PREPARATION OF NON-SOY OILSEED PROTEIN PRODUCTS ("*810")

Abstract

The present invention is directed to non-soy oilseed protein products, very low in, or free of, beany, green, vegetable or similar flavour notes and useful for the fortification of food and beverage products and prepared without the use of salt in the process. The non-soy oilseed protein products of the present invention are obtained by extracting non-soy oilseed protein source with water to form an aqueous non-soy oilseed protein solution, at least partially separating the aqueous non-soy oilseed protein solution from residual non-soy oilseed protein source, adjusting the pH of the aqueous non-soy oilseed protein solution to a pH between about 1.5 and a value about 1 pH unit lower than the typical pH of isoelectric precipitation to solubilize the bulk of the protein and form an acidified non-soy oilseed protein solution then separating the acidified non-soy oilseed protein solution from the acid insoluble solid material. The acidified non-soy oilseed protein solution may be dried following optional concentration and diafiltration to form a non-soy oilseed protein product, which may be an isolate. The acid insoluble solid material may be washed with acidified water and then dried to form another non-soy oilseed protein product. These products may be dried at the acidic pH at which they were prepared or may be adjusted in pH before drying.

Claims

1. A process of producing a sunflower protein product having a protein content selected from the group consisting of at least about 60, at least about 65, at least about 70, at least about 75, at least about 80, at least about 85 or at least about 90 wt % (N×6.25) on a dry weight basis, which process comprises: (a) extracting a sunflower protein source with water to cause solubilization of protein from the sunflower protein source and to form an aqueous protein solution and a residual sunflower protein source, (b) at least partially separating the aqueous sunflower protein solution from the residual sunflower protein source, (c) adjusting the pH of the aqueous sunflower protein solution to a pH of about 1.5 to about 3.5 to produce an acidified sunflower protein solution, (d) separating the acid insoluble solid material from the acidified sunflower protein solution, (e) optionally concentrating the acidified sunflower protein solution by a selective membrane technique, (f) optionally diafiltering the optionally concentrated sunflower protein solution, and (g) optionally drying the optionally concentrated and optionally diafiltered sunflower protein solution.

2. The process of claim 1, wherein said acid insoluble solid material is optionally diluted then optionally dried to form a sunflower protein product having a protein content of at least about 60, at least about 65, at least about 70, at least about 75 or at least about 80 wt % (N×6.25) on a dry weight basis.

3. The process of claim 2, wherein the pH of the optionally diluted acid insoluble solid material is raised to a value selected from the group consisting of less than about 8.0, about 6.0 to about 8.0 and about 6.5 to about 7.5, prior to the optional drying step.

4. The process of claim 2, wherein said acid insoluble solid material is washed by mixing with a quantity of water selected from the group consisting of about 1 to about 20 volumes of water and about 1 to about 10 volumes of water, having a pH selected from the group consisting of about 1.5 to about 3.5 and about the same as the pH of the acid insoluble material, then is separated from the wash solution prior to optional dilution then optional drying steps to obtain a sunflower protein product having a protein content of at least about 60, at least about 65, at least about 70, at least about 75, at least about 80, at least about 85 or at least about 90 wt % (N×6.25) on a dry weight basis.

5. The process of claim 4, wherein the pH of the optionally diluted washed acid insoluble material is raised to a value selected from the group consisting of less than about 8.0, about 6.0 to about 8.0 and about 6.5 to about 7.5, prior to the optional drying step.

6. The process of claim 4 wherein the wash solution is combined with the acidified sunflower protein solution of step (d) and processed as in at least one of steps (e)-(g).

7. The process of claim 2, wherein said acid insoluble solid material is simultaneously washed and adjusted in pH by mixing the acid insoluble solid material with a quantity of water selected from the group consisting of about 1 to about 20 volumes of water and about 1 to about 10 volumes of water, and sufficient food grade alkali to raise the pH to a value selected from the group consisting of less than about 8.0 and between about 5.0 and about 8.0, then is separated from the wash solution by centrifugation, prior to optional dilution then optional drying steps.

8. The process of claim 7, wherein the optionally diluted simultaneously washed and pH adjusted acid insoluble solid material is further raised in pH as to a value selected from the group of less than about 8.0, between about 6.0 and about 8.0 and between about 6.5 and about 7.5, prior to the optional drying step.

9. The process of claim 1, wherein following step b) said separated residual sunflower protein source is re-extracted to recover residual protein.

10. The process of claim 2, wherein said optionally diluted acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

11. The process of claim 3 wherein said optionally diluted and pH adjusted acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

12. The process of claim 4 wherein said optionally diluted washed acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

13. The process of claim 5 wherein said optionally diluted washed and pH adjusted acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

14. The process of claim 7 wherein said optionally diluted simultaneously washed and pH adjusted acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

15. The process of claim 8 wherein said optionally diluted simultaneously washed and pH adjusted and further pH adjusted acid insoluble solid material is pasteurized prior to drying, optionally at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

16. The process of claim 1, wherein the extraction step a) comprises a counter-current extract procedure.

17. The process of claim 1 wherein said extraction step (a) is effected at a temperature selected from the group consisting of about 1° to about 100° C., about 15° to about 65° C., and about 50° to about 60° C.

18. The process of claim 1 wherein said water used for the extraction contains a pH adjusting agent so that the extraction is conducted at a pH selected from the group consisting of about 6 to 11 and about 7 to about 8.5.

19. The process of claim 18 wherein the pH adjusting agent is selected from sodium hydroxide, potassium hydroxide and combinations thereof.

