CN113061193A - Method for preparing RS-5 type resistant starch by melt extrusion method - Google Patents

Method for preparing RS-5 type resistant starch by melt extrusion method Download PDF

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CN113061193A
CN113061193A CN202110348465.6A CN202110348465A CN113061193A CN 113061193 A CN113061193 A CN 113061193A CN 202110348465 A CN202110348465 A CN 202110348465A CN 113061193 A CN113061193 A CN 113061193A
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starch
resistant starch
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崔波
刘鹏飞
邹飞雪
袁超
吴正宗
于滨
郭丽
卢璐
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Qilu University of Technology
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/20Amylose or amylopectin
    • AHUMAN NECESSITIES
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    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/125Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The invention belongs to the technical field of resistant starch, and particularly relates to a method for preparing RS-5 type resistant starch by using a melt extrusion method. In the extrusion process, the high-temperature, high-pressure and strong shearing action in the double-screw extruder is utilized to destroy the 'shell' structure of the starch granules, break the alpha-1 → 6 glycosidic bond of a part of amylopectin and release more linear starch participating in the reaction; adding substance with strong hydrogen bond forming ability with starch molecule such as glycerol, weakening strong hydrogen bond acting force between original starch molecules, and lowering melting temperature of starch. And meanwhile, the crystalline region of the starch is damaged, so that more guest molecules can enter the starch granules possibly, the opportunity of contacting the host molecules and the guest molecules is increased, the complexing efficiency is improved, and the formation of RS-5 resistant starch is promoted. The prepared RS-5 resistant starch has high complexation index and high enzyme resistance. And can be used as food material for preventing and treating type II diabetes.

