WO2023231831A1 - 一种基于高压剪切诱导制备具有易食特性复合凝胶的方法 - Google Patents
一种基于高压剪切诱导制备具有易食特性复合凝胶的方法 Download PDFInfo
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- WO2023231831A1 WO2023231831A1 PCT/CN2023/095753 CN2023095753W WO2023231831A1 WO 2023231831 A1 WO2023231831 A1 WO 2023231831A1 CN 2023095753 W CN2023095753 W CN 2023095753W WO 2023231831 A1 WO2023231831 A1 WO 2023231831A1
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- Prior art keywords
- fish meat
- composite gel
- water
- compound material
- gel
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Links
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Definitions
- the invention relates to a method for preparing a composite gel with easy-to-eat properties based on high-pressure shear induction, and belongs to the technical field of food processing.
- Food texture improvement technology can reduce the incidence of dysphagia in most elderly people and has been considered an effective means to improve the quality of life of elderly people with dysphagia and ensure swallowing safety. Therefore, in order to meet consumers' personalized dietary needs for special nutrition and texture, technological innovation in easy-to-eat food processing has become a research direction for society and the food industry.
- the purpose of the present invention is to overcome the shortcomings of poor swallowing or esophageal retention that may occur in existing functional foods, as well as the instability of functional active substances in protein-based gels, and to provide a method based on high-pressure shear induction that is easy to eat.
- the method of characteristic composite gel uses high-pressure shearing to break up high-quality marine proteins and promote the cross-linking of protein molecules to form a highly water-retaining network structure.
- oils loaded with functional active ingredients are embedded in the protein gel network, and finally the result is both Composite gel with low gel strength (gel strength between 0.1 and 1.5N or storage modulus between 150 and 260 Pa) and high water/oil holding capacity (water/oil holding rate greater than or equal to 90%).
- the resulting composite gel is easy to eat at room temperature and can provide highly nutritious, soft gel-like easy-to-eat food for special groups such as the elderly and patients with dysphagia.
- the food can also be used as additives with the help of 3D printing technology. Personalized form customization.
- the first object of the present invention is to provide a method for preparing a composite gel with easy-to-eat properties based on high-pressure shear induction, which includes the following steps:
- Step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with the salt solution, rinse and filter to obtain prefabricated fish meat;
- Nutritional control of fish meat base Mix the prefabricated fish meat obtained in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: (1 ⁇ 3)kg: (0 ⁇ 200)g: 0 ⁇ 150)g;
- step S5 One-step emulsion filling-protein cross-linking:
- the compound material obtained in step S3 is subjected to high-pressure shearing treatment, and the functional grease described in step S4 is added simultaneously during the high-pressure shearing treatment to obtain a composite gel;
- the pressure is 20 ⁇ 100MPa
- the corresponding high-pressure shearing treatment time for each 100g compound material is 4 ⁇ 15min
- the mass ratio of compound material and functional oil is (85 ⁇ 90)g:(15 ⁇ 10)g.
- the material-to-liquid ratio of cooked fish meat and salt solution in step S2 is: 1:10 to 1:1000g/mL.
- the salt solution is a 0.01% to 0.2% NaCl solution.
- the rinsing temperature in step S2 is 40-70°C, and the rinsing is performed 3-10 times, each time for 1-5 minutes.
- the raw fish in step S1 is cod or sturgeon; the heating and maturing is performed at 60 to 100°C for 5 to 30 minutes.
- the filtration in step S2 is performed using 60-100 mesh filter cloth.
- the raw fish in step S1 is fresh raw fish. After slaughtering, the skin, bones and internal organs are removed in time to obtain fish meat; if the fish body after slaughter cannot be processed in time, the fish body needs to be cooled at low temperature to make the fish The body temperature drops rapidly, and then is stored at a low temperature of 4 to 6°C. After the fish is completely stiff, the fish is stored at about 0°C. If the refrigerated fish cannot be matured in time, the fish needs to be frozen at -80 to -20°C. save.
- the raw fish described in step S1 is the fish meat of frozen raw fish.
- the frozen fish body needs to be slowed down and then skinned, boned and internal organs removed to obtain the fish meat.
