CN115677866B - Preparation method of granular starch-lipid compound - Google Patents
Preparation method of granular starch-lipid compound Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229920002472 Starch Polymers 0.000 claims abstract description 156
- 235000019698 starch Nutrition 0.000 claims abstract description 154
- 239000008107 starch Substances 0.000 claims abstract description 153
- 238000000034 method Methods 0.000 claims abstract description 33
- 150000002632 lipids Chemical class 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000011786 L-ascorbyl-6-palmitate Substances 0.000 claims description 53
- QAQJMLQRFWZOBN-LAUBAEHRSA-N L-ascorbyl-6-palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](O)[C@H]1OC(=O)C(O)=C1O QAQJMLQRFWZOBN-LAUBAEHRSA-N 0.000 claims description 40
- 235000010385 ascorbyl palmitate Nutrition 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
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- 239000008267 milk Substances 0.000 claims description 17
- 210000004080 milk Anatomy 0.000 claims description 17
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- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 claims 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Natural products OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 claims 1
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 229920000856 Amylose Polymers 0.000 description 12
- 229940099112 cornstarch Drugs 0.000 description 12
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to the technical field of starch modification, in particular to a preparation method of a granular starch-lipid compound, which comprises the steps of firstly adopting gamma-rays to irradiate starch particles, then adopting a hydrothermal method technology as a matching process to compound the irradiated starch particles with lipid to prepare the granular starch-lipid compound.
Description
Technical Field
The invention relates to the technical field of starch modification, in particular to a preparation method of a granular starch-lipid compound.
Background
The starch-lipid complex is an important starch derivative, the fatty chain of the lipid can be stabilized in the amylose spiral cavity through hydrogen bond, hydrophobic interaction, van der Waals force and the like in the forming process of the starch-lipid complex, and the hydrophilic group of the lipid is exposed outside the spiral due to steric hindrance and electrostatic repulsion, so that the gelatinization, aging, enzymolysis, freeze thawing stability and the like of the starch can be influenced, and the texture characteristics, nutritional quality and the like of food are beneficially influenced; in addition, the starch-lipid complex can be used for embedding some 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 interesting for the industry. Because of the wide application prospect of the starch-lipid complex, the artificial synthesis of the starch-lipid complex has become a current research hot spot. However, most of the synthesis researches at home and abroad at present usually use pure amylose, debranched starch or gelatinized starch to prepare the compound, and the methods need a pungent chemical reagent and a higher reaction temperature, or are long in time consumption and high in cost, so that the industrial production is not facilitated, and therefore, development of a novel process for producing the efficient green starch-lipid compound is needed.
In recent years, the research of granular starch-lipid complex is focused, the method does not need to separate amylose or prepare debranched starch/starch paste, starch particles and lipid are subjected to composite reaction in an expanded state, and the product is subjected to proper recovery and drying treatment to form the granular starch-lipid complex; at present, two methods for preparing granular starch-lipid composite in laboratory are mainly adopted, the first preparation method is to pretreat starch firstly, the pretreated starch still keeps the form of particles because of incomplete gelatinization, but the physicochemical properties of the starch are changed and are different from those of starch particles of original starch, therefore, the first preparation method is to prepare granular starch firstly, and the granular starch is compounded with lipid to form composite by utilizing the characteristic that the granular starch is soluble in cold water at a lower temperature (20-60 ℃), the method is suitable for various lipids, and is especially suitable for embedding some heat-sensitive vitamins, antioxidants and the like, but the preparation of granular starch is generally complicated, and the common methods for preparing granular starch comprise spray drying, saturated monohydric alcohol, polyhydric alcohol, alcohol-alkali method, ball milling method or alcohol-alkali method and other methods, and the methods generally have high requirements on equipment (spray drying, saturated monohydric alcohol, polyhydric alcohol, ball milling), require a large amount of alcohol and/or alkaline solution (saturated monohydric alcohol, alcohol-alkali method, enzyme-alkali method, alkaline method and alkaline method); the second preparation method comprises the following steps: the traditional hydrothermal method is used for heating starch for a period of time under the condition that the starch is slightly lower than the gelatinization temperature (generally 80-90 ℃) to expand the starch, and then lipid is added to carry out a composite reaction.
