols free of the contaminating polyphenols from the enzyme solution by separating native feedstock-based polyphenols from the product or a by-product of the conversion of the feedstock to the product, wherein a native composition of the feedstock-based polyphenols is preserved in the pure mixture of native feedstock-based polyphenols and the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols is suitable for consumption.

12. The method of claim 11, wherein the feedstock comprises a grain.

13. The method of claim 12, wherein the grain comprises at least one of wheat, corn, barley, sorghum, oats, rye, soybean or canola.

14. The method of claim 11, wherein the by-product comprises an oil.

15. The method of claim 11, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols has beneficial human health effects.

16. The method of claim 15, wherein the beneficial health effect is digestive health.

17. The method of claim 11, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols is suitable for use as a food additive.

18. The method of claim 17, wherein the pure mixture of native feedstock-based polyphenols free of a contaminating polyphenols prevents oxidation of food.

19. The method of claim 11, wherein the feedstock comprises at least one of sugarcane, sugarbeets, woody biomass, grasses, algae, beans, fruits, and legumes.

20. The method of claim 11, wherein the feedstock is an edible biomass.

21. A method of treating an ailment in a human comprising the human consuming an effective amount of the pure mixture of native feedstock-based polyphenols free of the contaminating polyphenols from the enzyme solution formed according to claim 1.

22. A method of treating an ailment in a human comprising the human consuming an effective amount of the pure mixture of native feedstock-based polyphenols free of the contaminating polyphenols from the enzyme solution formed according to claim 11.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0025] FIG. 1 shows a side view of an apparatus for reformulating stabilized enzyme preparations; and

[0026] FIG. 2 is a overlaid chromatogram of various components of the present invention.

DETAILED DESCRIPTION OF THE INVENTION

[0027] The feedstock of use in the practice of the present invention, can be any renewable, biological material that can be converted to a product, such as a fuel, food or energy product, using an enzyme composition, and which contain native polyphenols. Preferred feedstocks are grain materials, such as corn, wheat, barley, sorghum, oats, rye, soybean, canola, etc. The feedstock however, can also be any carbohydrate, lipid and protein based material such as sugarcane, sugarbeets, woody biomass, grasses, algae, beans, fruits, and legumes. Preferably, the feedstock is an edible biomass.

[0028] The enzyme compositions can be any desired enzyme composition. For example, the present invention can be used in the commercial processing of feedstocks that utilize enzyme compositions, wherein the enzyme compositions comprise alpha-amylase, glucoamylase, cellulase, hem icellulase, beta-glucanase, invertase, lipase, protease, and related enzymes, or the like, to hydrolyze starch, cellulose, hemicellulose, lipids and proteins.

[0029] In general however, commercial production of products from feedstock using enzyme compositions is now well known, and the process of the present invention is applicable for any commercial production process of feedstock using enzyme compositions to make a product, and specifically when mixtures of pure feedstock-based native polyphenols are desired.

[0030] Removal of polyphenols from the enzyme composition, prior to use of the enzyme composition, can be performed using any desired process, such as, but not limited to, the process described in my previous U.S. Pat. No. 8,349,591.

[0031] Additionally, removal of the pure feedstock-based native polyphenols from the product or by-product can be achieved using any desired process for separating polyphenols from the product or by-product.

[0032] The native polyphenols from the feedstock, even those from mills used for biofuel production, can show beneficial human health effects. These effects include reduction in vasoreactivity, cholesterol levels, dementia, and cardiovascular disease including but not limited to stroke, myocardial infarction, and cardiovascular death.

[0033] The invention will now be explained with reference to the attached figures without being limited thereto.

[0034] As shown in the drawing in FIG. 1, the enzyme reformulation apparatus and method for removing contaminant phenols prior to introduction of the enzyme to the feedstock stream comprises an optional buffer vessel 1, a mixing vessel 2, a column containing a metal or metal-impregnated particulate matter or activated carbon material 3,a storage vessel 4, and an optional surge tank 10. The mixing vessel 2, the storage vessel 4, and surge vessel 10 are all preferably constructed of 304 or 316 stainless steel but can be constructed of any desired material suitable to hold the solutions.