Description

Method for preparing RS-5 type resistant starch by melt extrusion method
Technical Field
The invention belongs to the technical field of resistant starch, and particularly relates to a method for preparing RS-5 type resistant starch by using a melt extrusion method.
Background
Resistant starch refers to starch that is not digested and absorbed in the small intestine, but is fermented by the microflora in the colon after 120min, thereby exerting beneficial physiological effects. Resistant starches can generally be divided into four categories: RS1 (physical embedded starch); RS2 (native resistant starch granules); RS3 (retrograded starch); RS4 (chemically modified starch). In recent years, researchers have defined enzyme-resistant V-type amylose-lipid complexes as the fifth type of resistant starch RS 5. RS5 can reduce postprandial blood glucose response, and has certain preventive effect on metabolic syndrome, such as type II diabetes, obesity, hypertension and heart disease.
The preparation method of RS 5-type resistant starch is generally divided into chemical method and physical method. The chemical method includes DMSO dispersion method, KOH/HCl solution method, phosphorylase catalytic synthesis method, etc. Although the chemical method has high recombination rate, a large amount of waste liquid is generated in the production process, and the environment is polluted. Physical methods generally include heating methods, ultra-high pressure methods, extrusion cooking methods, and the like. Compared with a chemical method, the physical method has the defects of low production efficiency, long preparation time and the like. The method is mainly characterized in that sub-particles 'blocklets' at the periphery of starch particles are mutually fused to form a thicker 'shell', and a compact and firm crystallization area is formed in the starch particles due to mutual association of molecules and molecules through hydrogen bonds on hydroxyl groups, so that guest molecules are prevented from entering the interior of the starch particles and being complexed with amylose, and the physical preparation method has low complexation index and low reaction efficiency. There is a strong need for an efficient and pollution-free method for preparing RS 5-type resistant starch.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides the processing method for preparing the RS-5 type resistant starch, which has high efficiency, environmental protection, low energy consumption and capability of realizing continuous production, and the prepared RS-5 type resistant starch has higher enzymolysis resistance and high complexing index.
The invention is realized by the following technical scheme:
a method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: slowly stirring starch and fatty acid; adding glycerol, and rapidly stirring; uniformly mixing, bagging and standing;
(2) melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into a co-rotating parallel double-screw extruder set through a single-screw feeder system, and setting the rotating speed of a feeding screw, the rotating speed of an extruding screw and the temperature of the extruder set from a feeding port and a first area to a fifth area of a machine barrel;
(3) granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Preferably, the addition amount of the glycerol in the step (1) is 20-25% of the mass of the starch.
Preferably, the addition amount of the fatty acid in the step (1) is 3-12% of the mass of the starch.
Preferably, the fatty acid in step (1) is one of lauric acid, myristic acid, palmitic acid, stearic acid and arachidic acid.
Preferably, the conditions of slow stirring in step (1) are as follows: the rotation speed is 200-300rpm, and the time is 5-10 min; the conditions of rapid stirring were: the rotation speed is 1000-1500rpm, and the time is 5-10 min.
Preferably, in the step (2), the rotation speed of the feeding screw is 10-20rpm, the rotation speed of the extrusion screw is 50-120rpm, and the temperature of the extrusion unit from the feeding port, the first zone to the fifth zone of the cylinder is 80-90, 90-100, 105-115, 120-130, 110-120, 105-115 ℃.
The RS-5 type resistant starch prepared by the preparation method.
The RS-5 resistant starch can be used as food material for preventing and treating type II diabetes.
In the extrusion process, the high-temperature, high-pressure and strong shearing action in the double-screw extruder is utilized to destroy the 'shell' structure of the starch granules, break the alpha-1 → 6 glycosidic bond of a part of amylopectin and release more linear starch participating in the reaction; adding substance with strong hydrogen bond forming ability with starch molecule such as glycerol, weakening strong hydrogen bond acting force between original starch molecules, and lowering melting temperature of starch. And meanwhile, the crystalline region of the starch is damaged, so that more guest molecules can enter the starch granules possibly, the opportunity of contacting the host molecules and the guest molecules is increased, the complexing efficiency is improved, and the formation of RS-5 resistant starch is promoted.
The invention has the beneficial effects that:
(1) the invention adopts a melt extrusion method to prepare RS-5 type resistant starch, alpha-1 → 6 glycosidic bond of amylopectin is broken under the action of high temperature, high pressure and strong shearing in the extrusion process, a part of branched side chain is broken, the number of linear starch chains participating in the reaction is increased, and the formation of RS-5 type resistant starch is promoted.
(2) According to the invention, food-grade glycerol is added, and new hydrogen bonds are formed between glycerol molecules and starch molecules, so that the strong hydrogen bond acting force between the original starch molecules can be weakened, and the melting temperature of the starch is reduced. And meanwhile, the crystalline region of the starch is damaged, so that more guest molecules can enter the starch granules possibly, the contact chance of the fatty acid and the amylose of the guest molecules is increased, and the complexing efficiency is improved.
(3) The preparation process is safe, efficient, environment-friendly and low in energy consumption, and can realize continuous industrial production of RS-5 resistant starch.
(4) The RS-5 type resistant starch prepared by the method has high complexation index and high enzyme resistance. And can be used as food material for preventing and treating type II diabetes.
Detailed Description
In order to better understand the present invention, the technical solutions of the present invention are further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and lauric acid accounting for 3% of the starch addition amount into an SHR-50 type high-speed stirrer, slowly stirring at 300rpm for 5min, adding food grade glycerol accounting for 20% of the starch addition amount, rapidly stirring at 1000rpm for 10min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 15rpm, the rotating speed of an extrusion screw is set to be 70rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 85, 100, 105, 130, 115 and 115 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Example 2
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and stearic acid accounting for 5% of the starch addition amount into an SHR-50 type high-speed stirrer, slowly stirring at 250rpm for 8min, adding food grade glycerol accounting for 22% of the starch addition amount, rapidly stirring at 1300rpm for 7min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 16rpm, the rotating speed of an extrusion screw is set to be 80rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 90, 100, 110, 130, 110 and 105 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Example 3
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and myristic acid 7% of the starch addition amount into an SHR-50 type high-speed stirrer, slowly stirring at 300rpm for 6min, adding food grade glycerol 25% of the starch addition amount, rapidly stirring at 1500rpm for 5min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 18rpm, the rotating speed of an extrusion screw is set to be 100rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 85, 95, 110, 125, 110 and 115 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Example 4
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and palmitic acid accounting for 12% of the added amount of the starch into an SHR-50 type high-speed stirrer, slowly stirring at 300rpm for 10min, adding food-grade glycerol accounting for 25% of the added amount of the starch, rapidly stirring at 1400rpm for 10min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 20rpm, the rotating speed of an extrusion screw is set to be 120rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 85, 90, 115, 120, 110 and 105 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Example 5
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and arachidic acid accounting for 8% of the starch addition into an SHR-50 type high-speed stirrer, slowly stirring at 280rpm for 7min, adding food-grade glycerol accounting for 24% of the starch addition, rapidly stirring at 1200rpm for 6min, mixing well, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 16rpm, the rotating speed of an extrusion screw is set to be 75rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 90, 90, 110, 130, 120 and 115 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Example 6
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding sweet potato starch and palmitic acid accounting for 9% of the starch addition amount into an SHR-50 type high-speed stirrer, slowly stirring at 260rpm for 8min, adding food grade glycerol accounting for 25% of the starch addition amount, rapidly stirring at 1500rpm for 8min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 20rpm, the rotating speed of an extrusion screw is set to be 110rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 85, 90, 110, 125, 115 and 110 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Comparative example 1
A method for preparing RS-5 resistant starch by using a melt extrusion method comprises the following steps:
(1) mixing raw materials and auxiliary materials: adding corn starch and myristic acid 7% of the starch addition amount into an SHR-50 type high-speed stirrer, slowly stirring at 300rpm for 6min, adding water 25% of the starch addition amount, rapidly stirring at 1500rpm for 5min, uniformly mixing, bagging, and standing for 24 h.
(2) Melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into an SHJ20 type co-rotating parallel twin-screw extruder set through a single-screw feeder system, wherein the rotating speed of a feeding screw is set to be 18rpm, the rotating speed of an extrusion screw is set to be 100rpm, and the temperatures of the extruder set from a feeding port and a first zone to a fifth zone of a machine barrel are set to be 85, 95, 110, 125, 110 and 115 ℃.
(3) Granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
Examples of the effects of the invention
The in vitro digestibility of the resistant starches of the RS-5 type prepared in examples 1 to 6 and comparative example 1 was tested, and the test results are shown in Table 1 below.
Determination of in vitro digestion performance of RS-5 type resistant starch: the glucose oxidase method is adopted to determine the content of Resistant Starch (RS) in RS-5 type resistant starch and corn native starch, and the specific test method comprises the following steps: mixing 200 mg of a sample to be detected with water, gelatinizing the mixture at 95 ℃ for 20min, cooling the mixture to room temperature, placing the mixture in a constant-temperature water bath kettle at 37 ℃, adding a sodium acetate buffer solution with pH 5.2 after the temperature is balanced to constant volume of 15 mL, then adding 10 mL of mixed enzyme solution (290U/mL pancreatic alpha-amylase and 20U/mL amyloglucosidase), and fully reacting the mixture for 120min after the samples are uniformly mixed. Hydrolyzing for 20min and 120min, respectively taking out 0.5 ml of enzymolysis solution, rapidly adding appropriate amount of anhydrous ethanol to inactivate enzyme, standing, centrifuging, collecting appropriate amount of centrifuged supernatant, and measuring glucose content with glucose oxidase method.
The calculation formula is as follows:
RDS =(m20 – m0)× 0.9
SDS =(m120 – m20)× 0.9
RS =100 – (RDS+SDS)
in the formula: m is0Is the free glucose content of the starch before the enzyme hydrolysis treatment; m is20The glucose content is determined after 20min of amylase hydrolysis; m is120Is the glucose content measured after 120min of amylase hydrolysis.
Figure DEST_PATH_IMAGE001
As can be seen from table 1, the corn starch-lipid complex prepared by the present invention has a resistant starch content as high as 32.9% (example 3), and the resistant starch content is significantly increased compared to the corn native starch. Meanwhile, the resistant starch content of the corn starch-lipid complex prepared by the melt extrusion method of the present invention is significantly higher than that of the sample prepared by the conventional extrusion cooking method (comparative example 1), which indicates that the amylose-lipid complex is more easily formed by the melt extrusion method.