Starch is classified into cereal starch, rhizome starch, bean starch and other starch according to raw material sources, wherein cereal corn starch is one of starches with the largest starch yield ratio in China, and is frequently used for researching starch-lipid compound. Ascorbyl Palmitate (AP) is an esterification product of palmitic acid and ascorbic acid, an important antioxidant, and is a representative lipid often used in the study of starch-lipid complexes. The starch-ascorbyl palmitate complex is generally prepared by the first preparation method described above, namely: the starch is required to be pretreated and then subjected to a composite reaction with the AP at a lower temperature (20-70 ℃), the pretreatment methods generally require a large amount of irritant chemical reagents NaOH, DMSO and the like, or a large amount of ethanol solution and high-temperature conditions, and the recovered and dried starch, amylose or granular starch is reacted with the AP, so that the operation is relatively complicated, and the industrial production and the application of the starch-AP composite 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 compound, which solves the technical problems that the prior preparation method of the starch-lipid compound needs irritant chemical reagents NaOH, DMSO and the like, needs a large amount of ethanol solution and high temperature conditions, is relatively complicated to operate and has low compound preparation efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the granular starch-lipid compound comprises the steps of carrying out gamma-ray irradiation on starch particles, and then adopting the hydrothermal method to compound the irradiated starch particles with lipid to prepare the granular starch-lipid compound.
Preferably, the starch granule comprises rhizome starch, cereal starch, bean starch, and the starch is described in GB/T8887-2021 starch Classification.
Preferably, the rhizome 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 acid, derivative of fatty acid, phospholipid.
Preferably, the free fatty acids include palmitic acid, lauric acid, myristic acid, stearic acid, caprylic acid, caproic acid, oleic acid, butyric acid, linoleic acid, linolenic acid, arachidonic acid; derivatives of fatty acids include ascorbyl palmitate, retinol esters, phytosterol esters, glycerol monostearate, and the like; the phospholipid substance comprises lecithin, lysophospholipid, etc.
Preferably, the method for irradiating the starch granules comprises the following steps: placing silver dichromate dosimeter into starch granule, and adopting starch granule sample 60 Co-gamma radiation, determination of the actual absorbent of a sample by means of a silver dichromate dosimeterAmount of the components.
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 particles in water to prepare starch milk with the mass fraction of 6-10%, and stirring for 0.5-1.5 hours in a water bath at 50-70 ℃ to obtain expanded starch milk;
s2, preparing the lipid into an absolute ethyl alcohol lipid solution, adding the absolute ethyl alcohol lipid solution into the expanded starch milk obtained in the step S1, continuously heating and stirring for 1-2h, cooling to room temperature, centrifuging, washing and drying to obtain the granular starch-lipid compound.
Preferably, the mass ratio of the lipid to the irradiated starch granules in the step S2 is 1-15:100, the volume ratio of lipid to absolute ethanol is 5-10g to 100mL.
Preferably, in the step S2, the centrifugation, washing and drying methods are as follows: centrifuging for 15-20min under the condition of 3000-4000g centrifugal force, centrifugally washing with ethanol solution with volume fraction of 50%, washing precipitate with absolute ethanol, suction filtering, drying at 30-50deg.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 gamma-ray irradiation with a certain dosage is carried out on starch particles, a hydrothermal method is used for preparing the granular starch-lipid compound, and the irradiation has a certain degradation effect on starch chains, so that the content of lipid in a compound product can be effectively improved, and in addition, the irradiation can increase the viscosity peak of a compound viscosity curve in a cooling stage; with the increase of 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. Of all the composites, the composite product has relatively high composite efficiency with maximum swelling, relative crystallinity, and the strongest shear resistance, oxidation resistance and thermal stability when the irradiation dose of starch is 10kGy.
