CN115677866A - Preparation method of granular starch-lipid compound - Google Patents
Preparation method of granular starch-lipid compound Download PDFInfo
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- CN115677866A CN115677866A CN202211384102.9A CN202211384102A CN115677866A CN 115677866 A CN115677866 A CN 115677866A CN 202211384102 A CN202211384102 A CN 202211384102A CN 115677866 A CN115677866 A CN 115677866A
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Abstract
The invention relates to the technical field of starch modification, in particular to a preparation method of granular starch-lipid compound, which comprises the steps of firstly carrying out irradiation treatment on starch granules by adopting gamma-rays, then using a hydrothermal method technology as a matched process, and compounding the irradiated starch granules with lipid to prepare the granular starch-lipid compound.
Description
Technical Field
The invention relates to the technical field of starch modification, and in particular relates to a preparation method of a granular starch-lipid compound.
Background
The starch-lipid complex is an important starch derivative, in the process of forming the starch-lipid complex, a fat chain of lipid can be stabilized in the helical cavity of amylose through hydrogen bonds, hydrophobic interaction, van der waals force and the like, and a hydrophilic group of the lipid is exposed outside the helix due to steric hindrance and electrostatic repulsion, so that gelatinization, aging, enzymatic hydrolysis, freeze-thaw stability and the like of the starch can be influenced, and the starch-lipid complex has beneficial influence on the texture characteristics, nutritional quality and the like of food; in addition, the starch-lipid complex can be used for embedding unstable bioactive substances or flavor substances, and has important application prospects in the fields of medicines, health-care foods, films and the like.
The sustainable development of the starch and deep processing industry is highly concerned by the industry. Because the starch-lipid complex has wide application prospect, the artificial synthesis of the starch-lipid complex becomes a current research hotspot. However, most of the current domestic and overseas synthetic studies usually use pure amylose, debranched starch or gelatinized starch to prepare the compound, and these methods need irritant chemical reagents and higher reaction temperature, or have long time consumption and high cost, and are not beneficial to industrial production, so that a new process for producing the efficient and green starch-lipid compound is urgently needed to be developed.
In recent years, granular starch-lipid complexes have been studied, which do not require the isolation of amylose or the preparation of debranched starch/starch pastes, in which starch granules are subjected to a complex reaction with lipids in the swollen state, and the product is subjected to suitable recovery and drying treatments to form granular starch-lipid complexes; at present, there are two main methods for preparing granular starch-lipid complexes in laboratories, the first preparation method requires that starch is pretreated, and the pretreated starch still retains the granular form but has changed physicochemical properties and is different from starch granules of the original starch, so that the first preparation method firstly prepares granular starch, and utilizes the characteristic that the granular starch is soluble in cold water to be compounded with lipid at a lower temperature (20-60 ℃) to form complexes, which is suitable for various lipids, especially suitable for embedding some heat-sensitive vitamins, antioxidants and the like, but the preparation of granular starch is usually relatively complex, and the common methods for preparing granular starch include spray drying, saturated monohydric alcohol, polyhydric alcohol, alcohol-alkaline method, ball milling method or alcohol-alkaline method combined with other methods, which generally have higher requirements on equipment (spray drying, saturated monohydric alcohol, polyhydric alcohol, ball milling method), and/or complex methods using a large amount of reagents and/or alcohols (saturated monohydric alcohol, polyhydric alcohol-enzymatic method, enzyme method combined with polyhydric alcohol, and ultrasonic method combined with alkaline method, and pure alcohol method); the second preparation method comprises the following steps: the starch is heated for a period of time under the condition of slightly lower than the gelatinization temperature (generally 80-90 ℃) by utilizing the traditional hydrothermal method to swell the starch, and then lipid is added for complex reaction.