20. The process of claim 1 wherein said aqueous sunflower protein solution has a protein concentration selected from the group consisting of about 5 to about 50 g/L and about 10 to about 50 g/L.

21. The process of claim 1 wherein said water for extraction contains an antioxidant.

22. The process of claim 1 wherein said aqueous sunflower protein solution, after the separation step (b) and prior to the acidification step (c) is adjusted in temperature to a value selected from the group consisting of about 1 to about 35° C. and about 15 to about 35° C.

23. The process of claim 1 wherein the pH of said aqueous sunflower protein solution is adjusted in step (c) to value selected from the group consisting of about 2.0 to about 2.5.

24. The process of claim 1 wherein said acidified aqueous sunflower protein solution is dried to provide a sunflower protein product having a protein content of at least about 60 or at least about 65 wt % (N×6.25) d.b.

25. The process of claim 1 wherein said acidified aqueous sunflower protein solution is subjected to concentrating step (e) to produce a concentrated acidified sunflower protein solution having a protein concentration selected from the group consisting of about 50 to about 300 g/L, about 100 to about 200 g/L and about 50 to about 200 g/L.

26. The process of claim 25 wherein said concentration step (e) is effected by ultrafiltration using a membrane having a molecular weight cut-off selected from the group consisting of about 1,000 to about 1,000,000 daltons and about 1,000 to about 100,000 daltons.

27. The process of claim 1 wherein the acidified sunflower protein solution, partially concentrated acidified sunflower protein solution or concentrated acidified sunflower protein solution is subjected to diafiltering step (f).

28. The process of claim 27 wherein said diafiltration step (f) is effected using a diafiltration solution of water or acidified water, optionally using volumes of diafiltration solution selected from the group consisting of about 1 to about 40 volumes, and about 2 to about 25 volumes.

29. The process of claim 27 wherein said diafiltration step (f) is effected until no significant further quantities of contaminants or visible colour are present in the permeate.

30. The process of claim 27 wherein said diafiltration step (f) is effected until the retentate has been sufficiently purified so as to provide a sunflower protein isolate with a protein content of at least about 90 wt % (N×6.25) d.b.

31. The process of claim 27 wherein said diafiltration step (f) is effected using a membrane having a molecular weight cut-off selected from the group consisting of about 1,000 to about 1,000,000 daltons and about 1,000 to about 100,000 daltons.

32. The process of claim 27 wherein an antioxidant is present in the diafiltration medium during at least part of the diafiltration step (f).

33. The process of claim 25 wherein said concentration step (e) is carried out at a temperature selected from the group consisting of about 2° to about 65° C. and about 50° to about 60° C.

34. The process of claim 27 wherein said diafiltration step (f) is carried out at a temperature selected from the group consisting of about 2° to about 65° C. and about 50° to about 60° C.

35. The process of claim 1 wherein step e) and/or step f) are carried out and said concentrated and/or diafiltered acidified protein solution is pasteurized prior to drying.

36. The process of claim 35 wherein said pasteurization step is effected at a temperature and for a time selected from the group consisting of about 55° to about 85° C. for about 10 seconds to about 60 minutes, about 60° to about 70° C. for about 10 minutes to about 60 minutes and about 70° C. to about 85° C. for about 10 seconds to about 60 seconds.

37. The process of claim 27 wherein said concentrated and diafiltered acidified sunflower protein solution is subjected to drying step (g) to provide a sunflower protein isolate having a protein content of at least about 90 wt % (N×6.25) d.b.

38. The process of claim 1 wherein the pH of the optionally concentrated and optionally diafiltered acidified sunflower protein solution is raised to a value selected from the group consisting of less than about 8.0, about 6.0 to about 8.0 and about 6.5 to about 7.5, to produce a pH adjusted sunflower protein solution, prior to drying step (g).

39. The process of claim 1, wherein the sunflower protein source is in partially or fully defatted form.

40. A sunflower protein product having a protein content of at least about 60, at least about 65, at least about 70, at least about 75, at least about 80, at least about 85 or at least about 90 wt % (N×6.25) d.b. and which: is prepared without a process step involving the direct addition of salt; and wherein the sunflower protein product has a substantially clean flavour, which comprises little or no beany, green or vegetable flavour or off flavour.

41. The sunflower protein product of claim 58 which is derived from a partially or fully defatted sunflower protein source.

42. A food product formulated to contain the sunflower protein product of claim 40.

43. The food product of claim 42, which is a beverage.

Description

EXAMPLES

Example 1

[0108] This Example illustrates the preparation of canola protein products of the present invention.

[0109] 60 kg of defatted canola meal was added to 600 L of reverse osmosis purified (RO) water along with sufficient NaOH solution to adjust the pH to a target of 7. The mixture was agitated at ambient temperature for 30 minutes to provide an aqueous protein solution. The pH was monitored and maintained at about 7 throughout the extraction time. The bulk of the suspended solids were removed by centrifugation using a decanter centrifuge to provide a protein solution having a protein content of 1.37 wt %. The pH of the partially clarified protein solution was then lowered to about 2.0 by the addition of HCl solution (HCl diluted with an equal volume of water) and the solution centrifuged using a disc stack centrifuge to provide 411 L of acidified protein solution having pH 2.00 and an unrecorded amount of acid insoluble solid material.