3. After the starch is irradiated, the amylose and the amylopectin are degraded, the polymerization degree (chain length) of the starch is reduced, the expansion degree and the solubility of the starch in a certain temperature range are increased, and the expansion degree and the solubility are increased, so that lipid molecules can enter the starch particles or can be subjected to a composite reaction with the amylose molecules outside the particles; degradation of amylopectin reduces its barrier effect on amylose and lipid complexation; at the same time, the decrease 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 preparation method overcomes the technical defects that the pretreatment of the prior preparation method requires irritant chemical reagents of NaOH, DMSO and the like, a large amount of ethanol solution and high temperature conditions are required, and the operation is relatively complicated.
4. The irradiation technology is a green, low-carbon and non-thermal processing high-new technology, the irradiated food is safe and harmless, starch is subjected to degradation reaction after being irradiated by rays to cause starch chain breakage, the polymerization degree is reduced, the gelatinization property, the expansion property, the apparent amylose content, the crystallization structure and the like of the starch are possibly influenced, the structure is damaged after the starch is irradiated, water molecules are easier to permeate into starch particles, the expansion of the starch in hot water is promoted, and amylose is easier to dissolve out, so that the characteristic is favorable for promoting the composite reaction of amylose and lipid; meanwhile, the degradation of the amylopectin weakens the interference of the amylopectin on the linear chain and lipid composite, so that the preparation of the granular starch-lipid composite by combining irradiation and a hydrothermal method is theoretically feasible, and the method is helpful for developing a new green efficient production technology of the granular starch-lipid composite.
5. Compared with the non-granular starch-lipid compound, the granular starch-lipid compound prepared by the invention does not need to separate amylose or prepare debranched starch and starch paste, the starch particles and the lipid undergo a compound reaction in an expanded state, and the product is subjected to proper recovery and drying treatment, so that the process is simple, the preparation process is pollution-free, the time consumption is short, and the production cost is relatively low.
Drawings
FIG. 1 is a sample morphology of examples 1-4 and comparative example 1; a1, B1, C1, D1 and E1 are respectively C0, C1, C2.5, C5 and C10 irradiated starch samples, A2, B2, C2, D2 and E2 are respectively C-AP0, C-AP1, C-AP2.5, C-AP5 and C-AP10 granular starch-lipid complex samples, and the scale of the figure is 20 mu m;
FIG. 2 is a graph showing the results of the composite efficiencies of the samples of examples 1 to 4 and comparative example 1;
FIG. 3 is a graph showing the expansion curves of the samples of examples 1-4 and comparative example 1;
FIG. 4 is a graph showing the results of the gelatinization property test of the samples of examples 1 to 4 and comparative example 1, wherein, A is a graph showing the results of the gelatinization property test of the starch samples after C0, C1, C2.5, C5, C10 irradiation, and B is a graph showing the results of the gelatinization property test of the granular starch-lipid composite samples of C-AP0, C-AP1, C-AP2.5, C-AP5, C-AP 10;
FIG. 5 is an X-ray diffraction pattern of samples of examples 1-4 and comparative example 1, wherein, A is the X-ray diffraction pattern of the irradiated starch C0, C1, C2.5, C5, C10 samples; panel B shows the X-ray diffraction patterns 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 below with reference to the drawings, and it should be noted that the embodiments are illustrative, not limiting, and should not be construed as limiting the scope of the present invention.
