CA1317413C - Process for preparing protein concentrates from brewer's spent grain - Google Patents
Process for preparing protein concentrates from brewer's spent grainInfo
- Publication number
- CA1317413C CA1317413C CA000534712A CA534712A CA1317413C CA 1317413 C CA1317413 C CA 1317413C CA 000534712 A CA000534712 A CA 000534712A CA 534712 A CA534712 A CA 534712A CA 1317413 C CA1317413 C CA 1317413C
- Authority
- CA
- Canada
- Prior art keywords
- protein
- temperature
- extracted
- bsg
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/001—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste materials, e.g. kitchen waste
- A23J1/005—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste materials, e.g. kitchen waste from vegetable waste materials
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Peptides Or Proteins (AREA)
Abstract
ABSTRACT
A method of preparing protein concentrate from brewers' spent grain comprises extracting said brewer's spent grain with sodium dodecyl sulfate to solubilize the protein thereof, and thereafter removing a substantial proportion of the protein in solution.
A method of preparing protein concentrate from brewers' spent grain comprises extracting said brewer's spent grain with sodium dodecyl sulfate to solubilize the protein thereof, and thereafter removing a substantial proportion of the protein in solution.
Description
~ 3~7~ 3 The present invention relates to the field of processing of brewery waste into useful products.
The principal by-product of the brewing industry is brewer's spent grain (hereinafter referred to as BSG). The composition of BSG is approximately as follows:
Table A
Component% (dry weight basis) Moisture 7.41 Crude Protein 26.88 10 Crude Fat 8.07 Ash 4.71 Fiber 16.25 Nitrogen Free Extract 44.09 It will be seen, therefore, that protein is a major constituent of BSG, and potentially a rich source of food.
Several proposals have been made in the past for recovery of this protein. For instance, in The Molson Companies Limited's U.S. Patent No. 4,315,038, dated February 9, 1982, it is disclosed that protein can be extracted from trub by extraction with an azeotropic mixture of isopropanol and water. In an article by three of the present inventors (Crowe, Alli and Baker) in the Journal of the Institute of Brewing, Vol. 91, p.l48-150, titled Solubilization of Nitrogenous Constituents of Brewer's Spent Grains, it is disclosed that up to 50% of the Nitrogen from BSG
solubilized by an acid detergent (cetyl-trimethyl ammonium bromide in sulfuric acid - capable of solubilizing 90~ of BSG nitrogen) can be recovered as a solid.
~L317~13 The object of the present invention is to provide a fairly inexpensive but efficient method of preparing a protein concentrate from BSG.
In one broad aspect, the present invention relates to a method of preparing protein concentrate from brewer's spent grain comprising extracting said brewer's spent grain with sodium dodecyl sulfate to solubilize the protein thereof, and thereafter removing a substantial proportion of the protein in solution.
It has been discovered by the present invento~s that sodium dodecyl sulfate (SDS) can be used as an inexpensive extractant for BSG, with very good results. The extracted protein is precipitated by the addition of ethanol followed by refrigeration. It will be appreciated that other methods for the isolation of the protein from the extract, such as those involving, for instance, the use of a protein precipitant, ultrafiltration, or adjustment of pH, may be used.
The practice of the present invention will be apparent from the detailed comparative examples which follow, and which are set out in Table B, following.
~periment 1 Commercially dried BSG (5g) was mixed with extractant (lOOmL - 3% SDS - 0,5% Na2HP04; pH7,0). The mixture was heated ~3~7~13 under reflux for one hour. The residue was removed by filtration (California Buchner unnels). Analysis of the extract showed that 62% of the BSG nitrogen was solubilized). The extract was cooled to 4C and maintained at that temperature for 16 hours. The precipitates were recovered by centrifugation (9500g, 0C), washed with ethanol (95%; 20mL), centrifuged to remove the wash (12,500g;
0C) and lyophilized. Nitrogen analysis of the lyophilized product indicated that 5% of the BSG crude protein was recovered.
Experiment 2 BSG was extracted with SDS solution under the conditions used in Experiment 1. The reaction of the extract was adjusted to pH2.0 using dilute HCl. The protein was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 2%
of the BSG crude protein was recovered.
~periment 3 BSG was extracted with SDS solution under the conditions used in Experiment 1. The reaction of the extract was adjusted to pH 2.0 using dilute HCl and the resultant mixture was cooled to 4C and maintained at this temperature for 16 hours. The protein was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 3% of the BSG crude protein was recovered.