[0110] 410 L of acidified protein solution, having a protein content of 0.59 wt %, was reduced in volume to 50 L by concentration on a polyethersulfone membrane having a molecular weight cutoff of 10,000 daltons, operated at a temperature of about 31° C. The resulting protein solution, with a protein content of 3.48 wt %, was diafiltered on the same membrane with 250 L of RO water at about pH 2, with the diafiltration operation conducted at about 31° C. The diafiltered protein solution, having a protein content of 3.12 wt % was then further concentrated to a protein content of 5.46 wt %. 30.18 kg of diafiltered and concentrated protein solution was obtained and represented a yield of 24.9% of the protein in the post-decanter extract solution. The diafiltered and concentrated protein solution was pasteurized at about 67° C. for 60 seconds. 16.76 kg of pasteurized, diafiltered and concentrated solution, having a pH of 2.17 was spray dried to yield a product found to have a protein content of 80.25% (N×6.25) d.b. The product was termed SD092-D23-15A C810A. 16.20 kg of pasteurized, diafiltered and concentrated protein solution was adjusted to pH 7.45 using NaOH/KOH solution (2.5 kg of 50% w/w NaOH solution mixed with 1.25 kg of KOH flakes and 6.25 kg of water). The pH adjusted, diafiltered and concentrated solution was spray dried to yield a product found to have a protein content of 77.62% (N×6.25) d.b. The product was termed SD092-D23-15A C810N.

[0111] The acid insoluble solid material collected had a protein content of 5.11 wt %. A sample of acid insoluble solid material was freeze dried to yield a product found to have a protein content of 75.42% (N×6.25) d.b. The product was termed SD092-D23-15A C810PA.

Example 2

[0112] This Example illustrates the preparation of hemp protein products of the present invention.

[0113] 20 kg of hemp protein powder (51.96% protein as-is) (Hemp Oil Canada, Ste. Agathe, MB) was combined with 200 L of RO water and sufficient NaOH solution to adjust the pH to 8.59 and the mixture agitated for 30 minutes at about 60° C. to provide an aqueous protein solution. The pH was monitored and maintained at about 8.5 throughout the extraction time. The bulk of the suspended solids were removed by centrifugation using a decanter centrifuge to provide a protein solution having a protein content of 2.34 wt %. The partially clarified protein solution was then subjected to a fat removal step by passing the solution through a cream separator. 160 L of the post-separator protein solution was then lowered in pH to 2.09 by the addition of HCl solution (HCl diluted with an equal volume of water) and the solution centrifuged using a disc stack centrifuge to provide 142 L of acidified protein solution having pH 1.99 as well as 19.88 kg of acid insoluble solid material.

[0114] 132 L of acidified protein solution was reduced in volume to 42 L using a microfiltration system containing ceramic membranes having a pore size of 0.8 μm and operated at a temperature of about 46° C. The sample was then further reduced in volume to 17 L and concurrently diafiltered with 25 L of pH 2 RO water at about 52° C. The microfiltration retentate was then diafiltered with an additional 50 L of pH 2 RO water at about 49° C. The diafiltered retentate had a weight of 16.32 kg and a protein content of 2.05 wt %.

[0115] The microfiltration and diafiltration permeates were combined to form a membrane feed solution having a protein content of 1.03 wt % and a pH of 2.04. 190 L of this membrane feed solution was reduced in volume to 33 L using an ultrafiltration system containing a PES membrane having a pore size of 10,000 daltons and operated at a temperature of about 46° C. The protein solution was then diafiltered with 9 volume of pH 2 RO water at about 51° C. followed by one volume of RO water at the natural pH at about 52° C. The diafiltered protein solution was then further concentrated to provide 26.52 kg of protein solution having a protein content of 4.79% and representing a yield of 38.4% of the protein in the post-separator protein solution. The diafiltered and further concentrated protein solution was pasteurized at 72° C. for several minutes. 13.26 kg of the pasteurized protein solution was spray dried to yield a product found to have a protein content of 101.56 wt % (N×6.25) d.b. The product was termed H002-L03-15A H810A. 13.26 kg of the pasteurized protein solution was adjusted to pH 7.15 using a NaOH solution. The pH adjusted solution was diluted with 3.52 L of RO water then spray dried to yield a product found to have a protein content of 98.32 wt % (N×6.25) d.b. The product was termed H002-L03-15A H810N.

[0116] The 19.88 kg of acid insoluble solid material was mixed with 40 L of RO water at pH 2 and then the sample centrifuged using a disc stack centrifuge to provide 48 L of acidified wash solution having pH 1.85 as well as 9.34 kg of washed acid insoluble solid material. The acidified wash solution was sampled for analysis and then discarded. 9.34 kg of the washed acid insoluble solid material was pasteurized at 72° C. for several minutes and then the pH adjusted to 7.02 with NaOH solution. This material represented a yield of 10.0% of the protein in the post-separator protein solution. The pH adjusted sample was spray dried to yield a product found to have a protein content of 77.44 wt % (N×6.25) d.b. The product was termed H002-L03-15A H810PN.

[0117] The protein content of the hemp products prepared in this Example were found to be higher than the protein content of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB), which was found to have a protein content of 64.98% (N×6.25) d.b.

Example 3

[0118] 120 g of sunflower meal (33.06% protein as-is) (ADM, Decatur, Ill.) was combined with 1200 ml of RO water and sufficient 6M NaOH solution to adjust the pH to a target of 7.1 and the mixture agitated for 30 minutes at about 60° C. minutes to provide an aqueous protein solution. The pH was monitored and maintained at about 7.1 throughout the extraction time. The bulk of the suspended solids were removed by centrifuging 1271.32 g of extraction slurry at 3,500 g for 3 minutes and then decanting the concentrate through a screen. 786.54 g of protein extract solution having a protein content of 1.27 wt % and a pH of 7.31 was collected and cooled to room temperature. 749.31 g of protein extract solution was adjusted in pH to 1.98 by the addition of 6.75 g of HCl solution (HCl diluted with an equal volume of water). 752.01 g of the acidified sample was centrifuged at 7,000 g for 3 minutes and then the concentrate decanted to provide 554.89 g of acidified protein solution that was cleanly decanted. Another 169.29 g of acidified protein solution was discarded because it contained a significant amount of acid insoluble solid material (SF810P) that decanted with the concentrate.

