US3922200A
Expired / Lapsed
US
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Enzymatic hydrolysis of granular starch
Assignee: Unilever Bestfoods North America
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Filing: 1974-03-18
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Granted: 1975-11-25
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Expires: 1994-03-18
Abstract
Abstract A method for the hydrolysis of starch wherein an aqueous slurry of granular starch is first stabilized in part by the action of alpha-amylase under non-gelatinizing conditions, then heated briefly to solubilize the remaining granular starch, then saccharified by treatment with a saccharifying enzyme.
Inventors
- 👤 Raoul Guillaume Philippe Walon
- 👤 Elie Francois Berghmans
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 22:44
CPC Classifications
C; C13; C13K; C13K7/00; Y; Y10; Y10S; Y10S435/00; Y10S435/8215; Y10S435/822; Y10S435/832; Y10S435/836
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
203 words
A PROCESS FOR DIRECTLY CONVERTING GRANULAR STARCH TO A SOLUBLE STARCH HYDO R ROLYSATE, COMPRISING: A. AGITATING A MIXTURE OF GRANULAR STARCH, WATER, AND AN ALPHA-AMYLASE ENZYME PREPARATION, ENZYMATICALLY SOLUBILIZING THE STARCH IN SAID AGITATED MIXTURE AT A TEMPERATURE IN THE RANGE FROM THE NORMAL INITIAL GELATINIZATION TEMPERATURE OF THE STARCH TO THE ACTUAL GELATINIZATION TEMPERATURE OF THE STARCH, MIANTAINING SAID CONDITIONS OF ENZYMATIC SOLUBILIZAT ON FOR A PERIOD OF TIME TO ENZYMATICALLY CONVERT AT LEAST ABOUT 10% OF THE STARCH TO A SOLUBLE STARCH HYDROLYSATE, WHEREBY ANY RESIDUAL, NON-SOLUBLE STARCH FROM SAID CONDITIONS HAS SUBSTANTIALLY RETAINED ITS GRANULAR, UNGELATINIZED FROM; B. HEATING SAID MIXTURE TO A TEMPERATURE ABOVE THE GELATINIZATION TEMPERATURE OF THE STARCH SO AS TO GELATINIZE SUBSTANTIALLY ALL OF THE REMAINING NON-SOLUBLE, UNGELATINIZED GRANULAR STARCH IN THE MIXTURE; AND C. ADJUSTING THE TEMPERATURE TO WITHIN THE RANGE FROM ABOUT 50*C. TO ABOUT 65*C. AND THE PH TO WITHIN THE RANGE FROM ABOUT 4 TO ABOUT 6, AND ADDING AT LEAST ONE SACCHARIFYING ENZYME PREPARATION TO ENZYMATICALLY SACCHARIFY AND CONVERT THE HEAT-TREATED SOLUBLE STARCH ENZYME PREPARATION IS THE ACTION OF THE SACCHARIFICATION ENZYME PREPARATION IS CONDUCTED SUCH AS TO SUBSTANTIALLY INCREASE THE DEXTROSE EQUIVALENT VALUE (D.E.) OF THE SOLUBLE STARCH HYDROLYSATE.
Claim 2
Dependent Claim
203 words
A PROCESS FOR DIRECTLY CONVERTING GRANULAR STARCH TO A SOLUBLE STARCH HYDO R ROLYSATE, COMPRISING: A. AGITATING A MIXTURE OF GRANULAR STARCH, WATER, AND AN ALPHA-AMYLASE ENZYME PREPARATION, ENZYMATICALLY SOLUBILIZING THE STARCH IN SAID AGITATED MIXTURE AT A TEMPERATURE IN THE RANGE FROM THE NORMAL INITIAL GELATINIZATION TEMPERATURE OF THE STARCH TO THE ACTUAL GELATINIZATION TEMPERATURE OF THE STARCH, MIANTAINING SAID CONDITIONS OF ENZYMATIC SOLUBILIZAT ON FOR A PERIOD OF TIME TO ENZYMATICALLY CONVERT AT LEAST ABOUT 10% OF THE STARCH TO A SOLUBLE STARCH HYDROLYSATE, WHEREBY ANY RESIDUAL, NON-SOLUBLE STARCH FROM SAID CONDITIONS HAS SUBSTANTIALLY RETAINED ITS GRANULAR, UNGELATINIZED FROM; B. HEATING SAID MIXTURE TO A TEMPERATURE ABOVE THE GELATINIZATION TEMPERATURE OF THE STARCH SO AS TO GELATINIZE SUBSTANTIALLY ALL OF THE REMAINING NON-SOLUBLE, UNGELATINIZED GRANULAR STARCH IN THE MIXTURE; AND C. ADJUSTING THE TEMPERATURE TO WITHIN THE RANGE FROM ABOUT 50*C. TO ABOUT 65*C. AND THE PH TO WITHIN THE RANGE FROM ABOUT 4 TO ABOUT 6, AND ADDING AT LEAST ONE SACCHARIFYING ENZYME PREPARATION TO ENZYMATICALLY SACCHARIFY AND CONVERT THE HEAT-TREATED SOLUBLE STARCH ENZYME PREPARATION IS THE ACTION OF THE SACCHARIFICATION ENZYME PREPARATION IS CONDUCTED SUCH AS TO SUBSTANTIALLY INCREASE THE DEXTROSE EQUIVALENT VALUE (D.E.) OF THE SOLUBLE STARCH HYDROLYSATE.