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 compound comprises the following steps:
(1) Weighing 100g of starch, sealing in self-sealing bags, selecting 3 parallel samples for each irradiation dose, placing 3 silver dichromate dosimeters in each sample for measuring actual absorption dose of the samples, and placing the packaged samples 60 Carrying out 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 irradiated sample is named as C10, and the sample is placed in a refrigerator at 4 ℃ for standby after the irradiation is finished;
(2) Weighing 30g of starch (dry basis) from the sample C10 irradiated in the step (1), mixing with distilled water to prepare starch milk with the mass fraction of 8%, and stirring in a water bath at 65 ℃ for 1h to obtain expanded starch milk;
(3) Preparing 1.5g of ascorbyl palmitate into an ascorbyl palmitate-absolute ethyl alcohol solution with the mass concentration of 10%, slowly adding the ascorbyl palmitate-absolute ethyl alcohol 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 three times with the ethanol solution with the volume fraction of 50%, washing and filtering the precipitate with absolute ethyl alcohol, drying overnight at 40 ℃, crushing, sieving with a 120-mesh sieve to obtain a granular corn starch-ascorbyl palmitate compound, and naming the granular corn starch-ascorbyl palmitate compound as C-AP10.
Example 2
The procedure was the same as in example 1, except that the irradiation dose was replaced with 1kG from 10kGy, the irradiated starch was designated as C1, and then the sample C1 was compounded with ascorbyl palmitate to give a granular corn starch-ascorbyl palmitate complex designated as C-AP1.
Example 3
The procedure for the preparation of example 1 was identical, except that the irradiation dose was replaced by 2.5kGy, the irradiated starch was designated as C2.5, and the sample C2.5 was compounded with ascorbyl palmitate to give a granular corn starch-ascorbyl palmitate complex designated as C-AP2.5.
Example 4
The procedure was the same as in example 1, except that the irradiation dose was replaced with 5kGy from 10kGy, the irradiated starch was designated as C5, and then the sample C5 was compounded with ascorbyl palmitate to give a granular corn starch-ascorbyl palmitate compound designated as C-AP5.
Example 5
The preparation method of the granular potato starch-glycerin monostearate compound comprises the following steps:
(1) Weighing 100g of potatoThe starch is sealed in a self-sealing bag, 3 parallel samples are selected for each irradiation dose, 3 silver dichromate dosimeters are placed in each sample for measuring the actual absorbed dose of the sample, and the sub-packaged samples are placed in the 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 standby after the sample 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 three times by using the ethanol solution with the volume fraction of 50%, washing and filtering the precipitate by using absolute ethyl alcohol, drying overnight at 30 ℃, crushing, and sieving by a 100-mesh sieve to obtain the granular potato starch-glyceryl monostearate compound.
Example 6
The preparation method of the granular tapioca starch-lysophospholipid compound comprises the following steps:
(1) Weighing 100g of tapioca starch, sealing in self-sealing bags, selecting 3 parallel samples for each irradiation dose, placing 3 silver dichromate dosimeters in each sample for measuring actual absorption dose of the samples, and placing the packaged samples 60 Carrying out irradiation treatment in a Co-gamma irradiation device, setting the irradiation dose to be 2.5kGy, setting the average irradiation dose rate to be 0.55kGy, and placing the sample in a refrigerator at 4 ℃ for standby after the irradiation of the sample is completed;
(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 1.5 hours 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 lysophospholipid-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 20min under 4000g of centrifugal force, centrifuging, repeatedly centrifuging and washing three times by using the ethanol solution with the volume fraction of 50%, washing and precipitating by using absolute ethanol, filtering, drying overnight at 50 ℃, crushing, and sieving by a 150-mesh sieve to obtain the granular tapioca starch-lysophospholipid compound.
Comparative example 1
The procedure was the same as in example 1, except that the irradiation dose was changed from 1kGy to 0kGy, i.e., the irradiation treatment was not performed, the irradiated sample was designated as C0, and the resultant granular corn starch-ascorbyl palmitate complex was designated as C-AP0 by compounding the sample C0 with ascorbyl palmitate.