- the water in step S3 is purified water or mineral water.
- the fat-soluble nutrients in step S4 include but are not limited to vitamin E and carotenoids.
- the liquid oil in step S4 includes but is not limited to linseed oil and olive oil.
- the mixing ratio of liquid oil and fat-soluble nutrients in step S4 is 1kg:(0.005 ⁇ 0.3)g.
- the mass ratio of liquid oil to vitamin E and carotenoids in step S4 is 1kg: (0.1-0.2)g: (0-0.06)g.
- the pressure during the high-pressure shearing treatment in step S5 is 40 MPa, and the high-pressure shearing treatment time per 100 g of compound material is 9 minutes.
- step S5 after step S5, it also includes: S6: packaging, sterilizing, sealing, and cooling the composite gel obtained in step S5 to room temperature to obtain an easy-to-eat composite gel food.
- the container used for packaging in step S6 includes but is not limited to metal cans or composite material bags/cans.
- the sterilization method in step S6 includes but is not limited to at least one of low-temperature long-term sterilization and radiation sterilization; specifically, the low-temperature long-term sterilization conditions are: temperature 60-80°C, The time is 15 to 30 minutes; the specific radiation sterilization conditions are: 1 to 10kGy.
- the storage temperature of the easy-to-eat composite gel food obtained in step S6 is 2 to 10°C.
- the second object of the present invention is to provide a composite gel with easy-to-eat properties prepared by the aforementioned method.
- the composite gel with easy-to-eat properties has a gel strength of 0.1 to 1.5 N, a storage modulus of 150 to 260 Pa, and a water/oil holding rate of not less than 98%.
- the products after 3D printing have good precision and shape.
- the gastric half-emptying time (t 1/2 ) is not higher than 150 minutes.
- the second object of the present invention is to provide the application of composite gel with easy-to-eat properties in the field of 3D printing.
- the application of the composite gel with easy-to-eat properties in 3D printing provided by the present invention includes the following steps:
- step (1) Shaping: The gel with a three-dimensional shape printed in step (1) is left to stand at 0 to 25°C for 10 to 30 minutes to set, in order to increase the elasticity and water retention of the easy-to-eat composite gel.
- 3D printing in step (1) The brand and model of the 3D printer is Shiyin Technology FoodBot-D2. Introduce the composite gel with easy-to-eat properties into the feed barrel of the 3D printer, select the printing model for printing, Select the nozzle diameter as 0.8 ⁇ 1.8mm, the printing speed as 15 ⁇ 30mm/s, the extrusion force as 2 ⁇ 7N, and the printing environment temperature as 4 ⁇ 25°C.
- the present invention creatively proposes a one-step emulsion filling-protein cross-linking method, that is, the compound material is subjected to high-pressure shearing treatment, and functional oil is added simultaneously during the high-pressure shearing treatment process to obtain a composite gel; through reasonable settings
- the pressure and shearing time control the size of heat-denatured protein particles and the degree of cross-linking of the gel network, using high-pressure shearing to break high-quality marine proteins and promote the cross-linking of protein molecules to form a high water-retention network structure, while "embedding" functional oils
- the composite gel network structure it not only realizes the embedding of fat-soluble nutrients, but also improves the water-locking ability of the composite gel, achieves efficient control of the water/oil holding rate of more than 90%, and improves the easy-to-eat properties of functional oils.
- the comprehensively regulated product has a gel strength of 0.1 to 1.5N and a storage modulus of 150 to 260Pa. It is easy to eat at room temperature and can be used by special groups such as the elderly and patients with dysphagia. It provides highly nutritious, soft gel-like easy-to-eat foods; it overcomes the shortcomings of poor swallowing or esophageal retention that may occur with existing functional foods, and solves problems such as the instability of functional active substances in protein-based gels.
- the present invention preforms the fish meat by rinsing the cooked fish meat in a salt solution, which helps to reduce the pressure of subsequent high-pressure shearing, reduce energy consumption, and increase gel production.