[0119] 16.62 g of acid insoluble solid material was collected from the bottom of the centrifuge tube and mixed with 30 ml of RO water. The pH of the sample was then adjusted in pH from 2.29 to 6.92 with 6M NaOH and freeze dried to provide 1.38 g of a product having a protein content of 64.04 wt % on an as-is basis. This product was termed SF810PN.

[0120] 510.13 g of acidified protein solution, having a protein content of 0.76 wt %, was reduced in volume to about 44 ml using Vivaflow 200 polyethersulfone membranes having a molecular weight cutoff of 10,000 Da. The ultrafiltration retentate was combined with 220 ml of RO water for diafiltration and the pH of the mixture lowered from 2.59 to 2.01 with HCl solution. The sample was then run on the Vivaflow membranes until 222 ml of permeate was collected. The volume of diafiltered, concentrated protein solution was about 44 ml. This sample had a protein content of 5.92 wt % and represented a yield of about 26.0% of the protein in the protein extract solution. 18.33 g of diafiltered and concentrated protein solution was freeze dried as is to provide 1.29 g of product having a protein content of 79.47 wt % on an as-is basis. This product was termed SF810A. A second aliquot of diafiltered and concentrated protein solution was adjusted in pH to 6.94 with NaOH solution and freeze dried to provide 1.34 g of product having a protein content of 77.70 wt % on an as-is basis. This product was termed SF810N.

Example 4

[0121] This Example contains an evaluation of the dry colour of the hemp protein products prepared according to Example 2 compared to that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB). Dry colour was assessed using a HunterLab ColorQuest XE operated in reflectance mode. The results are shown in the following Table 1.

TABLE-US-00001 TABLE 1 Dry colour of protein products Product L* a* b* H002-L03-15A H810A 76.24 0.87 19.33 H002-L03-15A H810N 73.64 1.08 19.48 H002-L03-15A H810PN 62.14 1.44 20.19 Hemp Pro 70 58.15 2.43 26.89

[0122] As may be seen from the results in Table 1, the hemp protein products of the present invention were lighter, less red and less yellow than the commercial hemp protein product evaluated.

Example 5

[0123] This Example contains an evaluation of the phytic acid content of the hemp protein products prepared according to the present invention as described in Example 2 and the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB). Phytic acid content was determined using the method of Latta and Eskin (J. Agric. Food Chem., 28: 1313-1315).

[0124] The results obtained are set forth in the following Table 2.

TABLE-US-00002 TABLE 2 Phytic acid content of hemp products % phytic acid H002-L03-15A H810A 0.56 H002-L03-15A H810N 0.54 H002-L03-15A H810PN 2.90 Hemp Pro 70 1.95

[0125] As may be seen from the results in Table 2, the H002-L03-15A H810A and H810N were lower in phytic acid than the commercial hemp protein product.

Example 6

[0126] This Example contains an evaluation of the acid hydrolysable carbohydrate content of the hemp protein products prepared according to the present invention as described in Example 2 and the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB). The acid hydrolysable carbohydrate content was determined according to the method of Dubois et al. (Anal. Chem., 28: 350-356). The results are shown in the following Table 3.

TABLE-US-00003 TABLE 3 Acid hydrolysable carbohydrate content of samples sample % acid hydrolysable carbohydrates d.b. H002-L03-15A H810A 2.48 H002-L03-15A H810N 2.70 H002-L03-15A H810PN 8.07 Hemp Pro 70 11.46

[0127] As may be seen from the results presented in Table 3, the hemp protein products of the present invention, particularly the H810A and H810N, were lower in acid hydrolysable carbohydrate than the commercial hemp protein product.

Example 7

[0128] This Example illustrates a comparison of the flavour of H002-L03-15A H810N, prepared as described in Example 2 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0129] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 3 g of protein in 150 ml purified drinking water. The pH of the solution of H810N was determined to be 6.00 while the pH of the solution of Hemp Pro 70 was 7.48. Food grade NaOH was added to the solution of H810N to raise the pH to 7.48. An informal panel of ten panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0130] Nine out of ten panelists indicated that the flavour of the H810N was cleaner. One panelist indicated that the flavour of the Hemp Pro 70 was cleaner.

Example 8

[0131] This Example illustrates a comparison of the flavour of H002-L03-15A H810PN, prepared as described in Example 2 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0132] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2 g of protein in 100 ml purified drinking water. The pH of the solution of H810PN was determined to be 7.13 while the pH of the solution of Hemp Pro 70 was 7.51. Food grade NaOH was added to the solution of H810PN to raise the pH to 7.51. An informal panel of seven panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0133] Four out of seven panelists indicated that the flavour of the H810N was cleaner. Three panelists indicated that the flavour of the Hemp Pro 70 was cleaner.

Example 9

[0134] This Example illustrates the protein solubility of the hemp protein products prepared according to the present invention as described in Examples 2. Protein solubility was tested by a modified version of the procedure of Mon et al., J. Food Sci., 50: 1715-1718.