The starch is divided into cereal starch, rhizome starch, bean starch and other starch according to raw material sources, wherein the corn starch of the cereal is the starch with the largest proportion of the starch yield in China, and is the starch frequently used for researching the starch-lipid compound. Ascorbyl Palmitate (AP), an esterification product of palmitic acid and ascorbic acid, is an important antioxidant and is a representative lipid commonly used in the study of starch-lipid complexes. The starch-ascorbyl palmitate complex is prepared by the first preparation method described above, namely: the starch needs to be pretreated and then undergoes a complex reaction with the AP at a lower temperature (20-70 ℃), the pretreatment methods usually require irritant chemical reagents such as NaOH and DMSO, or require a large amount of ethanol solution and a high temperature condition, and the recovered and dried starch, amylose or granular starch reacts with the AP, so that the operation is relatively complex, and the industrial production and application of the starch-AP complex are limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a granular starch-lipid complex, which overcomes the technical problems that the prior preparation method of the starch-lipid complex needs irritant chemical reagents such as NaOH and DMSO for pretreating starch, needs a large amount of ethanol solution and high-temperature conditions, is relatively complex to operate and has low complex preparation efficiency.
In order to solve the technical problem, the invention adopts the following technical scheme:
a granular starch-lipid composition is prepared by irradiating starch granules with gamma-ray, and preparing granular starch-lipid composition by hydrothermal method.
Preferably, the starch granules comprise rhizome starch, cereal starch and bean starch, and the types of the starch are referred to GB/T8887-2021 starch Classification.
Preferably, the root starch comprises potato starch, tapioca starch, sweet potato starch and yam starch, the cereal starch comprises corn starch, wheat starch, buckwheat starch, rice starch and glutinous rice starch, and the bean starch comprises pea starch, mung bean starch and red bean starch.
Preferably, the lipid comprises free fatty acids, fatty acid derivatives, phospholipids.
Preferably, the free fatty acids include palmitic acid, lauric acid, myristic acid, stearic acid, caprylic acid, caproic acid, capric acid, oleic acid, butyric acid, linoleic acid, linolenic acid, arachidonic acid; the derivatives of the fatty acids include ascorbyl palmitate, retinol ester, phytosterol ester, glycerol monostearate, and the like; the phospholipid material includes lecithin, lysophospholipid, etc.
Preferably, the irradiation method of the starch granules comprises the following steps: putting a silver dichromate dosimeter into starch granules, and sampling the starch granules by adopting 60 Co-gamma ray irradiation by gravityThe silver chromate dosimeter measures the actual absorbed dose of the sample.
Preferably, the irradiation dose of the starch granules is 1-10kGy.
Preferably, the granular starch-lipid complex is prepared according to the following steps:
s1, dissolving the irradiated starch granules in water to prepare starch milk with the mass fraction of 6-10%, and stirring for 0.5-1.5h in water bath at 50-70 ℃ to obtain expanded starch milk;
s2, preparing lipid into an absolute ethyl alcohol lipid solution, adding the absolute ethyl alcohol lipid solution into the swollen starch milk obtained in the step S1, continuously heating and stirring for 1-2 hours, then cooling to room temperature, centrifuging, washing and drying to obtain the granular starch-lipid complex.
Preferably, the mass ratio of the lipid to the starch granules after irradiation in the step S2 is 1-15:100, the volume ratio of lipid to absolute ethyl alcohol is 5-10 g.
Preferably, the centrifugation, washing and drying method in step S2 is: centrifuging at 3000-4000g for 15-20min, washing with 50% ethanol solution, washing with anhydrous ethanol, vacuum filtering, drying at 30-50 deg.C overnight, pulverizing, and sieving with 100-150 mesh sieve.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, after the starch granules are irradiated by gamma-rays with a certain dose, the granular starch-lipid compound is prepared by a hydrothermal method, and the irradiation has a certain degradation effect on starch chains, so that the content of lipid in the compound product can be effectively improved, and in addition, the irradiation can increase the viscosity peak of the viscosity curve of the compound in the cooling stage; with the increase of the irradiation dose, the expansion degree, the relative crystallinity and the thermal stability of the compound are gradually increased, and the oxidation resistance is firstly reduced and then increased.