[0035] The buffer vessel 1 contains a polymeric compound or a mixture of water and polymeric compound. The desired final concentration of polymeric compound in mixing vessel 2 can be adjusted accordingly. The polymeric compound 11 can be pumped using a variable speed pump 5 to the mixing vessel 2 containing the necessary quantity of water 22 to obtain the desired concentration of the polymeric compound. Once the final concentration of buffer is reached in mixing vessel 2, commercial enzyme preparation 23 is added to the mixing vessel 2.

[0036] Commercial enzyme preparation 23 is reformulated in the mixing vessel with water and polymeric compound. Passing the composition through the column 3 (over a time period between 1 and 15 minutes) which column is composed of a metal, a metal impregnated material, or activated carbon, facilitates the reformulation and removal of phenol contaminants in the enzyme solution, and the reformulated enzyme (and now phenol deplete solution) is collected in storage vessel 4. An optional surge tank 10 can be connected to the storage vessel 4 so that the storage vessel 4 can be emptied as desired. The reformulated and now phenol deplete enzyme solution is added to bioreactor 9. The reformulated and phenol depleted enzyme solution may sit in storage vessel 4 for up to 100 hours.

[0037] The reformulated polyphenol deplete enzyme solution can be pumped to the bioreactor with a variable speed pump 7. Two variable drive pumps 7 and 8 are in communication with each other and flow meters 27 and 28 to ensure adequate delivery of enzyme to the bioreactor.

[0038] The control system 18 for the apparatus contains programmed settings for the automated control of all valves and pumps associated with the apparatus and process. A computer screen provides visual cues to operators for tasks to complete.

[0039] Upon completion of the reformulation process for enzyme dose optimization and reduction and/or removal of phenol contaminants, the enzyme preparation is now ready for introduction to the bioreactor where the feedstock to be treated, will not be contaminated by the addition of contaminant phenols, and the reactant product(s) from the feedstock treatment, may be subsequently removed in a downstream process.

EXAMPLE 1

[0040] A commercial enzyme solution was processed to decrease the amount of contaminant phenol. The reformulated, phenol reduced solution was obtained by mixing 1 part of Liquozyme SC DS, a stabilized alpha-amylase from Novozymes, with 9 parts water and 1 part propylene glycol at room temperature. The enzyme solution was passed through a column containing activated carbon over a period of 15 minutes. A 5 ml of sample was collected and subsequently analyzed.

[0041] 5 ml of Liquozyme SC DS, 5 ml of reformulated, phenol reduced enzyme, and 4 grams of activated carbon were analysed by qualitative gas chromatography/mass spectroscopy (GC/MS) with a Supelco Grey (50/30 Micrometer DVB/CAR/PDMS) fiber at 80 degrees C. with 30 minute extraction time. The samples were analysed by GC/MS with water and air blanks. The sample chromatograms were evaluated against the blanks and the differences were characterized. The peaks were integrated and the average of the replicate preparations were reported.

[0042] The primary difference was the reformulated, phenol reduced enzyme contained a significant amount of propylene glycol. The Liquozyme SC DS contained more free fatty acids and sorbic acid.

[0043] At retention time 14.25 a comparison of the phenol levels was: 1,154,775 for the Liquozyme SC DS, 229,226 for diluted enzyme, 113,352 for reformulated, phenol reduced enzyme, and 69,021 for the spent activated carbon.

[0044] See FIG. 2 for a partial zoomed overlaid chromatogram of results.

[0045] These results illustrate the ability to reformulate a commercial enzyme and reduce phenol contamination of the subsequent enzyme product such that it may be added without activity degradation, and with phenol contamination minimized, so that the native polyphenols may subsequently be harvested from the feedstock during downstream processing.

[0046] While the claimed invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one of ordinary skill in the art that various changes and modifications can be made to the claimed invention without departing from the spirit and scope thereof.