[0135] Sufficient protein powder to supply 0.5 g of protein was weighed into a beaker and then a small amount of reverse osmosis (RO) purified water was added and the mixture stirred until a smooth paste formed. Additional water was then added to bring the volume to approximately 45 ml. The contents of the beaker were then slowly stirred for 60 minutes using a magnetic stirrer. The pH was determined immediately after dispersing the protein and was adjusted to the appropriate level (2, 3, 4, 5, 6 or 7) with diluted NaOH or HCl. The pH was measured and corrected periodically during the 60 minutes stirring. After the 60 minutes of stirring, the samples were made up to 50 ml total volume with RO water, yielding a 1% w/v protein dispersion. The protein content of the dispersions was measured by combustion analysis using a Leco Nitrogen Determinator. Aliquots of the dispersions were then centrifuged at 7,800 g for 10 minutes, which sedimented insoluble material and yielded a supernatant. The protein content of the supernatant was measured by Leco analysis and the solubility of the product calculated as follows:

Protein solubility (%)=(% protein in supernatant/% protein in initial dispersion)×100

Values calculated as greater than 100% were reported as 100%.

[0136] The protein solubility of the products at different pH values is shown in Table 4.

TABLE-US-00004 TABLE 4 Protein solubility of hemp protein products at different pH values Solubility (%) sample pH 2 pH 3 pH 4 pH 5 pH 6 pH 7 H002-L03-15A H810A 100 99.0 100 15.4 15.3 12.8 H002-L03-15A H810N 52.0 36.7 24.0 17.4 12.8 13.5

[0137] As may be seen from the results presented in Table 4, the H810A product was highly soluble in the pH range 2-4.

Example 10

[0138] This Example further illustrates preparation of hemp protein products according to the present invention.

[0139] ‘a’ kg of ‘b’ was combined with ‘c’ L of RO water and sufficient 12.5% NaOH/12.5% KOH solution to adjust the pH to a target of ‘d’ and the mixture agitated for 30 minutes at about 60° C. to provide an aqueous protein solution. The pH was monitored and maintained at about ‘d’ throughout the extraction time. The bulk of the suspended solids were removed by centrifugation using a decanter centrifuge to provide a protein solution having a protein content of ‘e’ wt %. The protein solution was then lowered in pH to a target of 2 by the addition of HCl solution (HCl diluted with an equal volume of water) and the solution centrifuged using a disc stack centrifuge to provide ‘f’ L of acidified protein solution having pH of ‘g’ and a protein content of ‘h’ wt % as well as T kg of acid insoluble solid material having a protein content of ‘j’ wt %. The acidified protein solution was ‘k’.

[0140] ‘l’ L of ‘m’ acidified protein solution having a protein content of ‘n’ wt % was reduced in volume to ‘o’ L using an ultrafiltration system containing a PES membrane having a pore size of 10,000 daltons and operated at a temperature of about ‘p’ ° C. The protein solution, having a protein content of ‘q’ wt % was then diafiltered with ‘r’ L of RO water adjusted to pH 2 at about ‘s’ ° C., followed by T L of RO water at the natural pH at about ‘u’ ° C. The diafiltered protein solution had a protein content of ‘v’ wt %. This solution was further concentrated to ‘w’ wt % protein then pasteurized at ‘x’ ° C. for ‘y’ seconds. ‘z’ kg of the pasteurized protein solution was spray dried to yield a product found to have a protein content of ‘aa’ wt % (N×6.25) d.b. The product was termed ‘ab’ H810A. ‘ac’ kg of the pasteurized protein solution was adjusted to pH ‘ad’ using a 12.5% NaOH/12.5% KOH solution. The pH adjusted solution was spray dried to yield a product found to have a protein content of ‘ae’ wt % (N×6.25) d.b. The product was termed ‘ab’ H810N.

[0141] ‘af’ kg of acid insoluble material was combined with ‘ag’ L of RO water and the pH adjusted to ‘ah’ with 12.5% NaOH/12.5% KOH solution. The sample was then centrifuged again to provide ‘ai’ kg of washed acid insoluble solids having a protein content of ‘aj’. These solids were pasteurized at ‘ak’ ° C. for ‘al’ and then spray dried to yield a product found to have a protein content of ‘am’ wt % (N×6.25) d.b. The product was termed ‘ab’ H810PA.

[0142] The parameters ‘a’ to ‘am’ are set forth in the following Table 5.

TABLE-US-00005 TABLE 5 Parameters for the runs to produce hemp protein products aa H003-I15- H003-I27- H005-K01- H003-L05- 16A 16A 16A 16A a 24 30 29 60 b hull material hull material “seed meats” hull material from the from the (unders) obtained from the dehulling of dehulling of by sieving hull dehulling of hemp seeds, hemp seeds, material from the hemp seeds, defatted by defatted by dehulling of hemp defatted by pressing then pressing then seeds, defatted by pressing then ground ground pressing then ground ground c 240 300 290 600 d 8.5 10.5 8.5 8.5 e 0.66 1.20 2.05 0.96 f 220 225 212 508 g 1.80 1.96 2.12 2.00 h 0.58 1.20 1.83 0.88 i 23.86 50.70 52.2 73.74 j 0.93 1.43 not recorded 1.21 k further clarified further clarified N/A further clarified by successive by successive by successive filtration filtration filtration through filter through filter through filter pads having pads having pads having pore sizes of pore sizes of pore sizes of 2.0 μm and 2.0 μm and 2.0 μm and 0.8 μm 0.2 μm 0.2 μm l 245 250 212 462 m filtered filtered N/A filtered n 0.49 0.90 1.83 0.58 o 25 31 65 46 p 48 46 51 45 q 3.06 5.52 5.10 5.59 r 225 279 585 414 s 52 50 52 50 t 215 31 94 141 u 52 50 52 51 v 3.70 5.27 5.70 3.30 w N/A 6.92 10.26 5.64 x 72 74 76 about 72 y not recorded, 16 16 16 about 30 to 60 z 11.80 14.05 N/A N/A aa 98.95 99.45 N/A N/A ac 11.34 14.69 32.66 39.62 ad 7.45 6.95 6.80 7.06 ae 95.75 95.58 75.20 95.61 af N/A 50.70 52.20 73.74 ag N/A 202 210 295 ah N/A about 5.5 about 5.5 5.63 ai N/A 18.98 23.18 28.56 aj N/A 3.74 4.52 1.97 ak N/A 74 74 about 72 al N/A 16 16 16 am N/A 79.30 78.14 68.86