2. In all the compounds, when the irradiation dose of the starch is 10kGy, the compound product has relatively high compound efficiency, the swelling degree and the relative crystallinity are the maximum, and the shearing resistance, the oxidation resistance and the thermal stability are the strongest.
3. After the starch is irradiated, amylose and amylopectin are degraded, the degree of polymerization (chain length) of the starch is reduced, the swelling degree and the solubility of the starch in a certain temperature range are increased, and the swelling degree and the solubility are increased, so that lipid molecules can enter the starch granules or can perform composite reaction with amylose molecules outside the starch granules; the degradation of amylopectin reduces its hindering effect on amylose and lipid complexation; meanwhile, the reduction of the chain length of the amylose (within a certain degree of polymerization) is also beneficial to forming an ordered V-shaped crystal structure and enhancing the stability of the amylose-lipid complex; and the result shows that compared with the preparation method of the starch-ascorbyl palmitate in the prior art, the method overcomes the technical defects that the pretreatment of the prior preparation method needs stimulating chemical reagents such as NaOH and DMSO, a large amount of ethanol solution is needed, the high temperature condition is needed, and the operation is relatively complicated.
4. The irradiation technology is a green, low-carbon and non-thermal processing high and new technology, irradiated food is safe and harmless, starch is subjected to ray irradiation and then subjected to degradation reaction to cause breakage of starch chains, the degree of polymerization is reduced, the gelatinization characteristic, the expansion characteristic, the apparent amylose content, the crystal structure and the like of the starch are possibly influenced, the structure is damaged after the starch is irradiated, water molecules can easily permeate into starch granules, the starch is promoted to expand in hot water, the amylose is easily dissolved out, and the characteristic is favorable for promoting the complex reaction of the amylose and lipid; meanwhile, the degradation of the amylopectin weakens the interference of the amylopectin on the amylose and lipid complex, so that the preparation of the granular starch-lipid complex by combining the irradiation and the hydrothermal method is theoretically feasible, and the method is favorable for developing a new green and efficient production technology of the granular starch-lipid complex.
5. Compared with non-granular starch-lipid complexes, the granular starch-lipid complexes prepared by the invention do not need to separate amylose or prepare debranched starch and starch paste, the starch granules and the lipid undergo a complex reaction in an expanded state, and the products are appropriately recovered and dried.
Drawings
FIG. 1 is a sample morphology of examples 1-4 and comparative example 1; a1, B1, C1, D1 and E1 are respectively starch samples after C0, C1, C2.5, C5 and C10 irradiation, A2, B2, C2, D2 and E2 are respectively starch-lipid complex samples in granular state of C-AP0, C-AP1, C-AP2.5, C-AP5 and C-AP10, and the scale in the figure is 20 mu m;
FIG. 2 is a graph of the composite efficiency results for the samples of examples 1-4 and comparative example 1;
FIG. 3 is a graph of the overrun curves of the samples of examples 1-4 and comparative example 1;
FIG. 4 is a graph showing the results of gelatinization feature tests of samples of examples 1 to 4 and comparative example 1, wherein A is a graph showing the results of gelatinization feature tests of starch samples after C0, C1, C2.5, C5 and C10 irradiation, and B is a graph showing the results of gelatinization feature tests of starch-lipid complex samples in granular state of C-AP0, C-AP1, C-AP2.5, C-AP5 and C-AP 10;
FIG. 5 is an X-ray diffraction pattern of samples of examples 1 to 4 and comparative example 1, wherein A is an X-ray diffraction pattern of C0, C1, C2.5, C5 and C10 starch samples after irradiation; and the B picture is an X-ray diffraction pattern of C-AP0, C-AP1, C-AP2.5, C-AP5 and C-AP10 samples.