The measuring method comprises the following steps:
(1) Morphology determination of granular corn starch-ascorbyl palmitate complex
2mg of the granular corn starch-ascorbyl palmitate complex sample is taken and suspended in 1mL of 30% glycerol solution by volume percentage, 10 mu L of 0.1mol/L iodine solution is added, after 5min of dyeing, the morphology of the granular corn starch-ascorbyl palmitate complex of the samples of examples 1-4 and comparative example 1 is observed by using an Olinbas BX53 biological microscope.
(2) Content determination of ascorbyl palmitate
Accurately weighing 50mg of granular corn starch-ascorbyl palmitate complex 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 10.5mL of 1M NaOH solution to adjust pH to 6.0, and then adding absolute ethanol to constant volume to 50mL. The absorbance of the above solution at 247nm was measured by an ultraviolet spectrophotometer. And (3) preparing a proper amount of AP standard substance into standard liquid of 1.25mg/mL, respectively taking 2mL, 1mL, 0.5mL, 0.25mL and 0.125mL of standard liquid to replace the starch sample, establishing a standard curve, and measuring the content of the AP.
AP content (%) =mass of AP/dry weight of starch sample×100
Embedding rate (%) =mass of embedded AP/addition amount of ap×100
The 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 final bound AP mass in the complex to the total AP content added during the preparation of the complex, expressed as a percentage.
(3) Determination of the degree of swelling
Preparing starch milk, wherein the volume ratio of starch to water in the starch milk is 1.11:100, placing the granular corn starch-AP compound in a water bath at 20 ℃ for 30min, placing the corn starch in the water bath at 75 ℃ for 30min, vortex mixing once every 5min, cooling the mixture to room temperature in a cold water bath after the reaction is finished, centrifuging for 15min under the condition of 4000g centrifugal force, separating supernatant and precipitate, and recording the quality of the precipitate:
the swelling degree of the irradiated corn starch and the granular corn starch-AP compound sample was measured separately, and swelling degree=W 1 /W 2
Wherein W is 1 For the mass of the precipitate, W 2 Is the dry weight of the starch sample.
(4) Test of gelatinization characteristics
The gelatinization properties of the irradiated corn starch and granular corn starch-AP complex were determined by reference to national standard GB/T24853-2010 Rapid viscosimeter method for determination of wheat, rye and flour and starch gelatinization properties.
(5) Determination of crystallinity
The crystal form structure of the irradiated starch sample and the granular corn starch-AP compound is measured by an X-ray diffractometer, the test conditions are a copper target, the voltage is 40kV, the current is 40mA, the scanning range is 5-35 degrees (2 theta), the scanning speed is 3 degrees/min, the step length is 0.02 degrees, and the Relative Crystallinity (RC) of the irradiated starch and the granular corn starch-AP compound is calculated according to the following formula:
RC(％)＝100×Ac/(Ac+Aa)
wherein 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 the composite
50mg of the complex sample was taken and dispersed in 5mL of steamAdding H with volume percentage of 1% into distilled water and oscillating on a water bath table, and adding H with volume percentage of 1% into a sample when measuring oxidation resistance 2 O 2 Reacting for 1h at room temperature; when the thermal stability is measured, the reaction is carried out for 6 hours at 90 ℃ in a dark place, after the reaction is finished, 1mL of concentrated hydrochloric acid and 3% citric acid (starch base) are added into a sample, water bath is carried out for 50 minutes at 70 ℃, 10.5mL of 1M NaOH solution is added to adjust the pH, then absolute ethyl alcohol is added to constant volume to 50mL, and the residual AP content is measured according to the method (2).
Results and discussion
1. Morphological analysis of granular corn starch-AP complexes
After staining of the irradiated cornstarch with iodine solution, it was observed that the granular structure remained after irradiation of the starch with gamma rays at different doses, and that there was no significant difference in the degree of coloration between C0, C1, C2.5, C5 and C10 (A1, A2, C1, D1, E1 in FIG. 1), and that the degree of coloration of the granular starch-AP complex was significantly lower than that of C-AP0, C-AP1 and C-AP2.5 (A2, B2 and C2 in FIG. 1) after staining of the granular starch-AP complex with iodine solution.
