CN115010818A - Method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment - Google Patents
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
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Abstract
The invention discloses a method for preparing resistant starch RS4 by far infrared cooperative vacuum treatment, which comprises the following steps: (1) mixing a citric acid solution (with a concentration of 50%) with natural corn starch according to a mass ratio of 0.4-0.6, adjusting the pH of the mixed solution to 2.5-3.5 by using a 10mol/L NaOH solution, and standing for 16 hours at room temperature. Drying the mixture in a drying oven at 50 deg.C until the water content is about 8%, grinding, and sieving. (2) Uniformly spreading the starch treated by the citric acid on a stainless steel tray for infrared ion treatmentAnd (5) performing vacuum synergistic treatment. The vacuum degree of the processing environment is 100kPa, and the infrared radiation intensity is 1500-3800W/m 2 And the infrared radiation time is 6-8 min. And after the reaction is finished, taking out the starch, respectively washing the starch for 3 times and 1 time by using distilled water and absolute ethyl alcohol, then placing the washed starch in a drying box at 50 ℃ for drying until the water content is about 8%, and grinding the starch by using a screen with a sieve pore of 0.075mm to obtain the resistant starch RS 4. The method can effectively improve the yield and the preparation rate of the resistant starch in the natural starch on the basis of realizing green production, energy conservation and emission reduction.
Description
Technical Field
The invention belongs to the technical field of agricultural product processing, and particularly relates to a method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment.
Background
The resistant starch is starch which is not easy to be enzymolyzed by small intestine and has the function similar to dietary fiber, and has important practical significance for controlling blood sugar, reducing cholesterol, regulating intestinal flora and improving dietary structure. According to the difference of starch sources and enzymolysis mechanisms, the starch is mainly classified into four types including RS1, RS2, RS3 and RS 4.
Resistant starch RS4, i.e., chemically modified starch, refers to a type of starch that produces new functional groups through modification such as esterification, etherification, or crosslinking. Esterification modification is one of the most important ways in chemical modification, which optimizes the physicochemical properties of the starch by introducing new ester functions. Citric acid is used as a nontoxic and harmless organic acid, is considered as a safe food additive by many countries and regions, has stronger depolymerization capability on starch, and is more beneficial to the synthesis of starch ester. The citric acid starch ester has the characteristics of green safety, high heat stability and digestion resistance, is widely applied to the fields of food, chemical industry, medicine and the like, contains digestion resistance similar to the physiological function of dietary fiber, can reduce blood sugar reaction, reduce fat accumulation, reduce the risk of rectal cancer, diabetes and intestinal diseases, and improve intestinal flora; the characteristics of thermal stability and green safety are used as related substitutes for manufacturing edible films, medicine slow release, degradable packages and the like.
However, the research on the preparation of starch ester is mainly focused on the basis of the traditional dry and wet heating method, the preparation efficiency of the method is low, the pollution of waste gas and waste water to the environment is large, and the contradiction between the product quality and the production efficiency is outstanding. In order to improve the preparation efficiency and reduce the pollution discharge, some researchers introduce physical technologies such as microwave, extrusion, ultrahigh pressure and the like into the starch modification and esterification processes, and although the research shortens the preparation time of the resistant starch to a certain extent, the research also has some defects. The invention discloses an efficient modified starch processing technology (patent publication No. CN 112321735A), which discloses a novel technology for preparing cassava modified starch by directly performing microwave treatment on a semi-finished product crushed by a crusher through a microwave heating drying tank, coupling the microwave and enzyme processes to form a microwave-enzyme method coupled process, and preparing a series of cassava modified starch products. The invention patent 'a composite process for preparing modified starch' (patent publication No. CN 112812195A) discloses a method for preparing modified starch by using common starch or flour as raw material, adding acidic modifier, oxidant, water, auxiliary components or a mixture thereof before or after entering a double-screw extruder, and simultaneously pre-gelatinizing, acidifying or oxidizing and modifying the starch in the screw extruder. Therefore, the establishment of a more robust and efficient starch ester preparation method is an urgent problem to be solved in the field.
Disclosure of Invention
In order to solve the problems, the application provides a method for preparing resistant starch RS4 by far infrared cooperative vacuum treatment, so as to improve the preparation efficiency of RS 4.