Detailed Description
The embodiments of the present invention will be described in detail with reference to the accompanying drawings, which are intended to be illustrative, not limiting, and not limiting.
The starch granules and lipids selected in examples 1-4 and comparative example 1 below were selected from corn starch and ascorbyl palmitate, respectively.
Example 1
The preparation method of the granular corn starch-ascorbyl palmitate complex comprises the following steps:
(1) Weighing 100g of starch, sealing the starch in a self-sealing bag, selecting 3 parallel samples for each irradiation dose, putting 3 silver dichromate dosimeters into each sample for measuring the actual absorbed dose of the sample, and placing the subpackaged samples in 60 Performing irradiation treatment in a Co-gamma irradiation device, wherein the irradiation dose is set to be 10kGy, the average irradiation dose rate is 0.55kGy/h, the sample after irradiation is named as C10, and the sample is irradiated completelyPlacing the mixture in a refrigerator at 4 ℃ for later use;
(2) Weighing 30g of starch (dry basis) from the sample C10 irradiated in the step (1), mixing with distilled water to prepare 8% of starch milk, and stirring in a water bath at 65 ℃ for 1h to obtain expanded starch milk;
(3) Preparing 1.5g of ascorbyl palmitate into 10% ascorbyl palmitate-absolute ethanol solution, slowly adding the 10% ascorbyl palmitate-absolute ethanol solution into the expanded starch milk obtained in the step (2), continuously heating and stirring for 1h, cooling to 20 ℃ after the reaction is finished, centrifuging for 15min under 3000g of centrifugal force, repeatedly centrifuging and washing for three times by using 50% ethanol solution in volume fraction, finally washing and precipitating by using absolute ethanol, carrying out suction filtration, drying overnight at 40 ℃, crushing, and sieving by using a 120-mesh sieve to obtain a granular corn starch-ascorbyl palmitate compound which is named as C-AP10.
Example 2
The same procedure as in example 1 was followed, except that the irradiation dose was changed from 10kGy to 1kG, the starch after irradiation was designated C1, and the sample C1 was complexed with ascorbyl palmitate to give a granular corn starch-ascorbyl palmitate complex designated C-AP1.
Example 3
The same procedure as in example 1 was followed, except that the irradiation dose was changed from 10kGy to 2.5kGy, the starch after irradiation was named C2.5, and the sample C2.5 was used to complex with ascorbyl palmitate, to obtain a granular corn starch-ascorbyl palmitate complex named C-AP2.5.
Example 4
The same procedure as in example 1 was followed, except that the irradiation dose was changed from 10kGy to 5kGy, the starch after irradiation was designated C5, and the sample C5 was used to complex with ascorbyl palmitate, to obtain a granular corn starch-ascorbyl palmitate complex designated C-AP5.
Example 5
The preparation method of the granular potato starch-glyceryl monostearate compound comprises the following steps:
(1) Weighing 100g of potato starch, sealing the potato starch in a self-sealing bag, selecting 3 parallel samples for each irradiation dose, putting 3 silver dichromate dosimeters into each sample for measuring the actual absorbed dose of the sample, and putting the subpackaged samples into a self-sealing bag 60 Carrying out irradiation treatment in a Co-gamma irradiation device, setting the irradiation dose to be 5kGy, setting the average irradiation dose rate to be 0.55kGy, and placing the sample in a refrigerator at 4 ℃ for later use after the irradiation is finished;
(2) Weighing 50g of starch (dry basis) from the sample irradiated in the step (1), mixing with distilled water to prepare starch milk with the mass fraction of 6%, and stirring in a water bath at 50 ℃ for 0.5h to obtain expanded starch milk;
(3) Preparing 0.5g of glyceryl monostearate into a glyceryl monostearate-absolute ethyl alcohol solution with the mass concentration of 8%, slowly adding the solution into the expanded starch milk obtained in the step (2), continuously heating and stirring for 1h, cooling to 20 ℃ after the reaction is finished, centrifuging for 17min under 3500g of centrifugal force, repeatedly centrifuging and washing for three times by using an ethyl alcohol solution with the volume fraction of 50%, finally washing and precipitating by using absolute ethyl alcohol, carrying out suction filtration, drying overnight at 30 ℃, crushing, and sieving by using a 100-mesh sieve to obtain the granular potato starch-glyceryl monostearate compound.