Analysis of the results of the measurement of AP content
After gamma-ray irradiation with a certain dosage, the compounding efficiency of the corn starch and the AP is obviously improved, and the embedding rate of the AP is increased from 33.39 percent (0 kGy) to about 40 percent; the AP content of the granular corn starch-AP compound is increased from 1.66 percent (0 kGy) to 2.07 percent (5 kGy) at most, the increase reaches 25 percent, but within 2.5-10 kGy, the different irradiation doses have no obvious effect on the content of the starch combined with the AP (P is more than 0.05).
3. Analysis of results of measurement of swelling degree
For corn starch, the swelling degree (75 ℃) of the starch is not obviously affected when the irradiation dose is less than or equal to 1kGy, the swelling degree of the corn starch is obviously increased (P < 0.05) to about 10 when the irradiation dose is more than or equal to 2.5kGy (figure 3), and after the irradiated starch is compounded with the 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 for gelatinization characteristics
As shown in fig. 4 (a), the peak viscosity, the trough viscosity, and the final viscosity of the starch granules were gradually reduced from 2754.0cP (C0) to 2358.0cP (C10), 1918.5cP (C0) to 512.0cP (C10), 2916.5cP (C0) to 824.5cP (C10), respectively, with increasing irradiation dose, and the time to peak viscosity was reduced from 324s (C0) to 280s (C10), and the time to trough viscosity was increased from 464s to 520s (table 1), while the attenuation value of the starch was gradually increased, the retrogradation value was gradually reduced, and the gelatinization temperature was relatively less affected, with increasing irradiation dose, with the gelatinization temperature of only C10 (74.25 ℃) significantly lower than other samples.
After the irradiation, the gelatinization curve of the compound is obviously changed, and in the cooling stage of the RVA program, an obvious viscosity peak (peak II) appears on the curve, wherein the peak is considered to be generated by depolymerization and repolymerization of the starch-lipid compound (figure 4B), the peak viscosity II of the compound gradually increases along with the increase of the irradiation dose of starch particles, and is reduced to 2000.0cP (C-AP 10) after reaching 2555.5cP (C-AP 5), unlike other samples, the viscosity of the C-AP10 tends to be stable after reaching the peak at 692s, and no obvious reduction appears; although the irradiation causes the reduction of the peak viscosity of the starch particles, after the starch is compounded with the AP, the peak viscosity I shows a tendency of increasing and then decreasing, the viscosity of the starch-AP compound after the irradiation is larger than C-AP0 as a whole, unlike the single change rule of the starch particles, the attenuation value of the starch-AP compound is firstly reduced and then increased along 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 tended to increase and decrease first, with the final viscosity of C-AP5 being the greatest (2151.0 cP) and the final viscosity of C-AP0 being the smallest (977.5 cP), although the gelatinization temperature of both the starch granule and the starch-AP composite tended to decrease, but the change in gelatinization temperature of the starch-AP composite was more pronounced.
5. Analysis of relative crystallinity results
The corn starch sample after irradiation shows a grain starch A-type crystal structure, has stronger diffraction peaks near 15 degrees, 17 degrees, 18 degrees and 23 degrees (figure 5A), the irradiation does not change the crystal form of the starch, but leads to slightly reduced crystallinity of the starch, after the starch is compounded with AP, obvious diffraction peaks near 7.5 degrees, 13 degrees and 20 degrees (figure 5B), and shows a typical V-type crystal structure; as the starch irradiation dose increases, the crystallinity of the starch-AP complex tends to increase.
6. Analysis of results of oxidation resistance and thermal stability of AP in composite
The residual AP content (0.40%) in C-AP1 after the oxidant treatment was significantly (P < 0.05) lower than C-AP0 (0.55%); the residual AP content of the starch-AP complex gradually increased with increasing starch irradiation dose, and the residual AP content (0.71%) of the C-AP10 was significantly higher (P < 0.05) than that of the C-AP0 and other samples.