Specifically, the present invention is realized by:
a method for preparing resistant starch RS4 by far infrared cooperative vacuum treatment comprises the following steps:
(1) mixing a citric acid solution (with the concentration of 50%) with natural corn starch to obtain a mixed solution, adjusting the pH value to 2.5-3.5, and standing to obtain a mixture; drying the mixture in a drying oven at 50 ℃ until the water content is about 8%, taking out, grinding and sieving to obtain a starch crude product;
(2) uniformly spreading the starch crude product obtained in the step (1) on a stainless steel tray, placing the stainless steel tray in a vacuum environment, starting a vacuum pump and a far infrared emitter, and performing far infrared-vacuum synergistic treatment, wherein the vacuum degree of the treatment environment is 100kPa, and the infrared radiation intensity is 1500-3800W/m 2 The wavelength is 3.2-7.8 mu m, and the infrared radiation time is 6-8 min;
after the radiation is finished, taking out the reactant, respectively washing the reactant for 3 times and 1 time by using distilled water and absolute ethyl alcohol, and removing unreacted citric acid; and then drying the starch in a drying oven at 50 ℃ until the water content is about 8 percent, and grinding the starch through a sieve mesh with 0.075mm meshes to obtain the resistant starch RS 4.
In a preferred embodiment, the mass ratio of citric acid to starch in step (1) is 0.4-0.6: 1, preferably 0.5: 1.
in a preferred embodiment, the step (1) "adjusting the pH to 2.5-3.5" means adjusting the pH of the mixed solution to 2.5-3.5 by using 10mol/L NaOH solution; the pH value is preferably 3.0.
In a preferred embodiment, the standing in step (1) means standing at room temperature (24 to 26 ℃) for at least 16 hours.
In a preferred embodiment, the sieving in step (1) is through a 0.075mm mesh screen.
In a preferred embodiment, the step (2) "uniformly spreading on a stainless steel tray" means that the thickness of the starch crude product spread on the stainless steel tray is 4-10 mm. Preferably 6 to 8mm, and more preferably 7 mm.
In a preferred embodiment, the distance between the far infrared emitter and the tray/crude starch product in step (2) is 25 cm. The far infrared transmitter may use any product conventional in the art, such as MB-EHR12 system manufactured by zhenjiang mebo infrared technologies ltd.
In a preferred embodiment, the intensity of the infrared radiation in step (2) is preferably 3300W/m 2 。
In a preferred embodiment, said infrared irradiation time in step (2) is preferably 6 min.
The application utilizes infrared radiation treatment to affect the multi-scale structure of starch to enhance its tolerance, water absorption, solubility, reduce relative crystallinity, gelatinization parameters. The long chains of the starch molecules can be broken and the particle structure can be destroyed through vacuum treatment, the starch particles can be swelled and gelatinized at a certain temperature along with the increase of the internal pressure of the starch particles, the gelatinization proportion is higher and higher, and most of amylose in the particles is dissolved out to synergistically promote the synthesis of resistant starch.
Compared with the existing preparation method of resistant starch, the preparation method has the following advantages that the infrared radiation is utilized to cooperate with vacuum treatment:
(1) the resistant starch RS4 is prepared by using infrared-vacuum synergistic treatment, so that the starch granules can be broken more easily at higher temperature, and the citric acid can enter the starch molecule granules more favorably, and can generate strong esterification and crosslinking reaction with starch molecules to generate steric hindrance, reduce the action sites of enzyme, and effectively improve the yield of the resistant starch.
(2) The resistant starch RS4 is prepared by using infrared-vacuum synergistic treatment, the dry heat modification effect similar to that of the traditional method can be achieved in a short dry heat treatment time by adopting higher infrared radiation intensity and vacuum degree, the preparation time of the resistant starch is shortened to a greater extent, the preparation process is green and environment-friendly, no three wastes are generated, the electric energy and heat energy consumption is low, the product quality is ensured, the cost is effectively reduced, and the method is easy for commercial application.
(3) After the starch esterification reaction, distilled water and absolute ethyl alcohol are adopted for washing and purifying, so that residual citric acid can be well adsorbed, the product concentration of the starch ester is increased, and the stability of the product is not damaged.