Example 6
The preparation method of the granular cassava starch-lysophospholipid complex comprises the following steps:
(1) Weighing 100g of cassava starch, sealing the cassava starch in a self-sealing bag, selecting 3 parallel samples for each irradiation dose, putting 3 silver dichromate dosimeters into each sample for determining the actual absorbed dose of the sample, and placing the subpackaged samples in 60 Carrying out irradiation treatment in a Co-gamma irradiation device, wherein the irradiation dose is set to be 2.5kGy, the average irradiation dose rate is 0.55kGy, and the sample is placed in a refrigerator at 4 ℃ for later use after the irradiation is finished;
(2) Weighing 20g of starch (dry basis) from the sample C1 irradiated in the step (1), mixing with distilled water to prepare starch milk with the mass fraction of 10%, and stirring in a water bath at 70 ℃ for 1.5h to obtain expanded starch milk;
(3) Preparing 3g of lysophospholipid into a lysophospholipid-absolute ethanol solution with the mass concentration of 5%, slowly adding the solution into the expanded starch milk obtained in the step (2), continuously heating and stirring for 1h, cooling to 20 ℃ after the reaction is finished, centrifuging for 20min under the centrifugal force of 4000g, repeatedly centrifuging and washing for three times by using an ethanol solution with the volume fraction of 50%, finally washing and precipitating by using absolute ethanol, carrying out suction filtration, drying at 50 ℃ overnight, crushing, and sieving by using a 150-mesh sieve to obtain the granular cassava starch-lysophospholipid composite.
Comparative example 1
The same procedure as in example 1 was followed, except that the irradiation dose was changed from 1kGy to 0kGy, that is, irradiation treatment was not performed, the sample after irradiation was designated as C0, and the sample C0 was then complexed with ascorbyl palmitate to give a granular corn starch-ascorbyl palmitate complex designated as C-AP0.
The measuring method comprises the following steps:
(1) Morphology determination of granular corn starch-ascorbyl palmitate complex
Taking 2mg of granular corn starch-ascorbyl palmitate complex samples, suspending the samples in 1mL of 30 vol% glycerol solution, adding 10 mu L of 0.1mol/L iodine solution, dyeing for 5min, and observing the forms of the granular corn starch-ascorbyl palmitate complexes of the samples of examples 1-4 and comparative example 1 by using an Olympus BX53 biomicroscope.
(2) Content determination of ascorbyl palmitate
Accurately weighing 50mg of granular corn starch-ascorbyl palmitate compound sample, adding 5mL of distilled water, 1mL of concentrated hydrochloric acid and 3% citric acid (starch base) by mass fraction, carrying out water bath at 70 ℃ for 50min, adding 10.5mL1MNaOH solution to adjust the pH to 6.0, and then adding absolute ethyl alcohol to reach 50mL of constant volume. The absorbance of the solution at 247nm was measured by an ultraviolet spectrophotometer. Preparing a proper amount of AP standard substance into 1.25mg/mL standard solution, respectively replacing the starch sample with 2mL, 1mL, 0.5mL, 0.25mL and 0.125mL standard solution, establishing a standard curve, and determining the content of AP.
AP content (%) = mass of AP/dry weight of starch sample × 100
Embedding rate (%) = mass of embedded AP/amount of added AP × 100
AP content (%) refers to the mass of AP bound per gram of starch in the complex, expressed as a percentage;
the entrapment (%) refers to the ratio of the mass of AP finally bound in the composite to the total AP content added during the preparation of the composite, expressed as a percentage.
