CN115336741A - Processing method for preparing anti-digestion starch through heat treatment and 3D printing - Google Patents

Processing method for preparing anti-digestion starch through heat treatment and 3D printing Download PDF

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CN115336741A
CN115336741A CN202210814604.4A CN202210814604A CN115336741A CN 115336741 A CN115336741 A CN 115336741A CN 202210814604 A CN202210814604 A CN 202210814604A CN 115336741 A CN115336741 A CN 115336741A
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starch
printing
heat treatment
digestion
lipid
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郑波
刘紫鹏
陈玲
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South China University of Technology SCUT
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03—Organic compounds
    • A23L29/035—Organic compounds containing oxygen as heteroatom
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/349—Organic compounds containing oxygen with singly-bound oxygen
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P30/00—Shaping or working of foodstuffs characterised by the process or apparatus
    • A23P30/20—Extruding
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention belongs to the field of food processing, and discloses a processing method for preparing anti-digestion starch by heat treatment in cooperation with 3D printing. The invention selects lipid and polyphenol as double ligands, utilizes heat treatment to cooperate with 3D printing to induce molecular interaction rearrangement to construct a V-shaped crystalline starch compound with high digestion resistance, simultaneously utilizes the antioxidant property of the polyphenol to inhibit the oxidative rancidity of the lipid in the heat processing process, the content of the digestion resistant starch can reach 36.7 percent, and simultaneously oxidation indexes comprising peroxide value, anisidine value and total oxidation value are respectively reduced to 0.2,0.83 and 0.91. The anti-digestion starch prepared by the invention has the advantages of simple preparation method, easy repetition and batch production and the like, and is suitable for industrial application in the food field.

Description

Processing method for preparing anti-digestion starch through heat treatment and 3D printing
Technical Field
The invention belongs to the technical field of food processing, and relates to a processing method for preparing anti-digestion starch through heat treatment in cooperation with 3D printing.
Background
In recent years, with the annual increase of incidence of chronic metabolic diseases related to diet, nutritional and healthy diet has become a demand in the fields of modern food science and nutrition, and researchers of the prior arts find that eating Resistant Starch (RS) can effectively regulate blood sugar and blood lipid metabolism of human bodies, reduce the pH environment of intestinal tracts, and improve the abundance and quantity of beneficial bacteria in intestinal tracts, thereby preventing nutrient imbalance diseases such as obesity, diabetes, cardiovascular and cerebrovascular diseases, metabolic syndrome and the like (Zheng B, wang T, wang H, et al. Wherein, the compound formed between the starch and other food components is induced by the interaction among the components (including hydrogen bond, hydrophobic acting force, van der Waals force, pi-pi conjugation and the like), is a novel anti-digestion starch, and has higher nutritional value. At present, lipid ligand enters the inside of the helical cavity of starch through hydrophobic interaction to form a stable starch lipid complex with enzymolysis resistance, which is a common complex type digestion resistant starch (Krishnan V, mondal D, thomas B, et al starch-lipid interaction indicators and inorganic Biological availability: A complex sensitive viewing. International Journal of Biological Macromolecules,2021, 182), and the main preparation methods thereof comprise steam jet cooking method, screw extrusion method, damp-heat method and the like. Although the thermal processing method can improve the preparation efficiency compared with the common cooking method, strong mechanical shearing and thermal effects are usually accompanied in the process, so that the unsaturated lipid is easily oxidized and rancid, a 'rancid' taste and the generation of some small-molecule harmful substances are generated, and the flavor and the nutritional characteristics of the compound are reduced, so that the problem of lipid oxidation and rancid in the processing process is also concerned while the compound digestion performance is regulated, so as to ensure higher nutritional function. The polyphenol substances as plant-derived active ingredients have various nutritional functions such as blood pressure reduction, cancer resistance and the like, and are gradually used in food processing to enrich the nutritional quality of foods. Studies have shown that polyphenols have a good Antioxidant function, which competitively compete with unsaturated fatty acids for active oxygen by pi-pi conjugation, and at the same time bind lipid oxidative free radicals, converting the free radicals into inert compounds, thereby terminating lipid oxidative chain reactions (Lv Q, long J, gong Z, et al. Current State of Knowledge on the oxidative Effects and Mechanisms of Action of polymeric compounds. Natural Product Communications,2021, 16). Meanwhile, polyphenol can enter a starch spiral cavity through hydrophobic effect to form a V-shaped compound, molecular chain orderly rearrangement is promoted through intermolecular hydrogen bond action, the starch ordering degree is improved, and the digestion resistance of the starch is further effectively improved (Deng N, deng Z, tang C, et al. Formation, structure and properties of the stage-polyphenol inclusion complex: A review. Trends in Food Science & Technology,2021, 112). Therefore, polyphenol molecules can be properly added into a starch and lipid system, so that the system is endowed with higher digestion resistance while lipid oxidation is prevented, and the method has good practical value. At present, the research on the construction of the composite digestion-resistant starch by simultaneously inducing the starch by lipid and polyphenol is not reported for a long time.