Drawings
FIG. 1 is a perspective view of an infrared-vacuum co-processing apparatus of an embodiment.
FIG. 2 is a perspective view of an infrared-vacuum co-processing apparatus according to an embodiment.
FIG. 3 is a sectional view of an infrared-vacuum co-processing apparatus according to an embodiment.
Wherein, 1 is a vacuum chamber, 2 is a far infrared emitter, 3 is a control cabinet, 4 is a vacuum pump, 5 is a tray, and 6 is a sealing door;
FIG. 4 is a graph showing the change in swelling power of raw corn starch, resistant starch produced by far infrared ray in cooperation with vacuum treatment, and resistant starch produced by conventional dry heat in examples.
FIG. 5 is a graph showing the digestion characteristics of the raw corn starch, the resistant starch produced by far infrared ray in cooperation with vacuum treatment, and the resistant starch produced by conventional dry heat in the examples.
Detailed Description
The present invention will now be further illustrated by reference to the following examples, which are provided for the purpose of illustration and description and are not intended to be limiting. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Example 1
(1) The citric acid solution (50% strength) was mixed with a natural corn starch from Shanghai Town industries, Ltd at a ratio of 0.4: 1 to obtain a citric acid-starch mixed solution;
(2) adjusting the pH value of the citric acid-starch mixed solution obtained in the step (1) to 3.0 by using 10mol/L NaOH solution to obtain a starch crude product;
(3) and (3) uniformly spreading the starch crude product obtained in the step (2) on a stainless steel tray for infrared-vacuum cooperative treatment, wherein the spread thickness of the starch sample is 7mm (in the specific implementation, the thickness of the starch crude product can be selected from the range of 4-10 mm), the distance between a far infrared emitter and the tray (the starch crude product) is 25 cm, and the irradiation wavelength is 3.2 mu m.
(4) The vacuum degree of the processing environment is 100kPa, and the infrared radiation intensity is 3300W/m 2 And the infrared radiation time is 6 min.
(5) After the radiation is finished, taking out the reactant, respectively washing the reactant for 3 times and 1 time by using distilled water and absolute ethyl alcohol, and removing unreacted citric acid; and then the mixture is placed in a drying oven with the temperature of 50 ℃ to be dried until the water content is about 8 percent, and the mixture is ground and sieved to obtain the resistant starch RS 4.
The infrared-vacuum co-processing equipment used in this embodiment has a structure as shown in fig. 1-3, and includes a vacuum chamber 1 having a sealing door 6, a far infrared emitter 2 (purchased from MB-EHR12, mabo infrared technologies, ltd) is disposed at the top of the vacuum chamber 1, a stainless steel tray 5 is further disposed in the vacuum chamber 1, and the tray 5 is fixedly connected to the inner wall of the vacuum chamber 1; the outer wall of the vacuum chamber 1 is provided with a control cabinet 3 corresponding to the far infrared emitter 2; the outer wall of the vacuum chamber 1 is also provided with a vacuum pump 4 (purchased from the company Sifang vacuum equipment, Inc. in Wuxi city) for pumping air, and the vacuum pump 4 is connected with the inner space of the vacuum chamber 1 through an air pumping pipeline. When in use, the sample is flatly paved on the tray 5, the sealing door 6 is closed, the vacuum pump 4 is started to pump air, and the vacuum environment in the vacuum chamber 1 can be maintained; then, the far infrared emitter 2 is opened by using the control cabinet 3, and the experiment can be carried out.
In the specific implementation, the vacuum-infrared cooperative treatment can be realized by utilizing other conventional sealing equipment/environment and combining with a conventional far infrared emitter, so that the aim of the invention is fulfilled.
Comparative examples
Selecting The resistant starch prepared by far infrared cooperative vacuum treatment in The example 1, The traditional dry heat prepared resistant starch (The preparation method is shown in The literature of Wangzhou, Wu Yilong, citric acid sweet potato starch ester preparation process optimization and property research [ J ]. Food science, 2012, 33(24): 86-91.), carrying out a physical and chemical index comparison experiment with natural corn starch, analyzing and researching The expansion force of each starch sample (Mei J Q, Zhou D N, Jin Z Y, et al. Effects of environmental acid discovery on differentiation, structural and physical properties of casasastarc [ J ]. Fochechemistry, 2015,187: 384.) and digestion characteristics (Englyt K N, Englyh N, dson G J, et al. soluble starch in chemical ] and digestion J. conversion of The physical index J., 1999, 69(3): 448-.