- the present invention found through a large number of experiments that in the nutritional regulation step of fish meat, the selection of dietary fiber compounded with fish will have a significant impact on the 3D printing performance of the composite gel product: based on the method of the present invention, only the method of the present invention can be selected A specific compound combination of prefabricated fish meat, water, inulin and soybean dietary fiber, combined with a specific ratio, can produce a composite gel with good 3D printing performance.
- the 3D printed products have good accuracy and
- the composite gel obtained by using chia seeds, quinoa powder or konjac gum is not suitable for 3D printing or it is difficult to successfully prepare gel products at all.
- the present invention relates to the nutritional regulation of fish meat base, which improves the nutritional properties of the product and at the same time, the prepared composite gel has Good 3D printing performance.
- the 3D printed products have good accuracy and shape, and can still maintain high water/oil holding rates after 3D printing.
- the present invention fully improves the utilization rate of marine resources, and can use some of the remaining minced meat and frozen preservation resources as raw materials to prepare easy-to-eat foods, thereby increasing the added value of the product.
- the composite gel prepared by the present invention is used as a 3D printing additive, combined with 3D printing molding technology, to satisfy consumers' needs.
- the nutrition, taste and appearance requirements of food can increase consumers' appetite and realize the personalized form customization of fish and meat products.
- Figure 1 is a microstructure diagram of the composite gel prepared in Example 1 of the present invention.
- Figure 2 is an actual picture of the IDDSI test and evaluation of the composite gel prepared in Example 1 of the present invention.
- Figure 3 is an actual picture of the IDDSI test and evaluation of the composite gel prepared in Comparative Example 1 of the present invention.
- Figure 4 is an actual picture of the composite gel 3D printed product prepared in Example 2 of the present invention.
- Figure 5 shows the state of digesta of samples prepared in Example 3, Example 4, Comparative Example 2, and Comparative Example 3 of the present invention after passing through the dynamic in vitro digestion system (DIVHS).
- DIVHS dynamic in vitro digestion system
- Figure 6 is a gastric emptying curve of samples prepared in Example 4, Comparative Example 2, and Comparative Example 3 of the present invention.
- Figure 7 is an actual picture of the composite gel 3D printed product prepared in Comparative Example 6 of the present invention.
- Figure 8 is an actual picture of the composite paste 3D printed product prepared in Comparative Example 7 of the present invention.
- Gel strength measurement method Use the P/0.5S probe to conduct a puncture experiment, and determine the maximum force (N) induced when the probe penetrates to a gel depth of 15 mm as the gel strength of the sample.
- the pre-test speed is set to 10.0mm/s
- the test speed is set to 1.0mm/s
- the post-test speed is set to 1.0mm/s
- the trigger force is 3.0g.
- the storage modulus is measured as follows : using a rotational rheometer and a parallel plate fixture (40mm in diameter), frequency scanning (Oscillation Frequency) mode, and conducting an oscillation experiment at a frequency of 0.1 to 100rad/s to obtain the sample energy storage modulus.
- the water/oil retention rate is measured using the centrifugal method : put the sample into a 10 mL centrifuge tube, and centrifuge at 5000 rpm for 10 minutes in a high-speed refrigerated centrifuge at 4°C. Remove the supernatant and record the weight of the gel in the tube. Calculated as follows:
- Dynamic in vitro digestion test Gastrointestinal digestion of different samples was performed in the dynamic in vitro digestion system (DIVHS), and gastric emptying curves were produced for comparative analysis. Take 100g of the sample and mix it with an equal mass of artificial saliva in a food processor and stir at low speed for 100 seconds to obtain a food mass. Put the food bolus after simulated oral processing into the DIVHS with the help of a conical funnel, and start the electromechanical equipment immediately. One minute before the sample enters the stomach, 30 mL of simulated gastric juice flows into the empty stomach model to simulate cavity digestion.
- DIVHS dynamic in vitro digestion system
- the simulated gastric juice (purchased from Shanghai Yuanye Biotechnology Co., Ltd.) was formulated according to the Chinese Pharmacopoeia and contained dilute hydrochloric acid, sodium chloride and pepsin with a pH of 1.2, in which the pepsin activity was 3000U/MG. After 180 minutes, the stomach roller pressed the stomach model, and the speed of the gastric peristalsis device was 500mm/min. At the same time, through the extrusion of the peristaltic pump, the simulated gastric juice is secreted into the stomach model, and the flow rate is as shown in the table below. As the sample gradually enters the simulated small intestine for digestion during gastric emptying, the simulated intestinal fluid flow rate is as shown in the table below.