Therefore, it is necessary to develop a processing method for improving the anti-digestion performance of starch and inhibiting the oxidative rancidity of lipid during the processing process, so as to create healthy and safe anti-digestion starch.
Disclosure of Invention
The invention aims to provide a processing method for preparing anti-digestion starch by heat treatment in cooperation with 3D printing. According to the invention, the starch-lipid-polyphenol ternary complex is firstly pretreated through heat treatment, and the ternary digestion resistant starch is further prepared by cooperating with a low-temperature 3D printing technology, so that the digestion resistance of the starch is improved, the oxidation rancidity of lipid in the processing process is inhibited, and the healthy and safe digestion resistant starch is prepared.
The invention also aims to provide the digestion-resistant starch prepared by the method.
The specific technical scheme for realizing the purpose of the invention is as follows:
a processing method for preparing anti-digestion starch through heat treatment and 3D printing comprises the following steps:
(1) Heat treatment of ternary mixture: uniformly mixing lipid, polyphenol and starch, and then placing the mixture in an oil bath pan for heat treatment to obtain a heat-treated ternary mixture;
(2) Preparing a printing base material: placing the heat-treated ternary mixture into a three-neck flask containing a certain amount of distilled water, heating in water bath to gelatinize the ternary mixture, and preparing into uniform printing base material under the stirring of a digital display motor
(3) Preparing the digestion-resistant starch at a low temperature by using 3D printing: filling the prepared printing base material into a printer charging barrel for heat preservation, and then printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch.
Preferably, the starch in step (1) is rice starch or wheat starch, the lipid is corn oil, olive oil, oleic acid or linoleic acid, and the polyphenol is resveratrol, caffeic acid or chlorogenic acid;
preferably, the lipid, the polyphenol and the starch in the step (1) are mixed by dissolving 0.3-3.0 parts of the lipid and 0-1.8 parts of the polyphenol in 5 parts of absolute ethyl alcohol, slowly and uniformly spraying the solution to 30 parts of the starch, and simultaneously spraying and stirring the solution to uniformly disperse the solution;
preferably, before the heat treatment in the step (1), the oil bath is preheated to the heat treatment temperature of 90-130 ℃, and is continuously stirred in the heat treatment process to ensure that the mixture is uniformly heated, wherein the heat treatment time is 1-3 hours;
preferably, the concentration of the printing base material in the step (2) is that 20-30 parts of the heat treatment ternary mixture is placed into a three-neck flask containing 100 parts of distilled water according to parts by weight;
preferably, the water bath heating in the step (2) is to preheat a water bath kettle to the gelation temperature of 40-60 ℃ before the preparation of the printing base material, and the water bath heating is carried out for 15-30min under the temperature condition; the stirring is continuously rotating and stirring to ensure that the base material is uniformly heated, wherein the rotating speed of a stirring paddle is 100-180r/min;
preferably, the 3D printing low-temperature preparation in the step (3) is realized by adopting a food hot extrusion 3D printer, and a charging barrel is preheated to a set printing temperature of 35-55 ℃ in advance before printing and is kept warm for 1-5min;
preferably, the 3D printing low-temperature preparation in the step (3) has the printing parameters of 0.7mm of nozzle height, 0.4-1.0mm of nozzle diameter, 60mm/s of printing speed, 60mm/s of drawing speed and 1.8mm of drawing distance.
A digestion resistant starch prepared by the above method.