(3) Measurement of degree of swelling
Preparing starch milk, wherein the volume ratio of the mass of starch in the starch milk to the volume of water is 1.11:100, placing the granular corn starch-AP compound in a water bath at 20 ℃ for 30min, placing the corn starch in a water bath at 75 ℃ for 30min, uniformly mixing the corn starch and the water bath in a vortex manner once every 5min, cooling the corn starch to room temperature in a cold water bath after the reaction is finished, centrifuging the corn starch for 15min under the condition of 4000g centrifugal force, separating supernate and precipitate, and recording the mass of the precipitate:
respectively detecting the swelling degrees of the irradiated corn starch and the irradiated granular corn starch-AP composite sample, wherein the swelling degree = W 1 /W 2
Wherein, W 1 For the quality of the precipitate, W 2 Is the dry weight of the starch sample.
(4) Test for gelatinization Property
And (3) determining the gelatinization characteristics of the irradiated corn starch and granular corn starch-AP compound by referring to the national standard GB/T24853-2010 rapid viscometry for determining the gelatinization characteristics of wheat, rye and flour and starch thereof.
(5) Determination of crystallinity
The crystal form structures of the irradiated starch sample and the granular corn starch-AP compound are measured by an X-ray diffractometer, the test conditions are copper target, voltage is 40kV, current is 40mA, scanning range is 5-35 degrees (2 theta), scanning speed is 3 degrees/min, step length is 0.02 degree, the Relative Crystallinity (RC) of the irradiated starch and the granular corn starch-AP compound is calculated, and the formula is as follows:
RC(％)＝100×Ac/(Ac+Aa)
where Ac represents the area of the crystalline region in the X-ray diffraction pattern, and Aa represents the area of the amorphous region.
(6) Oxidation resistance and thermal stability of AP in composites
A50 mg sample of the composite was dispersed in 5mL of distilled water and shaken on a water bath shaker, and 1% by volume of H was added to the sample to determine oxidation resistance 2 O 2 Reacting for 1h at room temperature; and (3) during measurement of thermal stability, reacting for 6 hours at 90 ℃ in a dark place, after the reaction is finished, adding 1mL of concentrated hydrochloric acid and citric acid (starch base) with the mass fraction of 3% into a sample, carrying out water bath at 70 ℃ for 50min, adding 10.5mL of 1MNaOH solution to adjust the pH, adding absolute ethyl alcohol to a constant volume of 50mL, and measuring the content of the residual AP according to the method (2).
Results and discussion
1. Morphological result analysis of granular corn starch-AP complex
After the corn starch is dyed by using iodine solution, the granular structure of the starch still exists after the starch is irradiated by gamma rays with different doses (A1, A2, C1, D1 and E1 in figure 1), and the color development degree among C0, C1, C2.5, C5 and C10 is not obviously different, and after the granular starch-AP compound is dyed by using the iodine solution, the color development degree of C-AP5 and C-AP10 (D2 and E2 in figure 1) is obviously lower than that of C-AP0, C-AP1 and C-AP2.5 (A2, B2 and C2 in figure 1).
Analysis of measurement result of AP content
After a certain dose of gamma-ray irradiation, the compounding efficiency of the corn starch and the AP is obviously improved, and the embedding rate of the AP is increased to about 40 percent from 33.39 percent (0 kGy); the AP content in the granular corn starch-AP compound is increased from 1.66% (0 kGy) to 2.07% (5 kGy) at most, the amplification reaches 25%, but within 2.5-10 kGy, different irradiation doses have no significant influence on the content of the starch combined with the AP (P > 0.05).