Claim 3
Dependent Claim
11 words
The process of claims 1, wherein the starch is corn starch.
Claim 4
Dependent Claim
20 words
The process of claim 1, wherein the concentration of the starch is from about 5% to about 40%, by weight.
Claim 5
Dependent Claim
32 words
The process of claim 1, wherein the starch is corn starch and the enzymatic solubilization of step (a) is conducted at a temperature in the range from about 55*C. to about 75*C.
Claim 6
Dependent Claim
34 words
The process of claim 1, wherein the amount of alpha-amylase used in step (a) is sufficient to provide from about 0.1 to about 25 alpha-amylase units of activity per gram of starch (dry basis).
Claim 7
Dependent Claim
18 words
The process of claim 1, wherein the alpha-amylase used in step (a) is derived from a Bacillus organism.
Claim 8
Dependent Claim
19 words
The process of claim 1, wherein the alpha-amylase used in step (a) is derived from a Bacillus licheniformis organism.
Claim 9
Dependent Claim
18 words
The process of claim 1, wherein a saccharification enzyme preparation is added to the mixture of step (a).
Claim 10
Dependent Claim
28 words
The process of claim 1, wherein the agitated mixture in step (a) contains from about 0.01 to about 1.0% of an anionic surfactant, by weight of the mixture.
Claim 11
Dependent Claim
25 words
The process of claim 1, wherein the temperature of the heating in step (b) is in the range of from about 85*C. to about 150*C.
Claim 12
Dependent Claim
57 words
The process of claim 1, wherein one of the saccharification enzymes of step (c) is a glucoamylase enzyme preparation and the pH is in the range from about 4 to about 4.5, said preparation being present in an amount to provide from about 0.05 to about 5 glucoamylase units of activity per gram of starch (dry basis).
Claim 13
Dependent Claim
45 words
The process of claim 1, wherein one of the saccharification enzymes of step (c) is a beta-amylase enzyme preparation, said preparation being present in a amount to provide from about 0.1 to about 5 of beta-amylase units of activity per gram of starch (dry basis).
Claim 14
Dependent Claim
45 words
The process of claim 1, wherein a pullulanase enzyme preparation is added to the mixture of step (a) and/or step (c) in an amount to provide from about 0.1 to about 0.5 pullulanase units of activity per gram of starch (dry basis) in the mixture.
Claim 15
Dependent Claim
23 words
The process of claim 1, wherein the mixture of step (a) additionally includes starch solubilization products to inhibit the gelatinization of the starch.
Claim 16
Dependent Claim
221 words
A process for directly converting granular starch to a soluble starch hydrolysate, comprising: a. agitating a mixture of granular starch, water, and a bacterial alpha-amylase enzyme preparation, said starch having a concentration from about 5% to about 40%, by weight of the mixture, enzymatically solubilizing the starch in said agitated mixture, at a temperature in the range from the normal initial gelatinization temperaTure of the starch to the actual gelatinization temperature of the starch, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convert at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, nonsoluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 85*C. to about 150*C. to gelatinize substantially all of the remaining non-soluble, residual granular starch in the mixture; and c. adjusting the temperature to within the range from about 50*C. to about 65*C. and the pH from about 4 to about 6, and adding at least one saccharifying enzyme preparation selected from the group consisting of glucoamylase and/or beta-amylase to enzymatically saccharify and convert the heat-treated soluble starch hydrolysate whereby the action of the saccharification enzyme preparation(s) is conducted such as to substantially increase the dextrose equivalent value (D.E.) of the soluble starch hydrolysate.
Claim 17
Dependent Claim
221 words
A process for directly converting granular starch to a soluble starch hydrolysate, comprising: a. agitating a mixture of granular starch, water, and a bacterial alpha-amylase enzyme preparation, said starch having a concentration from about 5% to about 40%, by weight of the mixture, enzymatically solubilizing the starch in said agitated mixture, at a temperature in the range from the normal initial gelatinization temperaTure of the starch to the actual gelatinization temperature of the starch, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convert at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, nonsoluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 85*C. to about 150*C. to gelatinize substantially all of the remaining non-soluble, residual granular starch in the mixture; and c. adjusting the temperature to within the range from about 50*C. to about 65*C. and the pH from about 4 to about 6, and adding at least one saccharifying enzyme preparation selected from the group consisting of glucoamylase and/or beta-amylase to enzymatically saccharify and convert the heat-treated soluble starch hydrolysate whereby the action of the saccharification enzyme preparation(s) is conducted such as to substantially increase the dextrose equivalent value (D.E.) of the soluble starch hydrolysate.