~3174~3 Experiment 4 BSG was extracted with SDS solution under the conditions used in Experiment 1. Ethanol was added to the extract (70mL;
95~). The resultant precipitate was recovered by centrifugation, washed and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 29% of the BSG
crude protein was recovered.
Experiment 5 BSG was extracted with SDS solution under the conditions used in Experiment 1. Ethanol was added to the extract (70mL;
95%) and the resultant mixture was cooled to 4C and maintained at this temperature for 16 hours. The resultant precipitate was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 44% of the BSG crude protein was recovered.
Experiment 6 BSG was extracted with the SDS solution as described in Experiment 1 except that the extraction was conducted at 27C and with agitation. Analysis of the extract showed that 29% of the BSG nitrogen was solubilized. The protein in the extract was recovered as described in Experiment 5. ~itrogen analysis of the lyophilized product indicated that 16% of the BSG crude protein was recovered.
t317~3 Experiment 7 Experiment 6 was repeated except that the extraction was performed at 45C. Nitrogen analysis indicated that 33% of the BSG nitrogen was extracted and that 18% of the BSG crude protein was recovered.
Experiment 8 Experiment 6 was repeated except that the extraction was performed at 60C. Nitrogen analysis indicated that 30% of the BSG nitrogen was extracted and that 17~ of the BSG crude protein was recovered.
Experiment 9 Experiment 6 was repeated except that the extraction was performed at 75C. Nitrogen analysis indicated that 35% of the BSG nitrogen was extracted and that 22% of the BSG crude protein was recovered.
Experiment 10 Experiment 6 was repeated except that the extraction was performed at 90C. Nitrogen analysis indicated that 51~ of the BSG nitrogen was extracted and that 28% of the BSG crude protein was recovered.
Experiment 11 The SDS extraction was conducted under the refluxing conditions described in Experiment 1. The extracts were stored at ~L31~
4C for 16 hours. The cold extracts were centrifuged ~9500g; 0C) to remove the precipitated material. The proteins in the supernatant were concentrated by ultrafiltration and the retentate was lyophilized. Nitrogen analysis of the lyophilized product indicated that 47% of the BSG crude protein was recovered.
The procedure described in Experiment 5 gave a protein recovery of 44%. The product which was isolated contained 9 nitrogen or 53% protein (%N x 5.83 See: Methods of Protein Analysis (1984) I. Kerese ed. p.59, published by Ellis Horwood Limited, Chichester, England). The proteinaceous material was brown in colour and granular in texture. It will be understood that the Applicant did not attempt to differentiate between nitrogen from protein and from other sources, such as nucleic acids. However, amino acid analysis of the protein concentrates clearly indicates that they are proteinaceous materials.
The procedure described in Experiment ll gave a protein recovery of 47%. The product which was isolated contained 6%
nitrogen or 35% protein (%N x 5.83). The proteinaceous material was beige in colour and floury in texture.
It is to be understood that the examples described above are not meant to limit the scope of the present invention.
It is expected that numerous variants will be obvious to the person skilled in the art, without any departure from the , ~3~L7~3 spirit of the present invention. The appended claims, properly construed, form the only limitation upon the scope of the present invention ~L 3 1 7 1 A . ~ ,1 . _. ___ ~ __ _ O ~ h h ,~ ,~ r` 0~ ~; t~l ~ 3~
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.
The principal by-product of the brewing industry is brewer's spent grain (hereinafter referred to as BSG). The composition of BSG is approximately as follows:
Table A
Component% (dry weight basis) Moisture 7.41 Crude Protein 26.88 10 Crude Fat 8.07 Ash 4.71 Fiber 16.25 Nitrogen Free Extract 44.09 It will be seen, therefore, that protein is a major constituent of BSG, and potentially a rich source of food.
Several proposals have been made in the past for recovery of this protein. For instance, in The Molson Companies Limited's U.S. Patent No. 4,315,038, dated February 9, 1982, it is disclosed that protein can be extracted from trub by extraction with an azeotropic mixture of isopropanol and water. In an article by three of the present inventors (Crowe, Alli and Baker) in the Journal of the Institute of Brewing, Vol. 91, p.l48-150, titled Solubilization of Nitrogenous Constituents of Brewer's Spent Grains, it is disclosed that up to 50% of the Nitrogen from BSG
solubilized by an acid detergent (cetyl-trimethyl ammonium bromide in sulfuric acid - capable of solubilizing 90~ of BSG nitrogen) can be recovered as a solid.
~L317~13 The object of the present invention is to provide a fairly inexpensive but efficient method of preparing a protein concentrate from BSG.