The invention mechanism of the invention:
the dry heat treatment is used as a common food processing method, is simple to operate, can destroy the structure of starch granules through heat energy, enables partial inner molecular chains to be broken, and induces the starch molecular ordered rearrangement and the interaction with other components to construct an ordered structure in the water molecule migration process; and the hot extrusion 3D printing induces molecular interaction rearrangement through nozzle shearing and layer-by-layer deposition to form a compact and ordered spatial structure and endow the spatial structure with personalized appearance. This patent constructs a processing method that heat treatment cooperates with 3D to print preparation anti digestion starch, and this processing method utilizes the original granular structure of dry heat preliminary treatment destruction starch to promote the interact of starch and lipid and polyphenol, through the low temperature 3D on this basis and print the interact between the reinforcing component, further improve inside ordered structure, and then improve starch complex's anti digestion performance. Meanwhile, the oxidative rancidity of lipid in the processing process can be inhibited based on the interaction between the starch, the lipid and the polyphenol, and the healthy and safe digestion-resistant starch is prepared.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) Compared with the traditional preparation of a starch-lipid compound, the starch-lipid-polyphenol ternary compound has better digestion resistance and oxidation resistance, the digestion resistance RS and SDS respectively reach 36.7 percent and 9.2 percent, and the oxidation indexes including peroxide value, anisidine value and total oxidation value are respectively reduced to 0.2,0.83 and 0.91.
(2) Compared with the traditional preparation of the starch-lipid complex, the novel ternary starch complex is constructed by using the lipid and the polyphenol as double ligands, and the introduction of the polyphenol can compete for active oxygen through pi-pi conjugation, and simultaneously is converted into an inert compound by combining with lipid oxidation free radicals, so that the chain reaction of lipid oxidation rancidity is stopped, the peroxide value, the anisidine value and the total oxidation value of the complex are reduced, and the safety of the starch complex is improved.
(3) The digestion-resistant starch is prepared by heat treatment in cooperation with a low-temperature 3D printing technology, wherein the heat treatment enables starch granules to be cracked, molecular chains to be partially cracked, and at the moment, lipid and polyphenol permeate into the starch granules under the action of heat effect, particularly the lipid, and interact with the molecular chains to form a partial compound; the low-temperature 3D printing mainly utilizes the migration behavior of water molecules to destroy the amorphous area of the starch particles, the original ordered structure of the starch is well kept, and the released molecular chains generate molecular interaction with lipid and polyphenol in the system under the inducing action of 3D printing shearing and deposition to form an ordered V-shaped crystalline structure, so that the digestion resistance of the starch is improved.
(4) The anti-digestion starch prepared by the invention has the advantages of simple preparation method, easy repetition and batch production and the like, has more abundant nutritional functions, and is suitable for industrial application in the food field.
Drawings
FIG. 1 is an SEM photograph of raw rice starch, examples 1 and 6 and comparative examples 1 and 2 after heat treatment.
Figure 2 is an XRD pattern of example 1, 6 and comparative example 1, 2 prepared from raw rice starch, heat treatment in conjunction with 3D printing.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The materials, reagents, equipment and the like used in the present invention can be directly purchased from the market without specific description.
Example 1
Step 1: uniformly mixing 2.4 parts of oleic acid, 0.3 part of chlorogenic acid and 30 parts of rice starch in parts by weight, and then placing the mixture in an oil bath pan to perform heat treatment for 120min at the temperature of 120 ℃ to obtain a heat treatment ternary mixture;
step 2: placing 25 parts of the heat treatment ternary mixture into a three-neck flask containing 100 parts of distilled water by mass, heating the mixture in a water bath for 20min at 50 ℃ to gelatinize the mixture, and preparing a uniform printing base material under the stirring of a digital display motor at the rotating speed of 120r/min;
and step 3: filling the prepared mixture printing base material into a printer charging barrel, preserving heat for 5min at the temperature of 50 ℃, and printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch (anti-digestion starch 1), wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
example 2
This example differs from example 1 in that rice starch was replaced with wheat starch in step 1 to prepare a digestion resistant starch (digestion resistant starch 2).
Example 3
This example differs from example 1 in that oleic acid was replaced with corn oil in step 1 to produce a digestion resistant starch (digestion resistant starch 3).
Example 4
This example differs from example 1 in that chlorogenic acid was replaced with resveratrol in step 1 to prepare a resistant starch (resistant starch 4).
Example 5
This example differs from example 1 in that the amount of oleic acid added in step 1 was changed from 2.4 parts to 0.6 part to prepare a digestion-resistant starch (digestion-resistant starch 5).
Example 6
This example differs from example 1 in that 1.5 parts of chlorogenic acid were replaced from 0.3 in step 1 to prepare a resistant starch (resistant starch 6).