As can be seen from FIG. 4, in the measurement temperature range, the swelling force of each starch sample is in an increasing trend, but the amplitudes are different, the swelling force of the natural corn starch is obviously increased, the starch ester prepared by infrared cooperative vacuum treatment and the starch ester prepared by traditional dry heat show weaker swelling water absorption characteristics, but the swelling force of the sample subjected to infrared cooperative vacuum treatment is weaker, mainly because the esterification reaction degree of the sample subjected to infrared cooperative vacuum treatment is higher, and a stronger space cross-linked structure is formed to resist high-temperature damage.
As can be seen from fig. 5, compared with the natural starch, both the infrared cooperative vacuum treatment and the conventional dry heat significantly decrease RDS (rapidly digestible starch) and SDS (slowly digestible starch) in the starch, and the RS (starch with anti-digestion properties) content is significantly increased, but the infrared cooperative vacuum treatment group obtains a higher RS content, which is increased by 5.7% compared with the conventional group, but the preparation time is 2.7% of the conventional dry heat. Therefore, the resistant starch RS4 prepared by infrared cooperative vacuum treatment can effectively improve the industrial production efficiency of RS on the basis of realizing green environmental protection, energy conservation and emission reduction, and has important application value.
Claims (8)
1. A method for preparing resistant starch RS4 by far infrared cooperative vacuum treatment is characterized by comprising the following specific steps:
(1) mixing citric acid solution and corn starch, and adjusting the pH value to 3.0; standing, drying the mixture until the water content is 8%, grinding and sieving to obtain a starch crude product;
(2) uniformly spreading the starch crude product obtained in the step (1) on a tray, wherein the infrared radiation intensity is 3300W/m in a vacuum environment 2 The infrared wavelength is 3.2 mu m, and the infrared radiation time is 6 min;
(3) and after the radiation is finished, washing the reactant by using distilled water and absolute ethyl alcohol respectively, and drying until the water content is 8%, thereby obtaining the resistant starch RS 4.
2. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein the concentration of the citric acid solution in step (1) is 50%.
3. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein the mass ratio of citric acid to corn starch in step (1) is 0.5: 1.
4. the method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment as claimed in claim 1, wherein the step (1) of adjusting the pH to 3.0 is to adjust the pH of the mixed solution to 2.5-3.5 with 10mol/L NaOH solution; the pH value is preferably 3.0.
5. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein the standing in step (1) is at least 16h at 24-26 ℃.
6. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein the sieving in step (1) is 0.075mm mesh sieve.
7. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein in step (2), the uniform spreading on the tray means that the thickness of the starch crude product is 4-10 mm.
8. The method for preparing resistant starch RS4 through far infrared cooperative vacuum treatment according to claim 1, wherein in step (2), the vacuum environment is a vacuum degree of 100 kPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101507563B1 (en) * | 2013-10-15 | 2015-04-08 | 안동대학교 산학협력단 | Production method of indigestible citrate cross-linked starch |
| CN106967177A (en) * | 2017-04-20 | 2017-07-21 | 南昌大学 | Ocentyl succinic wheaten starch ester prepared by a kind of vacuum infrared collaboration processing |
| CN111234042A (en) * | 2020-01-17 | 2020-06-05 | 南京财经大学 | Preparation method of citric acid modified starch with anti-digestion characteristic |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101507563B1 (en) * | 2013-10-15 | 2015-04-08 | 안동대학교 산학협력단 | Production method of indigestible citrate cross-linked starch |
| CN106967177A (en) * | 2017-04-20 | 2017-07-21 | 南昌大学 | Ocentyl succinic wheaten starch ester prepared by a kind of vacuum infrared collaboration processing |
| CN111234042A (en) * | 2020-01-17 | 2020-06-05 | 南京财经大学 | Preparation method of citric acid modified starch with anti-digestion characteristic |
| WO2021143108A1 (en) * | 2020-01-17 | 2021-07-22 | 南京财经大学 | Preparation method for citric acid modified starch with anti-digestive properties |
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