- the simulated intestinal fluid (purchased from Shanghai Yuanye Biotechnology Co., Ltd.) contains potassium dihydrogen phosphate, sodium hydroxide and trypsin (250U/mg) according to the Chinese Pharmacopoeia, with a pH of 6.8. On this basis, bile salts are added (the final concentration is 2.6mg/mL).
- y(t) is the remaining percentage in the stomach at digestion tmin; k is the gastric emptying rate per minute during digestion; ⁇ is the curve intercept fitted by the nonlinear least squares method.
- the gastric half-emptying time (t 1/2 ) is calculated as follows, which is the time when y(t) is 50%:
- Preparation of fish meat Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the rinse mixture through 60 mesh Pre-prepared fish meat is filtered through nylon filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material, wherein the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg:1.4 kg: 160g: 70g;
- One-step emulsion filling-protein cross-linking subject the compound material described in step S3 to high-pressure shearing treatment, and simultaneously add the functional grease described in step S4 during the high-pressure shearing treatment to obtain a composite gel: the pressure is 40MPa, the corresponding high-pressure shearing treatment time for each 100g of compound material is 9 minutes, and the mass ratio of compound material to functional grease is 85kg:15kg.
- the gel strength of the obtained composite gel is about 0.5N
- the storage modulus is between 166 and 260Pa
- the water/oil holding rate is about 98%.
- the composite gel has a clear protein network structure, and functional oils are evenly distributed in the network in the form of oil droplets, proving that the one-step emulsion filling-protein cross-linking technology of the present invention combined with step S5 successfully achieves simultaneous construction Protein gel network structure, and the effect of "embedding" functional oils in the network structure.
- the spoon drop test and the fork drop test show that the composite gel can maintain its shape well on the spoon;
- the fork pressure test shows that it can be broken with the front end of the fork using a weak force. and will not restore its original shape, indicating that the composite gel constructed by the present invention combined with the one-step emulsion filling-protein cross-linking technology in step S5 meets the "soft type" characteristics in the "Easy to Eat Food” standard, and can be suitable for the elderly, young children, etc. who have special needs for food texture. Crowd consumption.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 120g: 120g;
- step S5 One-step emulsion filling-protein cross-linking:
- the compound material described in step S3 is subjected to high-pressure shearing treatment, and the functional grease described in step S4 is added simultaneously during the high-pressure shearing treatment to obtain a composite gel;
- the pressure is 40MPa
- the corresponding high-pressure shearing treatment time for each 100g of compound material is 9 minutes
- the mass ratio of compound material to functional grease is 90kg:10kg;
- step S6 Use the composite gel described in step S5 as a 3D printing raw material for 3D printing: the brand and model of the 3D printer is Shiyin Technology FoodBot-D2, and introduce the composite gel described in step S5 into the feed of the 3D printer.
- the printing model for printing select the nozzle diameter as 0.84mm, the printing speed as 20mm/s, the extrusion force as 2 ⁇ 7N, and the printing environment temperature as 25°C.
- step S7 Shaping: Place the composite gel with a three-dimensional shape printed in step S6 at 20°C for 10 minutes to set the shape to increase the elasticity and water retention of the composite gel.
- the gel strength of the composite gel obtained in step S5 of Example 2 is about 0.6N
- the storage modulus is between 150 and 230 Pa
- the water/oil holding rate is about 98%.
- the composite gel obtained in step S5 of Example 2 can be 3D printed according to the shape of the designed model.
- the 3D printed product has good accuracy and shape, indicating that the present invention combines the one-step emulsion filling of step S5.
- the composite gel prepared by protein cross-linking technology has the ability to be used as a 3D printing additive.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:100 (g/mL), rinse 3 times in a 60°C environment, 3 minutes each time, and pass the mixture through 60 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat and water described in step S2 to obtain a compound material.