Example 11

[0143] This Example further illustrates preparation of hemp protein products according to the present invention.

[0144] 30 kg of hull material from the dehulling of hemp seeds, defatted by pressing then ground was combined with 300 L of RO water and sufficient 12.5% NaOH/12.5% KOH solution to adjust the pH to a target of 8.5 and the mixture agitated for 30 minutes at about 60° C. to provide an aqueous protein solution. The pH was monitored and maintained at about 8.5 throughout the extraction time. The bulk of the suspended solids were removed by centrifugation using a decanter centrifuge to provide a protein solution having a protein content of 0.95 wt %. The protein solution was then lowered in pH to a target of 2 by the addition of HCl solution (HCl diluted with an equal volume of water). 42.62 kg of wet solids from the initial separation step were combined with 300 L of RO water and mixed for 30 minutes at 60° C. The pH of the suspension was 8.79 so no further pH adjustment was conducted. Again the suspended solids were removed by centrifugation using a decanter centrifuge to provide a protein solution having a protein content of 0.16 wt %. The pH of this solution was lowered to about 2 and the two acidified protein solutions were combined and centrifuged using a disc stack centrifuge to provide 598 L of acidified protein solution having pH of 1.92 and a protein content of 0.48 wt % as well as an unrecorded amount of acid insoluble solid material having a protein content of 0.80 wt %.

[0145] The acidified protein solution was further clarified by successive filtration through filter pads having pore sizes of 2.0 μm and 0.2 μm.

[0146] 585 L of filtered acidified protein solution having a protein content of 0.33 wt % was reduced in volume to 40 L using an ultrafiltration system containing a PES membrane having a pore size of 10,000 daltons and operated at a temperature of about 45° C. The protein solution, having a protein content of 4.90 wt % was then diafiltered with 360 L of RO water adjusted to about pH 2 at about 51° C., followed by an unrecorded amount of RO water at the natural pH at about 50° C. The diafiltered protein solution had a protein content of 4.30 wt %. This solution was further concentrated to 4.43 wt % protein then pasteurized at 75° C. for 16 seconds. 30.36 kg of the pasteurized protein solution was adjusted to pH 6.74 using a 12.5% NaOH/12.5% KOH solution. The pH adjusted solution was spray dried to yield a product found to have a protein content of 93.48% (N×6.25) d.b. The product was termed H003-K24-16A H810N.

Example 12

[0147] This Example contains an evaluation of the dry colour of the hemp protein products prepared according to Examples 10 and 11. Dry colour was assessed using a HunterLab ColorQuest XE operated in reflectance mode. The results are shown in the following Table 6.

TABLE-US-00006 TABLE 6 Dry colour of protein products Product L* a* b* H003-I15-16A H810A 75.29 1.20 18.23 H003-I27-16A H810A 66.77 5.44 20.26 H003-I15-16A H810N 70.78 1.59 19.69 H003-I27-16A H810N 61.34 6.17 18.94 H005-K01-16A H810N 67.03 0.22 27.13 H003-K24-16A H810N 67.49 1.75 19.82 H003-L05-16A H810N 71.21 0.61 17.01 H003-I27-16A H810PA 52.12 3.57 14.48 H005-K01-16A H810PA 67.33 0.44 21.05 H003-L05-16A H810PA 65.62 1.19 19.53

[0148] As may be seen from the results in Table 6, with the exception of the H810PA from the pH 10.5 extraction run, the hemp protein products of the present invention were lighter than the commercial hemp protein product evaluated (see Table 1).

Example 13

[0149] This Example contains an evaluation of the phytic acid content of the hemp protein products prepared according to the present invention as described in Examples 10 and 11. Phytic acid content was determined using the method of Latta and Eskin (J. Agric. Food Chem., 28: 1313-1315).

[0150] The results obtained are set forth in the following Table 7.

TABLE-US-00007 TABLE 7 Phytic acid content of hemp products sample % phytic acid H003-I15-16A H810A 0.00 H003-I27-16A H810A 0.08 H003-I15-16A H810N 0.12 H003-I27-16A H810N 0.09 H005-K01-16A H810N 1.05 H003-K24-16A H810N 0.02 H003-L05-16A H810N 0.05 H003-I27-16A H810PA 0.40 H005-K01-16A H810PA 0.75 H003-L05-16A H810PA 0.85

[0151] As may be seen from the results in Table 7, the hemp protein products were all generally low in phytic acid and were lower in phytic acid than the commercial hemp protein product (see Table 2).

Example 14

[0152] This Example contains an evaluation of the acid hydrolysable carbohydrate content of the hemp protein products prepared according to the present invention as described in Examples 10 and 11. The acid hydrolysable carbohydrate content was determined according to the method of Dubois et al. (Anal. Chem., 28: 350-356). The results are shown in the following Table 8.