In one broad aspect, the present invention relates to a method of preparing protein concentrate from brewer's spent grain comprising extracting said brewer's spent grain with sodium dodecyl sulfate to solubilize the protein thereof, and thereafter removing a substantial proportion of the protein in solution.
It has been discovered by the present invento~s that sodium dodecyl sulfate (SDS) can be used as an inexpensive extractant for BSG, with very good results. The extracted protein is precipitated by the addition of ethanol followed by refrigeration. It will be appreciated that other methods for the isolation of the protein from the extract, such as those involving, for instance, the use of a protein precipitant, ultrafiltration, or adjustment of pH, may be used.
The practice of the present invention will be apparent from the detailed comparative examples which follow, and which are set out in Table B, following.
~periment 1 Commercially dried BSG (5g) was mixed with extractant (lOOmL - 3% SDS - 0,5% Na2HP04; pH7,0). The mixture was heated ~3~7~13 under reflux for one hour. The residue was removed by filtration (California Buchner unnels). Analysis of the extract showed that 62% of the BSG nitrogen was solubilized). The extract was cooled to 4C and maintained at that temperature for 16 hours. The precipitates were recovered by centrifugation (9500g, 0C), washed with ethanol (95%; 20mL), centrifuged to remove the wash (12,500g;
0C) and lyophilized. Nitrogen analysis of the lyophilized product indicated that 5% of the BSG crude protein was recovered.
Experiment 2 BSG was extracted with SDS solution under the conditions used in Experiment 1. The reaction of the extract was adjusted to pH2.0 using dilute HCl. The protein was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 2%
of the BSG crude protein was recovered.
~periment 3 BSG was extracted with SDS solution under the conditions used in Experiment 1. The reaction of the extract was adjusted to pH 2.0 using dilute HCl and the resultant mixture was cooled to 4C and maintained at this temperature for 16 hours. The protein was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 3% of the BSG crude protein was recovered.
~3174~3 Experiment 4 BSG was extracted with SDS solution under the conditions used in Experiment 1. Ethanol was added to the extract (70mL;
95~). The resultant precipitate was recovered by centrifugation, washed and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 29% of the BSG
crude protein was recovered.
Experiment 5 BSG was extracted with SDS solution under the conditions used in Experiment 1. Ethanol was added to the extract (70mL;
95%) and the resultant mixture was cooled to 4C and maintained at this temperature for 16 hours. The resultant precipitate was recovered by centrifugation, washed, and lyophilized as described in Experiment 1. Nitrogen analysis of the lyophilized product indicated that 44% of the BSG crude protein was recovered.
Experiment 6 BSG was extracted with the SDS solution as described in Experiment 1 except that the extraction was conducted at 27C and with agitation. Analysis of the extract showed that 29% of the BSG nitrogen was solubilized. The protein in the extract was recovered as described in Experiment 5. ~itrogen analysis of the lyophilized product indicated that 16% of the BSG crude protein was recovered.
t317~3 Experiment 7 Experiment 6 was repeated except that the extraction was performed at 45C. Nitrogen analysis indicated that 33% of the BSG nitrogen was extracted and that 18% of the BSG crude protein was recovered.
Experiment 8 Experiment 6 was repeated except that the extraction was performed at 60C. Nitrogen analysis indicated that 30% of the BSG nitrogen was extracted and that 17~ of the BSG crude protein was recovered.
Experiment 9 Experiment 6 was repeated except that the extraction was performed at 75C. Nitrogen analysis indicated that 35% of the BSG nitrogen was extracted and that 22% of the BSG crude protein was recovered.
Experiment 10 Experiment 6 was repeated except that the extraction was performed at 90C. Nitrogen analysis indicated that 51~ of the BSG nitrogen was extracted and that 28% of the BSG crude protein was recovered.
Experiment 11 The SDS extraction was conducted under the refluxing conditions described in Experiment 1. The extracts were stored at ~L31~
4C for 16 hours. The cold extracts were centrifuged ~9500g; 0C) to remove the precipitated material. The proteins in the supernatant were concentrated by ultrafiltration and the retentate was lyophilized. Nitrogen analysis of the lyophilized product indicated that 47% of the BSG crude protein was recovered.
The procedure described in Experiment 5 gave a protein recovery of 44%. The product which was isolated contained 9 nitrogen or 53% protein (%N x 5.83 See: Methods of Protein Analysis (1984) I. Kerese ed. p.59, published by Ellis Horwood Limited, Chichester, England). The proteinaceous material was brown in colour and granular in texture. It will be understood that the Applicant did not attempt to differentiate between nitrogen from protein and from other sources, such as nucleic acids. However, amino acid analysis of the protein concentrates clearly indicates that they are proteinaceous materials.