- the mass ratio of the prefabricated fish meat and water is 1kg:1.4kg;
- step S4 One-step emulsion filling-protein cross-linking:
- the compound material described in step S3 is subjected to high-pressure shearing treatment.
- linseed oil was added at the same time to obtain a composite gel: the pressure was 40MPa, the high-pressure shearing treatment time for each 100g of the compound material was 9 minutes, and the mass ratio of the compound material to linseed oil was 90kg:10kg.
- Example 3 The composite gel prepared in Example 3 was subjected to a dynamic in vitro digestion test. The results are shown in Figure 5. At 0 min of digestion, it was observed under a microscope that Example 3 had a compact structure, and the average particle size of the sample was less than 15 ⁇ m. As the digestion time increases, the particle size in the sample gradually decreases, and voids can be observed on the surface of cod microfibers. At the end of digestion (180 min), it can be observed that the particle size of digested chyme in Example 3 is significantly reduced, and the average particle size is 5.86 ⁇ m after calculation and analysis.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-to-liquid ratio of 1:100 (g/mL), rinse it 10 times in a 60°C environment, 5 minutes each time, and pass the mixture through 100 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 160g: 70g;
- step S4 One-step emulsion filling-protein cross-linking:
- the compound material described in step S3 is subjected to high-pressure shearing treatment, and linseed oil is added simultaneously during the high-pressure shearing treatment to obtain a composite gel: the pressure is 40MPa, and the complex gel is added per 100g.
- the corresponding high-pressure shearing treatment time of the compound material is 9 minutes; the mass ratio of the compound material and linseed oil is 90kg:10kg.
- Example 4 The composite gel prepared in Example 4 was subjected to a gastric emptying curve test, and the composite gel prepared in Example 4 was subjected to a dynamic in vitro digestion test. As shown in Figure 5, at 0 min of digestion, the Example was observed under the microscope 4 has a compact structure. At the end of digestion (180 min), it can be observed that the particle size of the digested chyme of Example 4 dropped to 5.36 ⁇ m.
- the gastric half-emptying time (t 1/2 ) of Example 4 is approximately 93.80 minutes.
- the composite gel obtained in Examples 1-4 has both low gel strength (gel strength is 0.1-1.5N or storage modulus is 150-260Pa) and high water-holding/oil property (water-holding capacity). / oil rate is greater than or equal to 90%).
- the obtained composite gel has easy-to-eat properties at room temperature and can provide highly nutritious, soft gel-like easy-to-eat foods for special groups such as the elderly and patients with dysphagia. It can also be used as a 3D printing additive to achieve personalized form customization using 3D printing technology.
- step S5 the only difference is that the high-pressure shearing process in step S5 is replaced by a high-speed shearing process.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-to-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 60 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 160g: 70g;
- step S5 The compound material described in step S3 and the functional grease described in S4 are sheared at high speed (shearing rate is 3000rpm/min, time is 9 minutes).
- the mass ratio of the compound material to functional grease is 85kg. :15kg in an attempt to prepare a composite gel.
- step S5 It was found that the composite material obtained in step S5 was in the form of slurry, and the gel could not be successfully prepared at all. Even if the shear rate, time and other parameters of high-speed shearing are optimized, the gel cannot be successfully prepared at all.
- the storage modulus of the obtained composite slurry ranges from 1.2 to 12 Pa, and the water/oil holding rate is approximately 65%.
- the composite material prepared by high-speed shearing is fluid and slurry-like. Most samples fall off after the spoon is tilted, and a large number of samples remain on the surface of the spoon (obvious wall-hanging characteristics); this sample can easily flowing through the gaps between the fork tines indicates that the sample may have a certain amount of residue in the mouth during swallowing, which is not conducive to consumption by the elderly and other people with swallowing disorders.
- Example 4 the only difference is that the addition of inulin and soybean dietary fiber is omitted during nutritional adjustment of the fish base, and high-speed shearing treatment is used instead of high-pressure shearing treatment.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:100 (g/mL), rinse it 10 times in a 60°C environment, 5 minutes each time, and pass the mixture through 100 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat and water described in step S2 to obtain a compound material.