Claim 18
Dependent Claim
29 words
The process of claim 15, wherein the starch is corn starch and the temperature of agitated mixture in step (a) is in the range from 55*C. to about 75*C.
Claim 19
Dependent Claim
35 words
The process of claim 15, wherein the amount of the alpha-amylase used in step (a) is sufficient to provide from about 0.1 to about 25 alpha-amylase units of activity per gram of starch (dry basis).
Claim 20
Dependent Claim
19 words
The process of claim 15, wherein the alpha-amylase used in step (a) is derived from a Bacillus licheniformis organism.
Claim 21
Dependent Claim
43 words
The process of claim 15, wherein the alpha-amylase used in step (a) is derived from a strain of the Bacillus licheniformis organism selected from the group consisting of NCIB 8061, NCIB 8059, ATCC 6598, ATCC 6634, ATCC 8480, ATCC 9545A and ATCC 11945.
Claim 22
Dependent Claim
24 words
The process of claim 15, wherein the temperature of the heating step (b) is in the range of from about 100*C. to about 115*C.
Claim 23
Dependent Claim
54 words
The process of claim 15, wherein a glucoamylase enzyme preparation is used in step (c) in an amount such as to provide from about 0.05 to about 5.0 glucoamylase units of activity per gram of starch (dry basis) and the pH of the mixture is in the range of from 4.0 to about 4.5.
Claim 24
Dependent Claim
38 words
The process of claim 15, wherein a beta-amylase enzyme preparation is used in step (c) in an amount such as to provide from about 0.1 to about 5.0 beta-amylase units of activity per gram of starch (dry basis).
Claim 25
Dependent Claim
44 words
The process of claim 15, wherein a pullulanase enzyme preparation is added to the mixture of step (a) and/or step (c) in an amount such as to provide from about 0.1 to about 0.5 pullulanase units of activity per gram of starch (dry basis).
Claim 26
Dependent Claim
23 words
The process of claim 15, wherein the mixture of step (a) contains a saccharifying enzyme preparation in addition to the alpha-amylase enzyme preparation.
Claim 27
Dependent Claim
268 words
A process for directly converting granular corn starch to a soluble corn starch hydrolysate containing dextrose comprising: a. agitating a mixture of granular corn starch, water, an alpha-amylase enzyme preparation derived from a Bacillus licheniformis organism, wherein the starch is present at a concentration in the range from about 5% to about 40% by weight of the mixture, the alpha-amylase enzyme preparation present in the mixture is sufficient to provide from about 1.0 to about 10 alpha-amylase units of activity per gram of corn starch (dry basis), enzymatically solubilizing the corn starch in said agitated mixture at a temperature in the range from the normal initial gelatinization temperature to the actual gelatinization temperature of the coorn starch, at a pH from about 4 to about 7, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convErt at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, non-soluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 100*C. to about 115*C. to gelatinize substantially all of the remaining non-soluble residual, granular starch in the mixture; and c. adjusting the temperature of the mixture within the range from about 50*C. to about 65*C. and the pH from about 4 to about 4.5, and adding a glucoamylase enzyme preparation, in an amount such as to provide from about 0.05 to about 5 glucoamylase units of activity per gram of starch (dry basis) to ensymatically saccharify and convert the soluble starch hydrolysate to a soluble starch hydrolysate containing dextrose.
Claim 28
Dependent Claim
268 words
A process for directly converting granular corn starch to a soluble corn starch hydrolysate containing dextrose comprising: a. agitating a mixture of granular corn starch, water, an alpha-amylase enzyme preparation derived from a Bacillus licheniformis organism, wherein the starch is present at a concentration in the range from about 5% to about 40% by weight of the mixture, the alpha-amylase enzyme preparation present in the mixture is sufficient to provide from about 1.0 to about 10 alpha-amylase units of activity per gram of corn starch (dry basis), enzymatically solubilizing the corn starch in said agitated mixture at a temperature in the range from the normal initial gelatinization temperature to the actual gelatinization temperature of the coorn starch, at a pH from about 4 to about 7, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convErt at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, non-soluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 100*C. to about 115*C. to gelatinize substantially all of the remaining non-soluble residual, granular starch in the mixture; and c. adjusting the temperature of the mixture within the range from about 50*C. to about 65*C. and the pH from about 4 to about 4.5, and adding a glucoamylase enzyme preparation, in an amount such as to provide from about 0.05 to about 5 glucoamylase units of activity per gram of starch (dry basis) to ensymatically saccharify and convert the soluble starch hydrolysate to a soluble starch hydrolysate containing dextrose.