The procedure described in Experiment ll gave a protein recovery of 47%. The product which was isolated contained 6%
nitrogen or 35% protein (%N x 5.83). The proteinaceous material was beige in colour and floury in texture.
It is to be understood that the examples described above are not meant to limit the scope of the present invention.
It is expected that numerous variants will be obvious to the person skilled in the art, without any departure from the , ~3~L7~3 spirit of the present invention. The appended claims, properly construed, form the only limitation upon the scope of the present invention ~L 3 1 7 1 A . ~ ,1 . _. ___ ~ __ _ O ~ h h ,~ ,~ r` 0~ ~; t~l ~ 3~
l I
O .~
o o U~ ,~~`,1 0 ,~ a~ 1` ~ U~00 ~rl ~rl * . ~r ~ ~`I c3 0 1J
. O .c,l~
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.
Claims (11)
1. A method of preparing protein concentrate from brewer's spent grain comprising extracting said brewer's spent grain with sodium dodecyl sulfate to solubilize the protein thereof, and thereafter removing a substantial proportion of the protein in solution.
2. A method as claimed in Claim 1 wherein said protein is removed from solution by precipitation with ethanol.
3. A method as described in Claim 1, wherein said protein is extracted with sodium dodecyl sulfate at an elevated temperature, and removed from solution by precipitation with ethanol followed by refrigeration.
4. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 70° to 110°C and, after precipitation with ethanol, refrigerated to a temperature of from about 0°C to about 20°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
5. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 70° to 100°C and, after precipitation with ethanol, refrigerated to a temperature of from about 0°C to about 10°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
6. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 80° to 100°C and, after precipitation with ethanol, refrigerated to a temperature of from about 0°C to about 10°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
7. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 90° to 100°C and, after precipitation with ethanol, refrigerated to a temperature of from about 0°C to about 10°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
8. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 90° to 100°C and, after precipitation with ethanol, refrigerated to a temperature of from about 2°C to about 8°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
9. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at a temperature of from about 90° to 100°C and, after precipitation with ethanol, refrigerated to a temperature of from about 4°C to about 6°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
10. A method as described in Claim 3, wherein said protein is extracted with sodium dodecyl sulfate at about 100°C and, after precipitation with ethanol, refrigerated to about 4°C for a period of time sufficient to precipitate a substantial proportion of said protein from solution.
11
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000534712A CA1317413C (en) | 1987-04-14 | 1987-04-14 | Process for preparing protein concentrates from brewer's spent grain |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000534712A CA1317413C (en) | 1987-04-14 | 1987-04-14 | Process for preparing protein concentrates from brewer's spent grain |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1317413C true CA1317413C (en) | 1993-05-04 |
Family
ID=4135434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000534712A Expired - Fee Related CA1317413C (en) | 1987-04-14 | 1987-04-14 | Process for preparing protein concentrates from brewer's spent grain |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1317413C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004053108A1 (en) * | 2002-12-11 | 2004-06-24 | Andrzej Gamian | Protein fraction of barley spent grains as a medium for growth, sporulation and selection of actinomycetes and related bacteria |
| WO2017089655A1 (en) * | 2015-11-27 | 2017-06-01 | Teknologian Tutkimuskeskus Vtt Oy | Process for separating proteins from biomass materials |
| US11477994B2 (en) | 2017-07-28 | 2022-10-25 | Coors Brewing Company | Protein extraction from spent grains |
| WO2023010194A1 (en) * | 2021-08-04 | 2023-02-09 | Ambev S.A | Process for extracting protein from malt bagasse, food product, and use of proteins extracted by said process |
-
1987
- 1987-04-14 CA CA000534712A patent/CA1317413C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004053108A1 (en) * | 2002-12-11 | 2004-06-24 | Andrzej Gamian | Protein fraction of barley spent grains as a medium for growth, sporulation and selection of actinomycetes and related bacteria |
| WO2017089655A1 (en) * | 2015-11-27 | 2017-06-01 | Teknologian Tutkimuskeskus Vtt Oy | Process for separating proteins from biomass materials |
| US11477994B2 (en) | 2017-07-28 | 2022-10-25 | Coors Brewing Company | Protein extraction from spent grains |
| WO2023010194A1 (en) * | 2021-08-04 | 2023-02-09 | Ambev S.A | Process for extracting protein from malt bagasse, food product, and use of proteins extracted by said process |
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Legal Events
| Date | Code | Title | Description |
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| MKLA | Lapsed |