Example 7
This example differs from example 1 in that the heat treatment temperature in step 1 was changed from 120 ℃ to 130 ℃ to prepare resistant starch (resistant starch 7).
Example 8
This example differs from example 1 in that the heat treatment time in step 1 was changed from 2h to 3h to prepare a resistant starch (resistant starch 8).
Example 9
This example differs from example 1 in that the temperature of the water bath in step 2 was changed from 50 ℃ to 60 ℃ to prepare a resistant starch (resistant starch 9).
Example 10
This example differs from example 1 in that the mixture content in step 2 was changed from 25 parts to 20 parts to prepare a digestion-resistant starch (digestion-resistant starch 10).
Example 11
This example differs from example 1 in that the rotation speed was changed from 120r/min to 180r/min in step 2, and a digestion-resistant starch (digestion-resistant starch 11) was prepared.
Example 12
This example differs from example 1 in that the printing temperature was changed from 50 ℃ to 40 ℃ in step 3 to prepare a digestion-resistant starch (digestion-resistant starch 12).
Example 13
This example differs from example 1 in that the nozzle diameter was changed from 0.6mm to 1.0mm in step 3, and resistant starch (resistant starch 13) was prepared.
Comparative example 1
(1) According to the mass parts, 30 parts of rice starch is placed in an oil bath pan to be subjected to heat treatment for 120min at the temperature of 120 ℃, so that the heat-treated rice starch is obtained; (2) Placing 25 parts of heat-treated rice starch in a three-neck flask containing 100 parts of distilled water, heating in water bath at 50 deg.C for 20min to gelatinize, and stirring with a digital display motor to obtain uniform printing base material at a rotation speed of 120r/min; (3) Placing the prepared base material in a printer charging barrel, keeping the temperature at 50 ℃ for 5min, and performing printing preparation by using a food hot extrusion 3D printer, wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
comparative example 2
(1) Uniformly mixing 2.4 parts of oleic acid and 30 parts of rice starch in parts by weight, and then placing the mixture in an oil bath pan to perform heat treatment for 120min at the temperature of 120 ℃ to obtain a heat treatment binary mixture; (2) Placing 25 parts of the heat-treated mixture into a three-neck flask containing 100 parts of distilled water, heating in a water bath at 50 ℃ for 20min to gelatinize the mixture, and preparing a uniform printing base material under the stirring of a digital display motor at the rotating speed of 120r/min; (3) Placing the prepared base material in a printer charging barrel, keeping the temperature at 50 ℃ for 5min, and printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch, wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
comparative example 3
This comparative example differs from comparative example 2 in that oleic acid in step 1 was replaced with corn oil;
comparative example 4
(1) Uniformly mixing 2.4 parts of oleic acid, 0.3 part of chlorogenic acid and 30 parts of rice starch in parts by weight, and then placing the mixture in an oil bath pan to perform heat treatment for 120min at the temperature of 120 ℃ to obtain a heat treatment ternary mixture; (2) Placing 25 parts of the heat-treated mixture into a printing material cylinder filled with 100 parts of distilled water, and printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch, wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
comparative example 5
(1) Uniformly mixing 2.4 parts of oleic acid, 0.3 part of chlorogenic acid and 30 parts of rice starch in parts by weight, and then placing the mixture in an oil bath pan to perform heat treatment for 120min at the temperature of 120 ℃ to obtain a heat treatment ternary mixture; (2) Placing 25 parts of the heat-treated mixture into a three-neck flask containing 100 parts of distilled water, heating the mixture in a water bath at a high temperature of 95 ℃ to gelatinize the mixture, and preparing the mixture into a uniform printing base material under the stirring of a digital display motor; (3) Placing the prepared base material in a printer charging barrel, keeping the temperature at 70 ℃ for 5min, and printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch, wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
comparative example 6
(1) Uniformly mixing 2.4 parts of oleic acid, 0.3 part of chlorogenic acid and 30 parts of rice starch in parts by weight, and then placing the mixture in an oil bath pan to perform heat treatment for 120min at the temperature of 120 ℃ to obtain a heat treatment ternary mixture; (2) Placing 25 parts of the heat-treated mixture into a three-neck flask containing 100 parts of distilled water, heating in a water bath at 50 ℃ for 20min to gelatinize the mixture, and preparing a uniform printing base material under the stirring of a digital display motor at the rotating speed of 120r/min; (3) Placing the prepared base material in a printer charging barrel, keeping the temperature at 70 ℃ for 5min, and printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch, wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.6mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm;
according to the invention, the above examples are characterized by SEM and XRD, and the digestion performance and oxidation index of the digestion-resistant starch prepared in the examples and comparative examples are measured, specifically as follows:
(1) Morphology of the particles
Coating the starch and starch compound particles after heat treatment on a sample table adhered with a conductive double-sided adhesive tape, and blowing away redundant particles by an aurilave to ensure that the particles are at the same focusing level; placing the sample stage in an ion sputtering coating apparatus for plating gold for 5min, and selecting 4.0 × 10 under 20kV voltage 3 And observing and photographing at a magnification.