After 6h treatment in a 90℃water bath, the residual AP content of the composite gradually increased with increasing starch irradiation dose, although the gelatinization temperature of C-AP10 was 76.08 ℃only, significantly lower than other samples, and the embedded AP content was close to that of C-AP2.5 and C-AP5 (FIG. 2), the residual AP content in C-AP10 was 1.57%, significantly (P < 0.05) greater than that of C-AP2.5 and C-AP5, as shown in Table 2.
In conclusion, the irradiation has a certain degradation effect on the starch chain, so that the content of the AP in the composite product can be effectively improved, and the amplification is up to 25%; irradiation can increase the viscosity peak of the compound viscosity profile during the cooling phase; with the increase of the irradiation dose, the expansion 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, and has the maximum expansion degree, the maximum relative crystallinity and the strongest shear resistance, oxidation resistance and thermal stability.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (6)
1. The preparation method of the granular starch-lipid composite is characterized in that after gamma-ray irradiation is carried out on starch particles, the granular starch-lipid composite is prepared by adopting the composition of the irradiated starch particles and lipid through a hydrothermal method;
the granular starch-lipid complex is prepared according to the following steps:
s1, dissolving the irradiated starch particles in water to prepare starch milk with the mass fraction of 6-10%, and stirring for 0.5-1.5 hours in a water bath at 50-70 ℃ to obtain expanded starch milk;
s2, preparing lipid into absolute ethyl alcohol lipid solution, adding the absolute ethyl alcohol lipid solution into the expanded starch milk obtained in the step S1, continuously heating and stirring for 1-2h, cooling to room temperature, and centrifuging, washing and drying to obtain a granular starch-lipid compound;
the irradiation method of the starch granules comprises the following steps: placing silver dichromate dosimeter into starch granule, and adopting starch granule sample 60 Co-gamma ray irradiation, and measuring the actual absorption dose of a sample through a silver dichromate dosimeter;
the irradiation dose of the starch granules is 1-10kGy;
the lipid is selected from one of free fatty acid, fatty acid derivative and phospholipid.
2. The method for preparing a granular starch-lipid composite according to claim 1, wherein the starch granules are selected from one of rhizome starch, cereal starch and legume starch.
3. The method for preparing a granular starch-lipid composite according to claim 2, wherein the rhizome starch is selected from one of potato starch, tapioca starch, sweet potato starch and yam starch, the cereal starch is selected from one of corn starch, wheat starch, buckwheat starch, rice starch and glutinous rice starch, and the bean starch is selected from one of pea starch, mung bean starch and red bean starch.
4. The method for preparing a granular starch-lipid composite according to claim 1, wherein the free fatty acid is selected from one of palmitic acid, lauric acid, myristic acid, stearic acid, caprylic acid, caproic acid, capric acid, oleic acid, butyric acid, linoleic acid, linolenic acid, and arachidonic acid; the derivative of the fatty acid is selected from one of ascorbyl palmitate, retinol ester, phytosterol ester and glycerin monostearate; the phospholipid material is selected from one of lecithin and lysophospholipid.
5. The method for preparing a granular starch-lipid composite according to claim 1, wherein the mass ratio of lipid to starch granules after irradiation in step S2 is 1-15:100, the volume ratio of the mass of the lipid to the absolute ethyl alcohol is 5-10 g/100 mL.
6. The method for preparing a granular starch-lipid composite according to claim 1, wherein the centrifugation, washing and drying method in step S2 is as follows: centrifuging for 15-20min under the condition of 3000-4000g centrifugal force, centrifugally washing with ethanol solution with volume fraction of 50%, washing precipitate with absolute ethanol, suction filtering, drying at 30-50deg.C overnight, pulverizing, and sieving with 100-150 mesh sieve.
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