3. Measurement result analysis of swelling degree
For the corn starch, when the irradiation dose is less than or equal to 1kGy, the swelling degree (75 ℃) of the starch is not obviously influenced, when the irradiation dose is more than or equal to 2.5kGy, the swelling degree (P < 0.05) of the corn starch is remarkably increased to about 10 (figure 3), and after the irradiated starch is compounded with AP, the swelling degree of the compound in cold water (20 ℃) is gradually increased from 7.56 (C-AP 0) to 10.13 (C-AP 10) and is close to the swelling degree of the corresponding corn starch at 75 ℃.
4. Analysis of test results of gelatinization characteristics
As shown in fig. 4 (a), as the irradiation dose increases, the peak viscosity, the valley viscosity, and the final viscosity of the starch granules gradually decrease from 2754.0cP (C0) to 2358.0cP (C10), 1918.5cP (C0) to 512.0cP (C10), and 2916.5cP (C0) to 824.5cP (C10), respectively, while the time to reach the peak viscosity decreases from 324s (C0) to 280s (C10), and the time to reach the valley viscosity increases from 464s to 520s (table 1), and simultaneously, as the irradiation dose increases, the attenuation value and the reversion value of the starch gradually increase, while the gelatinization temperature is relatively less affected, and only the gelatinization temperature (74.25 ℃) of C10 is significantly lower than those of other samples.
After the starch and the AP are compounded after irradiation, the gelatinization curve of the compound is obviously changed, and in the cooling stage of the RVA procedure, an obvious viscosity peak (peak II) appears on the curve, the peak is considered to be generated by repolymerization after the depolymerization of the starch-lipid compound (figure 4B), along with the increase of the irradiation dose of the starch granules, the peak viscosity II of the compound is gradually increased and is reduced to 2000.0cP (C-AP 10) after reaching 2555.5cP (C-AP 5), different from other samples, the viscosity of the C-AP10 is stable after reaching the peak value in 692s, and no obvious reduction appears; although the peak viscosity of the starch granules is reduced due to irradiation, after the starch is compounded with the AP, the peak viscosity I tends to increase and then decrease, the viscosity of the starch-AP compound after irradiation is larger than that of C-AP0 on the whole, and different from the single change rule of the starch granules, the attenuation value of the starch-AP compound decreases and then increases with the increase of the irradiation dose, the attenuation degree of C-AP2.5 is the lowest (187.5 cP), and the attenuation degree of C-AP10 is the largest (827.5 cP); the final viscosity showed a tendency to increase and then decrease, with the maximum final viscosity of C-AP5 (2151.0 cP) and the minimum final viscosity of C-AP0 (977.5 cP), and although the gelatinization temperature of both the starch granules and the starch-AP complex tended to decrease, the change in gelatinization temperature of the starch-AP complex was more pronounced.
5. Analysis of relative crystallinity results
The corn starch sample after irradiation shows an A-type crystal structure of grain starch, and has stronger diffraction peaks (figure 5A) near 15 degrees, 17 degrees, 18 degrees and 23 degrees, the crystal form of the starch is not changed by irradiation, but the crystallinity of the starch is slightly reduced, and after the starch is compounded with AP, obvious diffraction peaks (figure 5B) near 7.5 degrees, 13 degrees and 20 degrees show a typical V-type crystal structure; the crystallinity of the starch-AP complex shows a tendency to increase with increasing irradiation dose of starch.
6. Results analysis of antioxidant and thermal stability of AP in composites
After the treatment of the oxidant, the content of the residual AP (0.40%) in the C-AP1 is remarkably lower (P < 0.05) than that of the C-AP0 (0.55%); with the increase of the irradiation dose of the starch, the content of the residual AP in the starch-AP complex is gradually increased, and the residual amount (0.71%) of the AP in the C-AP10 is obviously higher (P < 0.05) than that of the C-AP0 and other samples.