Claims (8)

1. A method for preparing RS-5 resistant starch by a melt extrusion method is characterized by comprising the following steps:
(1) mixing raw materials and auxiliary materials: slowly stirring starch and fatty acid; adding glycerol, and rapidly stirring; uniformly mixing, bagging and standing;
(2) melt extrusion construction of RS-5 type resistant starch: uniformly feeding the material obtained in the step (1) into a co-rotating parallel double-screw extruder set through a single-screw feeder system, and setting the rotating speed of a feeding screw, the rotating speed of an extruding screw and the temperature of the extruder set from a feeding port and a first area to a fifth area of a machine barrel;
(3) granulating and crushing RS-5 resistant starch: and (3) cutting the extrudate obtained in the step (2) into particles by a water-cooling bracing and particle cutting system, crushing the particles by a crusher, and sealing and packaging the particles for later use.
2. The method for preparing RS-5 resistant starch by using a melt extrusion process according to claim 1, wherein the glycerol is added in the step (1) in an amount of 20 to 25% by mass of the starch.
3. The method for preparing RS-5 resistant starch by using a melt extrusion process according to claim 1, wherein the fatty acid is added in the step (1) in an amount of 3-12% by mass of the starch.
4. The method for preparing RS-5 resistant starch according to claim 1, wherein the fatty acid in step (1) is one of lauric acid, myristic acid, palmitic acid, stearic acid, and arachidic acid.
5. The method for preparing RS-5 resistant starch by using a melt extrusion process according to claim 1, wherein the slow stirring condition in the step (1) is as follows: the rotation speed is 200-300rpm, and the time is 5-10 min; the conditions of rapid stirring were: the rotation speed is 1000-1500rpm, and the time is 5-10 min.
6. The method for preparing RS-5 resistant starch by melt extrusion as claimed in claim 1, wherein the feeding screw speed in step (2) is 10-20rpm, the extrusion screw speed is 50-120rpm, and the temperature of the extrusion unit from the feeding port, barrel zone one to zone five is 80-90, 90-100, 105-115, 120-130, 110-120, 105-115 ℃.
7. The RS-5 type resistant starch prepared by the method of claim 1.
8. Resistant starch of the RS-5 type according to claim 7 as food material for the prevention and treatment of type II diabetes.
CN202110348465.6A 2021-03-31 2021-03-31 Method for preparing RS-5 type resistant starch by melt extrusion method Pending CN113061193A (en)

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CN113907332A (en) * 2021-09-10 2022-01-11 天津科技大学 Efficient preparation method and application of crystal form-controllable starch-lipid compound
CN113907332B (en) * 2021-09-10 2024-05-24 天津科技大学 Efficient preparation method and application of crystal-controllable starch-lipid compound

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113907332A (en) * 2021-09-10 2022-01-11 天津科技大学 Efficient preparation method and application of crystal form-controllable starch-lipid compound
CN113907332B (en) * 2021-09-10 2024-05-24 天津科技大学 Efficient preparation method and application of crystal-controllable starch-lipid compound

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