(2) Crystalline structure
Freeze-drying the starch and the starch compound prepared by the heat treatment and the 3D printing, and then crushing and screening (200 meshes); compacting the sieved sample powder, placing the compacted sample powder in an XRD sample table, and continuously scanning by selecting the step size of 0.0165 degrees under the conditions of tube pressure of 40kV and tube flow of 40mA by adopting monochromatic Cu-Kalpha rays with the wavelength of 0.1542nm, wherein the scanning range is 5-40 degrees.
(3) Oxidation index test
The method for measuring the oxidation characteristic index of the embodiment of the invention refers to national standards GB 5009.227-2016 and GB/T24304-2009, including peroxide value, anisidine value and total oxidation value.
(4) Digestion Performance test
The digestion property determination method of the embodiment of the invention comprises the following steps: the contents of fast-digestible starch (RDS), slow-digestible starch (SDS) and Resistant Starch (RS) were analysed using the enzymes from Sigma (porcine pancreatic alpha-amylase: P-7545 and amyloglucosidase: A-3360) with reference to the procedure proposed by Englyst.
And (3) measuring results:
FIG. 1 is SEM images of raw rice starch, heat-treated examples 1 and 6 and comparative examples 1 and 2, and it can be seen that the surface of the granules becomes uneven after the heat treatment of the starch due to the moisture migration and the melt-swelling destruction of amorphous regions during the heat treatment, resulting in irregular changes in the appearance and morphology; with the addition of lipid and polyphenol, the irregularity of the appearance and the appearance of a large number of pits is increased, which shows that the original particle appearance is damaged as the lipid and the polyphenol migrate to the amorphous region of the starch under the action of heat energy and are compounded with the starch.
FIG. 2 is XRD patterns of original rice starch, heat treatment cooperated with 3D printing, examples 1 and 6 and comparative examples 1 and 2, which shows that the original A-type crystallization characteristic peak of the original rice starch disappears after processing treatment, and no other new characteristic peak is formed, thus showing a larger dispersion peak; with the addition of the lipid polyphenol, the starch molecular chain and the lipid polyphenol are subjected to hydrophobic compounding to form an ordered V-shaped crystal structure, and obvious crystallization characteristic peaks appear at 13.6 degrees and 20.1 degrees. With the increase of the addition amount of the lipid polyphenol, the crystallization characteristic peak is more obvious, which indicates that the crystallinity of the sample is increased.
Table 1 shows the oxidation index and digestion performance of the different examples and comparative examples. As can be seen from the table, the oxidation indexes of the examples are significantly reduced and the digestion resistance thereof is significantly increased compared to the comparative examples 1 to 3, wherein the digestion resistant starch RS of example 6 is as high as 36.7%, and the oxidation indexes including the peroxide value, the anisidine value and the total oxidation value are reduced to 0.2,0.83 and 0.91, respectively. Comparative examples 4 to 6 found that when the heat-treated ternary complex was not subjected to gelation, the starch thereof maintained a granular state and failed to successfully form a gel network structure, resulting in failure of 3D printing; when the gelatinization temperature or printing temperature is too high and the starch is in a completely gelatinized state, the oxidation index and the digestion resistance of the starch are reduced along with the aggravation of lipid oxidation and the disintegration of the original ordered structure. From example 2, it can be seen that rice starch has a relatively strong complexing power during thermal processing compared to wheat starch, since rice starch granules are smaller and can better interact with lipid polyphenols during processing, thereby improving the starch's resistance to digestion. As can be seen from example 3, oleic acid is more susceptible to oxidative rancidity than corn oil during thermal processing, but its complexing ability is relatively strong and starch digestion resistance is improved. As can be seen from example 4, resveratrol has a weaker antioxidant capacity and complexing capacity than chlorogenic acid. From example 5, it is clear that the digestion resistance is increased with increasing addition of oleic acid, but at the same time with a more severe oxidative rancidity. From examples 6-8, 10 and 11, it can be seen that as the temperature increases during the processing, the heating treatment time increases, the stirring speed increases, the lipid will be in contact with oxygen more sufficiently, and further more serious oxidation occurs, and the original ordered structure of the starch is further destroyed, resulting in a decrease in the digestion resistance. From examples 10 and 13, it can be seen that as the concentration of the printing base material increases, the diameter of the nozzle decreases, the shear-induced starch lipid polyphenol molecular interaction rearrangement effect during 3D printing is more obvious, and the formed compound has stronger digestion resistance.