TABLE-US-00008 TABLE 8 Acid hydrolysable carbohydrate content of samples sample % acid hydrolysable carbohydrates d.b. H003-I15-16A H810A 3.26 H003-I27-16A H810A 3.61 H003-I15-16A H810N 3.44 H003-I27-16A H810N 3.40 H003-K24-16A H810N 2.75 H003-L05-16A H810N 3.70 H003-I27-16A H810PA 5.64 H003-L05-16A H810PA 6.76

[0153] As may be seen from the results presented in Table 8, the hemp protein products of the present invention, particularly the H810A and H810N, were lower in acid hydrolysable carbohydrate than the commercial hemp protein product (see Table 3).

Example 15

[0154] This Example illustrates the protein solubility of the hemp protein products prepared according to the present invention as described in Examples 2, 10 and 11 and the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB). Protein solubility was tested by a modified version of the procedure of Mon et al., J. Food Sci., 50: 1715-1718.

[0155] Sufficient protein powder to supply 0.5 g of protein was weighed into a beaker and then a small amount of reverse osmosis (RO) purified water was added and the mixture stirred until a smooth paste formed. Additional water was then added to bring the volume to approximately 45 ml. The contents of the beaker were then slowly stirred for 60 minutes using a magnetic stirrer. The pH was determined immediately after dispersing the protein and was adjusted to the appropriate level (2, 3, 4, 5, 6 or 7) with diluted NaOH or HCl. The pH was measured and corrected periodically during the 60 minutes stirring. After the 60 minutes of stirring, the samples were made up to 50 ml total volume with RO water, yielding a 1% w/v protein dispersion. The protein content of the dispersions was measured by combustion analysis using a Leco Nitrogen Determinator. Aliquots of the dispersions were then centrifuged at 7,800 g for 10 minutes, which sedimented insoluble material and yielded a supernatant. The protein content of the supernatant was measured by Leco analysis and the solubility of the product calculated as follows:

Protein solubility (%)=(% protein in supernatant/% protein in initial dispersion)×100

Values calculated as greater than 100% were reported as 100%.

[0156] The protein solubility of the products at different pH values is shown in Table 9.

TABLE-US-00009 TABLE 9 Protein solubility of hemp protein products at different pH values Solubility (%) sample pH 2 pH 3 pH 4 pH 5 pH 6 pH 7 H003-I15-16A H810A 99.0 83.0 89.8 66 15.7 21.0 H003-I27-16A H810A 99.1 97.2 97.1 16.2 8.6 11.5 H003-I27-16A H810N 100 100 52.4 18.1 12.5 15.6 H005-K01-16A H810N 38.2 31.9 13.7 0.0 5.3 7.1 H003-L05-16A H810N 34.0 28.8 17.3 7.9 4.7 13.4 H005-K01-16A H810PA 14.4 0.0 5.8 0.0 1.0 0.9 H003-L05-16A H810PA 21.2 0.0 0.0 0.0 0.0 4.3 H002-L03-15A H810PN 10.0 9.3 5 1.9 6.8 13.9 Hemp Pro 70 52.5 53.1 16.8 15.1 13.4 21.9

[0157] As may be seen from the results in Table 9, the H810A had good protein solubility in the pH range 2 to 4. The protein solubility of the H810N was low in the pH range 5 to 7. The products derived from the acid insoluble solid material were generally low in protein solubility across the pH range tested.

Example 16

[0158] This Example illustrates the molecular weight profile of the hemp protein products prepared according to aspects of the present invention as described in Examples 2, 10 and 11 as well as hemp protein product prepared as described in U.S. patent application Ser. No. 13/956,619 (US Patent Publication No. 2014/0037824 published Feb. 6, 2014) and the commercial hemp protein product Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0159] Molecular weight profiles were determined by size exclusion chromatography using a Varian ProStar HPLC system equipped with a 300×7.8 mm Phenomenex Yarra SEC-2000 series column. The column contained hydrophilic bonded silica rigid support media, 3 micron diameter, with 145 Angstrom pore size.

[0160] Before the pulse protein samples were analyzed, a standard curve was prepared using a Biorad protein standard (Biorad product #151-1901) containing proteins with known molecular weights between 17,000 Daltons (myoglobulin) and 670,000 Daltons (thyroglobulin) with Vitamin B12 added as a low molecular weight marker at 1,350 Daltons. A 0.9% w/v solution of the protein standard was prepared in water, filtered with a 0.45 μm pore size filter disc then a 50 μL aliquot run on the column using a mobile phase of 0.05M phosphate/0.15M NaCl, pH 6 containing 0.02% sodium azide. The mobile phase flow rate was 1 mL/min and components were detected based on absorbance at 280 nm. Based on the retention times of these molecules of known molecular weight, a regression formula was developed relating the log of the molecular weight to the retention time in minutes.

[0161] For the analysis of the pulse protein samples, 0.05M phosphate/0.15M NaCl, pH 6 containing 0.02% sodium azide was used as the mobile phase and also to dissolve dry samples. Protein samples were mixed with mobile phase solution to a concentration of 1% w/v, placed on a shaker for at least 1 hour then filtered using 0.45 μm pore size filter discs. Sample injection size was 50 μL. The mobile phase flow rate was 1 mL/minute and components were detected based on absorbance at 280 nm.