After treatment in a 90 ℃ water bath for 6h, the residual AP content in the compound gradually increased with the increase of the radiation dose of starch, although the gelatinization temperature of C-AP10 is only 76.08 ℃, which is obviously lower than that of other samples, and the embedded AP content is close to that of C-AP2.5 and C-AP5 (figure 2), the residual amount of AP in C-AP10 is 1.57%, and the residual amount of AP in C-AP2.5 and C-AP5 is remarkably (P < 0.05) larger than that in C-AP2.5 and C-AP5, see Table 2.
In conclusion, irradiation has a certain degradation effect on starch chains, the content of AP in the composite product can be effectively improved, and the maximum amplification reaches 25%; irradiation can increase the viscosity peak of the compound viscosity curve in the cooling stage; with the increase of the irradiation dose, the swelling degree, the relative crystallinity and the thermal stability of the compound are gradually increased, the oxidation resistance is firstly reduced and then increased, and in all the compounds, when the irradiation dose of the starch is 10kGy, the compound product has relatively high compound efficiency, the swelling degree and the relative crystallinity are the maximum, and the shearing resistance, the oxidation resistance and the thermal stability are the strongest.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of granular starch-lipid complex is characterized in that after gamma-ray irradiation is carried out on starch granules, a hydrothermal method is adopted, and the irradiated starch granules and lipid are compounded to prepare the granular starch-lipid complex.
2. The method for preparing granular starch-lipid complex according to claim 1, wherein the starch granules comprise rhizome starch, cereal starch, and legume starch.
3. The method for preparing granular starch-lipid complex as claimed in claim 2, wherein the root starch includes potato starch, tapioca starch, sweet potato starch, and yam starch, the cereal starch includes corn starch, wheat starch, buckwheat starch, rice starch, and glutinous rice starch, and the bean starch includes pea starch, mung bean starch, and red bean starch.
4. The method of claim 1, wherein the lipid comprises free fatty acids, fatty acid derivatives, phospholipids.
5. The method for preparing granular starch-lipid complex as claimed in claim 4, wherein the free fatty acid comprises palmitic acid, lauric acid, myristic acid, stearic acid, caprylic acid, caproic acid, capric acid, oleic acid, butyric acid, linoleic acid, linolenic acid, arachidonic acid; the derivatives of the fatty acid comprise ascorbyl palmitate, retinol ester, phytosterol ester and glyceryl monostearate; the phospholipid material comprises lecithin and lysophospholipid.
6. The method for preparing granular starch-lipid complex according to claim 1, wherein the method for irradiating starch granules comprises the following steps: putting a silver dichromate dosimeter into the starch granules, and sampling the starch granules by adopting 60 Co-gamma irradiation, and the actual absorbed dose of the sample was determined by a silver dichromate dosimeter.
7. The method for preparing the granular starch-lipid complex according to claim 6, wherein the irradiation dose of the starch granules is 1-10kGy.
8. The method for preparing granular starch-lipid complex according to claim 1, wherein the granular starch-lipid complex is prepared by the following steps:
s1, dissolving the irradiated starch granules in water to prepare 6-10% of starch milk by mass percent, and stirring for 0.5-1.5 hours in a water bath at 50-70 ℃ to obtain expanded starch milk;
and S2, preparing lipid into an absolute ethyl alcohol lipid solution, adding the absolute ethyl alcohol lipid solution into the swelling starch milk obtained in the step S1, continuously heating and stirring for 1-2 hours, then cooling to room temperature, and obtaining the granular starch-lipid compound after centrifugation, washing and drying.
9. The method for preparing granular starch-lipid complex according to claim 8, wherein the mass ratio of lipid to starch granules after irradiation in step S2 is 1-15:100, the volume ratio of the lipid to the absolute ethyl alcohol is 5-10 g.
10. The method for preparing granular starch-lipid complex according to claim 8, wherein the centrifugation, washing and drying method in step S2 is: centrifuging at 3000-4000g for 15-20min, washing with 50% ethanol solution, washing with anhydrous ethanol, vacuum filtering, drying at 30-50 deg.C overnight, pulverizing, and sieving with 100-150 mesh sieve.
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