Claim 29
Dependent Claim
39 words
The process of claim 25, wherein a glucoamylase emzyme preparation is added to the mixture of step (a) in an amount to provide from about 0.01 to about 0.3 glucoamylase units of activity per gram of starch (dry basis).
Claim 30
Dependent Claim
46 words
The process of claim 25, wherein a pullulanase enzyme is added to the mixture of step (a) and/or step (c) in an amount such as to provide from about 0.1 to about 0.5 pullulanase units of activity per gram of starch (dry basis) in the mixture.
Claim 31
Dependent Claim
23 words
The process of claim 25, wherein the mixture of step (a) additionally includes starch solubilization products to inhibit the gelatinization of the starch.
Claim 32
Dependent Claim
32 words
The process of claim 25, wherein the mixture of step (a) additionally contains an anionic surfactant in an amount ranging from about 0.01% to about 1.0% by weight of the agitated mixture.
Claim 33
Dependent Claim
47 words
The process of claim 25, wherein the solubilization, and saccharification steps are conducted in an ultrafiltration cell wherein the enzyme preparation and non-soluble starch are retained in the cell and the soluble corn starch hydrolysate containing dextrose is passed through a semi-permeable membrane of said ultrafiltration cell.
Claim 34
Dependent Claim
266 words
A process for directly converting granular starch to a soluble starch hydrolysate containing maltose and maltotriose, comprising: a. agitating a mixture of granular starch, water, an alpha-amylase enzyme preparation derived from a Bacillus licheniformis organism, wherein the starch is present at a concentration in the range from about 5% to about 40%, by weight, of the mixture, the alpha-amylase enzyme preparation is present in an amount to provide from about 1.0 to about 10 alpha-amylase units of activity per gram of starch (dry basis), to enzymatically solubilize the starch in said agitated mixture at a temperature in the range from the normal initial gelatinization temperature to the actual gelatinization temperature of the starch, at a pH from about 4 to about 7, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convert at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, non-soluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 100*C. to about 115*C. to gelatinize substantially all of the remaining non-soluble residual, granular starch in the mixture; and c. adjusting the temperature of the mixture within the range from about 50*C. to about 65*C. and the pH from about 4 to about 6, and adding a beta-amylase enzyme preparation in an amount such as to provide from about 0.1 to about 5 beta-amylase units of activity per gram of starch (dry basis), to enzymatically saccharify and convert the soluble starch hydrolysate to a soluble starch hydrolysate containing maltose and maltotriose.
Claim 35
Dependent Claim
266 words
A process for directly converting granular starch to a soluble starch hydrolysate containing maltose and maltotriose, comprising: a. agitating a mixture of granular starch, water, an alpha-amylase enzyme preparation derived from a Bacillus licheniformis organism, wherein the starch is present at a concentration in the range from about 5% to about 40%, by weight, of the mixture, the alpha-amylase enzyme preparation is present in an amount to provide from about 1.0 to about 10 alpha-amylase units of activity per gram of starch (dry basis), to enzymatically solubilize the starch in said agitated mixture at a temperature in the range from the normal initial gelatinization temperature to the actual gelatinization temperature of the starch, at a pH from about 4 to about 7, maintaining said conditions of enzymatic solubilization for a period of time to enzymatically convert at least about 10% of the starch to a soluble starch hydrolysate, whereby any residual, non-soluble starch from said conditions has substantially retained its granular, ungelatinized form; b. heating said mixture to a temperature in the range from about 100*C. to about 115*C. to gelatinize substantially all of the remaining non-soluble residual, granular starch in the mixture; and c. adjusting the temperature of the mixture within the range from about 50*C. to about 65*C. and the pH from about 4 to about 6, and adding a beta-amylase enzyme preparation in an amount such as to provide from about 0.1 to about 5 beta-amylase units of activity per gram of starch (dry basis), to enzymatically saccharify and convert the soluble starch hydrolysate to a soluble starch hydrolysate containing maltose and maltotriose.
Claim 36
Dependent Claim
39 words
The process of claim 31, wherein a beta-amylase enzyme preparation is added to the mixture of step (a) in an amount to provide from about 0.1 to about 5 beta-amylase units of activity per gram of starch (dry basis).
Claim 37
Dependent Claim
44 words
The process of claim 31, wherein a pullulanase enzyme is added to the mixture of step (a) and/or step (c) in an amount to provide from about 0.1 to about 0.5 pullulanase units of activity per gram of starch (dry basis), in the mixture.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-11-24 | 1979-05-26 | 1979-11-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-11-24 | 1983-05-26 | 1983-11-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-11-24 | 1987-05-26 | 1987-11-25 | $7700.00 | Window Closed / Lapsed |