As can be seen from the results of the above examples and comparative examples, the starch and starch lipid complex has the disadvantages of low digestion resistance and severe oxidative rancidity after being subjected to heat treatment and 3D printing treatment; due to the addition of the polyphenol, the digestion resistance of the starch-lipid-polyphenol ternary system compound is obviously improved, and the polyphenol has an obvious inhibiting effect on the oxidative rancidity of the lipid. Compared with the traditional starch lipid complex, the ternary starch complex has lower oxidative rancidity degree and better digestion resistance.
TABLE 1 Oxidation index and digestion Performance of examples and comparative examples
Figure BDA0003741800470000111
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. It will be apparent to those skilled in the art that various equivalent substitutions and obvious modifications can be made without departing from the spirit of the invention, and all changes that come within the meaning and range of equivalency of the claims are to be embraced within their scope.

Claims (9)

1. The processing method for preparing the digestion-resistant starch through heat treatment and 3D printing is characterized by comprising the following steps of:
(1) Heat treatment of ternary mixture: uniformly mixing lipid, polyphenol and starch, and then placing the mixture in an oil bath pan for heat treatment to obtain a heat-treated ternary mixture;
(2) Preparation of printing base material: placing the heat-treated ternary mixture into a three-neck flask containing a certain amount of distilled water, heating in water bath to gelatinize the ternary mixture, and preparing a uniform printing base material under the stirring of a digital display motor;
(3) Preparing the anti-digestion starch by 3D printing at low temperature: filling the prepared printing base material into a printer charging barrel for heat preservation, and then printing by using a food hot extrusion 3D printer to prepare the anti-digestion starch.
2. The method of claim 1, wherein: the starch in the step (1) is rice starch or wheat starch, the lipid is corn oil, olive oil, oleic acid or linoleic acid, and the polyphenol is resveratrol, caffeic acid or chlorogenic acid.
3. The method of claim 1, wherein: the lipid, polyphenol and starch in the step (1) are mixed by dissolving 0.6-2.4 parts of lipid and 0.3-1.5 parts of polyphenol in 5 parts of absolute ethyl alcohol, slowly and uniformly spraying the solution into 30 parts of starch, and stirring while spraying to uniformly disperse the solution.
4. The method of claim 1, wherein: preheating the oil bath to the heat treatment temperature of 90-130 ℃ before the heat treatment in the step (1), and continuously rotating and stirring in the heat treatment process to ensure that the mixture is uniformly heated, wherein the heat treatment time is 1-3h.
5. The method of claim 1, wherein: and (3) the concentration of the printing base material in the step (2) is that 20-30 parts of the heat treatment ternary mixture is placed into a three-neck flask filled with 100 parts of distilled water according to parts by weight.
6. The method of claim 1, wherein: preheating a water bath kettle to the gelation temperature of 40-60 ℃ before preparing the printing base material in the step (2), and heating in water bath for 15-30min under the temperature condition; the stirring is continuously rotating stirring to ensure that the base material is uniformly heated, wherein the rotating speed of a stirring paddle is 100-180r/min.
7. The method of claim 1, wherein: and (3) adopting a food hot extrusion 3D printer for printing preparation, preheating a charging barrel to a set printing temperature of 35-55 ℃ in advance before printing, and keeping the temperature for 1-5min.
8. The production method according to claim 1, characterized in that: and (4) preparing the 3D printing at low temperature in the step (3), wherein the printing parameters are that the height of a nozzle is 0.7mm, the diameter of the nozzle is 0.4-1.0mm, the printing speed is 60mm/s, the pumping speed is 60mm/s, and the pumping distance is 1.8mm.
9. A digestion resistant starch produced by the method of any one of claims 1 to 8.
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