- the mass ratio of the prefabricated fish meat and water is 1kg:1.4kg;
- step S4 High-speed shearing: Shear the compound material and linseed oil described in step S3 at high speed (shearing rate is 3000rpm/min, time is 9min). The mass ratio of the compound material and linseed oil is 90kg:10kg. An attempt was made to prepare a composite gel, but the sample state had fluidity similar to that of Comparative Example 1 and did not have gel properties.
- Comparative Example 2 had obvious fish fiber particles with a particle size greater than 40 ⁇ m. At the end of digestion (180 min), it was observed that the particle size of the digested chyme of Comparative Example 2 dropped to 14.99 ⁇ m. .
- the gastric half-emptying time (t 1/2 ) of Comparative Example 2 was calculated to be approximately 103.76 minutes.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:100 (g/mL), rinse it 10 times in a 60°C environment, 5 minutes each time, and pass the mixture through 100 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a complex Preparing materials, the mass ratio of the prefabricated fish, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 160g: 70g;
- step S4 High-speed shearing: Shear the compound material and linseed oil described in step S3 at high speed to obtain compound slurry: the shearing rate is 3000rpm/min, the time is 9min; the mass ratio of the compound material and linseed oil is 90kg: 10kg; in an attempt to prepare a composite gel, but the sample state has fluidity similar to that of Comparative Example 1 and does not have gel properties.
- Example 2 the only difference is that the traditional method of first mixing materials and then high-pressure shearing treatment is used instead of the one-step emulsion filling-protein cross-linking treatment.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 120g: 120g;
- step S5 Traditional high-pressure shearing: First, fully mix the compound material described in step S3 and the functional grease described in step S4, and then undergo high-pressure shearing treatment to try to obtain a composite gel: the pressure is 40MPa, compounded per 100g The corresponding high-pressure shearing treatment time of the material is 9 minutes; the mass ratio of compound material and functional grease is 90kg:10kg.
- Example 2 the only difference is that the prefabricated fish, water, inulin and soy dietary fiber composite materials are first sheared under high pressure to prepare a protein gel, and then combined with oil through high pressure shearing in an attempt to prepare a composite gel.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg: 1.4kg: 120g: 120g;
- step S3 Each 100g of the compound material described in step S3 is subjected to high-pressure shearing at a pressure of 40MPa for 5 minutes. Obtain protein gel;
- Preparation of composite gel Mix the protein gel described in step S4 and the functional oil described in step S5, and perform a high-speed shearing process at a rotation speed of 3000 rpm/min for 4 minutes.
- the mass ratio of the compound material to the functional oil For 90kg: 10kg.
- the sample prepared was white paste, with stratification, and the water/oil holding rate was lower than 95%.
- soybean dietary fiber is first replaced with chia seeds.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and chia seeds to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and chia seeds is 1kg: 1.4kg: 120g: 120g;
- step S5 One-step emulsion filling-protein cross-linking:
- the compound material described in step S3 is subjected to high-pressure shearing treatment, and the functional grease described in step S4 is added simultaneously during the high-pressure shearing treatment to obtain a composite gel;
- the pressure is 40MPa
- the corresponding high-pressure shearing treatment time for each 100g of compound material is 9 minutes
- the mass ratio of compound material to functional grease is 90kg:10kg.
- step S6 Printing: Use the composite gel described in step S5 as a 3D printing raw material for printing;
- step S7 Shaping: Place the composite gel with a three-dimensional shape printed in step S6 at 20°C for 10 minutes to set the shape to increase the elasticity and water retention of the composite gel.
- Example 2 the only difference is that the soybean dietary fiber is replaced with quinoa flour, and appropriate temperature and resting time are used during shaping.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and quinoa flour to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and quinoa flour is 1kg:1.4kg. :120g:120g;
- One-step emulsion filling-protein cross-linking subject the compound material described in step S3 to high-pressure shearing treatment, and simultaneously add the functional grease described in step S4 during the high-pressure shearing treatment to obtain a composite paste; the pressure is 40MPa, the corresponding high-pressure shearing treatment time for each 100g of compound material is 9 minutes, and the mass ratio of compound material to functional grease is 90kg:10kg.