[0162] The regression formula relating molecular weight and retention time was used to calculate retention times that corresponded to molecular weights of 100,000 Da, 15,000 Da, 5,000 Da and 1,000 Da. The HPLC ProStar system was used to calculate the peak areas lying within these retention time ranges and the percentage of protein ((range peak area/total protein peak area)×100) falling in a given molecular weight range was calculated. Note that the data was not corrected by protein response factor.

[0163] The molecular weight profiles of the hemp protein products are shown in Table 10.

TABLE-US-00010 TABLE 10 HPLC protein profile of various products % % % % > 15,000- 5,000- 1,000- 100,000 100,000 15,000 5,000 product Da Da Da Da H002-L03-15A H810A 1.3 19.0 48.9 30.8 H003-I15-16A H810A 3.6 23.1 46.3 27.0 H003-I27-16A H810A 2.6 21.7 46.6 29.1 H002-L03-15A H810N 1.3 21.3 43.6 33.7 H003-I15-16A H810N 3.3 28.3 45.0 23.4 H003-I27-16A H810N 2.3 29.1 43.7 24.9 H005-K01-16A H810N 0.5 22.4 44.0 33.1 H003-K24-16A H810N 2.5 24.8 43.1 29.7 H003-L05-16A H810N 4.3 25.5 45.0 25.2 H003-I27-16A H810PA 11.6 61.2 13.4 13.8 H005-K01-16A H810PA 2.3 52.3 30.2 15.2 H003-L05-16A H810PA 0.0 34.0 40.9 25.0 H002-L03-15A H810PN 0.5 38.2 40.8 20.4 H001-H24-11A H701 0.3 15.6 63.6 20.5 Hemp Pro 70 1.7 12.8 15.8 69.7

[0164] As may be seen from the results of Table 10, the protein profiles of the products of the present invention differed from the profiles of the H701 and the commercial hemp protein concentrate.

Example 17

[0165] This Example illustrates a comparison of the flavour of H003-I15-16A H810N, prepared as described in Example 10 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0166] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810N was determined to be 6.86 while the pH of the solution of Hemp Pro 70 was 7.71. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 6.85. An informal panel of eight panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0167] Eight out of eight panelists indicated that the flavour of the H810N was cleaner.

Example 18

[0168] This Example illustrates a comparison of the flavour of H005-K01-16A H810N, prepared as described in Example 10 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0169] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810N was determined to be 6.71 while the pH of the solution of Hemp Pro 70 was 7.74. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 6.67. An informal panel of nine panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0170] Seven out of nine panelists indicated that the flavour of the H810N was cleaner. One panelist indicated that the flavour of the Hemp Pro 70 was cleaner, while one panelist could not identify one sample as having a cleaner flavour.

Example 19

[0171] This Example illustrates a comparison of the flavour of H003-K24-16A H810N, prepared as described in Example 11 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0172] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810N was determined to be 6.71 while the pH of the solution of Hemp Pro 70 was 7.74. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 6.67. An informal panel of eight panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0173] Six out of eight panelists indicated that the flavour of the H810N was cleaner. Two panelists could not identify one sample as having a cleaner flavour.

Example 20

[0174] This Example illustrates a comparison of the flavour of H002-L03-15A H810A, prepared as described in Example 2 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0175] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810A was determined to be 3.01 while the pH of the solution of Hemp Pro 70 was 7.89. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 3.06. An informal panel of nine panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0176] Eight out of nine panelists indicated that the flavour of the H810A was cleaner. One panelist could not identify one sample as having cleaner flavour.

Example 21

[0177] This Example illustrates a comparison of the flavour of H003-I15-16A H810A, prepared as described in Example 10 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0178] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810A was determined to be 3.89 while the pH of the solution of Hemp Pro 70 was 7.68. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 3.89. An informal panel of nine panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0179] Eight out of nine panelists indicated that the flavour of the H810A was cleaner. One panelist could not identify one sample as having cleaner flavour.

Example 22

[0180] This Example illustrates a comparison of the flavour of H005-K01-16A H810PA, prepared as described in Example 10 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0181] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810PA was determined to be 6.14 while the pH of the solution of Hemp Pro 70 was 7.72. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 6.17. An informal panel of nine panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0182] Six out of nine panelists indicated that the flavour of the H810PA was cleaner. Two panelists indicated that the flavour of the Hemp Pro 70 was cleaner and one panelist could not identify one sample as having cleaner flavour.

Example 23

[0183] This Example illustrates a comparison of the flavour of H005-L05-16A H810PA, prepared as described in Example 10 with that of the commercial hemp protein concentrate Hemp Pro 70 (Manitoba Harvest Hemp Foods, Winnipeg, MB).

[0184] Samples were prepared for sensory evaluation by dissolving sufficient protein powder to supply 2.4 g of protein in 120 ml purified drinking water. The pH of the solution of H810PA was determined to be 5.88 while the pH of the solution of Hemp Pro 70 was 7.71. Food grade HCl was added to the solution of Hemp Pro 70 to lower the pH to 5.86. An informal panel of nine panelists was asked to blindly compare the samples and indicate which had a cleaner flavour.

[0185] Seven out of nine panelists indicated that the flavour of the H810PA was cleaner. Two panelists indicated that the flavour of the Hemp Pro 70 was cleaner.

SUMMARY OF THE DISCLOSURE

[0186] In summary of this disclosure, there are provided novel and inventive non-soy oilseed protein products of enhanced taste and novel and inventive methods of producing non-soy oilseed protein products of enhanced taste, which methods do not involve the direct addition and use of calcium salts or other salts for extraction of the non-soy oilseed protein from the non-soy oilseed protein source or in any other process step. Modifications are possible within the scope of this invention.