- step S6 Printing: Use the composite paste described in step S5 as a 3D printing raw material for 3D printing;
- step S7 Shaping: Place the three-dimensional composite paste printed in step S6 at 4°C for 10 minutes to finalize the shape to increase the elasticity and water retention of the composite paste.
- the composite paste obtained in step S5 of Comparative Example 7 has a water/oil holding ratio of approximately 98%, but does not have a gel shape. After the composite paste is extruded through the 3D nozzle, the printed product does not have the shape of the designed model and collapses (as shown in Figure 8).
- soybean dietary fiber is first replaced with konjac gum.
- step S2 Preparation of fish meat: Mix the cooked fish meat obtained in step S1 with 0.1% NaCl solution according to the material-liquid ratio of 1:50 (g/mL), rinse it 5 times in a 60°C environment, 1 minute each time, and pass the mixture through 80 mesh nylon Filter the pre-made fish meat through filter cloth;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and konjac gum to obtain a compound material.
- the mass ratio of the prefabricated fish meat, water, inulin and konjac gum is 1kg:1.4kg :120g:120g;
- One-step emulsion filling-protein cross-linking subject the compound material described in step S3 to high-pressure shearing treatment, and simultaneously add the functional grease described in step S4 during the high-pressure shearing treatment to obtain a composite paste; the pressure is 40MPa, the estimated time for high-pressure shearing treatment per 100g of compound material is 9 minutes, and the mass ratio of compound material to functional grease is 90kg:10kg.
- Example 1 Referring to Example 1, the only difference is that unripened minced fish meat is used.
- Thaw fish meat Thaw minced cod meat for 12 hours at 4°C to obtain fish meat;
- Preparation of fish meat Mix the fish meat obtained in step S1 with 0.1% NaCl solution according to the material-to-liquid ratio of 1:50 (g/mL). Rinse 5 times in a 60°C environment, 1 minute each time, and filter the rinsing mixture through a 60-mesh nylon filter cloth to obtain premade fish meat;
- Nutritional control of fish meat base Mix the prefabricated fish meat described in step S2 with water, inulin and soybean dietary fiber to obtain a compound material, wherein the mass ratio of the prefabricated fish meat, water, inulin and soybean dietary fiber is 1kg:1.4 kg: 160g: 70g;
- step S5 One-step emulsion filling-protein cross-linking:
- the compound material described in step S3 is subjected to high-pressure shearing treatment, and the functional grease described in step S4 is simultaneously added during the high-pressure shearing treatment to obtain a composite sample: the pressure is 40MPa , the high-pressure shearing treatment time for each 100g of compound material is 9 minutes, and the mass ratio of compound material to functional grease is 85kg:15kg.
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Abstract
一种基于高压剪切诱导制备具有易食特性复合凝胶,其制备方法包括:鱼肉加热熟化;将熟鱼肉与盐溶液混合,漂洗,过滤得预制鱼肉;将预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:(1~3)kg:(0~200)g:0~150)g;将复配物料经高压剪切处理,在剪切过程中同时添加功能性油脂,得到复合凝胶,复配物料与功能性油脂的质量比为(85~90)g:(15~10)g。所述方法通过乳液填充-蛋白交联来控制热变性蛋白交联程度与功能性油脂结合程度,制备的复合凝胶强度低,持水/油率高,具有"软质型"易食食品特性,所述复合凝胶可通过3D打印制成不同的形状。
Description
本发明涉及一种基于高压剪切诱导制备具有易食特性复合凝胶的方法,属于食品加工技术领域。
21世纪以来,我国老年人口数呈现快速增长的趋势,老年化程度进一步加深。随着年龄的增加,机体功能逐渐衰退,易出现咀嚼能力减弱、牙齿脱落、唾液分泌不充分等现象,使得多数老年人存在咀嚼和吞咽功能下降的问题,对食物选择受到限制、食欲降低,对其身心健康产生重要的影响。《中国居民膳食指南》针对老年人膳食主要建议提高食物多样性,食物制作应细软,注意精准营养调控,这促使老年膳食的消费从温饱型转变为营养健康型,研创适合的食品以满足老年人特殊的生理特点和营养需求。食品质地改良技术可降低多数老年人吞咽障碍发生率,已被认为是提高老年吞咽障碍者生活品质和保证吞咽安全性的有效手段。因此,为满足消费者对特殊营养、质构的个性化饮食需求,易食食品加工技术创新已成为社会及食品工业研究方向。
发明内容
本发明的目的是克服现有功能食品可能产生的吞咽不畅或食管积留的缺点,与功能活性物质在蛋白基凝胶中不稳定等问题,提供一种基于高压剪切诱导制备具有易食特性复合凝胶的方法,利用高压剪切作用破碎海洋优质蛋白并促使蛋白分子交联形成高保水性网络结构,并同时将载有功能活性成分的油脂镶嵌在蛋白凝胶网络中,最终得到兼具低凝胶强度(凝胶强度在0.1~1.5N或储能模量在150~260Pa)、高持水/油性的复合凝胶(持水/油率大于等于90%)。所得的复合凝胶在室温下具有易食特性,可以为老年人、吞咽困难患者等特殊人群提供高营养、软质凝胶状易食食品,该食品还可做为增材借助3D打印技术实现个性化形态定制。
本发明的第一目的在于提供一种基于高压剪切诱导制备具有易食特性复合凝胶的方法,包括如下步骤:
S1、熟化:取原料鱼的鱼肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉与盐溶液混合,漂洗,过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所得预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:(1~3)kg:(0~200)g:0~150)g;
S4、油脂的功能化:将液态油脂与脂溶性营养素混合,得到功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所得复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合凝胶;压力为20~100MPa,每100g复配物料对应高压剪切处理时间为4~15min,复配物料与功能性油脂的质量比为(85~90)g:(15~10)g。
在一种实施方式中,步骤S2中熟鱼肉与盐溶液的料液比为:1:10~1:1000g/mL。
在一种实施方式中,盐溶液为0.01%~0.2%NaCl溶液。
在一种实施方式中,步骤S2中漂洗温度为40~70℃,漂洗3-10次,每次1~5min。
在一种实施方式中,步骤S1中原料鱼为鳕鱼或鲟鱼;加热熟化是在60~100℃加热5~30min。
在一种实施方式中,步骤S2中的过滤是采用60~100目滤布过滤。
在一种实施方式中,步骤S1中的原料鱼是鲜活原料鱼宰杀后及时去皮去骨去内脏,得鱼肉;宰杀后的鱼体若不能及时处理,需将鱼体低温冷却,使鱼体温迅速下降,再于4~6℃低温保存,待鱼体完全僵直后在0℃左右保存鱼体;冷藏后的鱼体若不能及时熟化,需将鱼体置于-80~-20℃冷冻保存。
在一种实施方式中,步骤S1所述的原料鱼是冷冻原料鱼的鱼肉,冷冻的鱼体需缓化后去皮去骨去内脏,得鱼肉。
在一种实施方式中,步骤S3中的水是纯净水或矿泉水。
在一种实施方式中,步骤S4中的脂溶性营养素包括但不限于维生素E、类胡萝卜素。
在一种实施方式中,步骤S4中的液态油脂包括但不限于亚麻籽油、橄榄油。
在一种实施方式中,步骤S4中液态油脂与脂溶性营养素的混合比为1kg:(0.005~0.3)g。
在一种实施方式中,步骤S4中的液态油脂与维生素E、类胡萝卜素的质量比为1kg:(0.1~0.2)g:(0~0.06)g。
在一种实施方式中,步骤S5中高压剪切处理时的压力为40MPa,每100g复配物料对应高压剪切处理时间为9min。
在一种实施方式中,在步骤S5之后还包括:S6、将步骤S5所得复合凝胶包装、灭菌、密封,冷却至室温得易食特性复合凝胶食品。
在一种实施方式中,步骤S6中包装所采用的容器包括但不限于金属罐或复合材料袋/罐。
在一种实施方式中,步骤S6中的灭菌方式包括但不限于低温长时杀菌、辐照灭菌中的至少一种;具体地,低温长时杀菌条件具体为:温度60~80℃,时间15~30min;辐照灭菌条件具体为:1~10kGy。
在一种实施方式中,步骤S6所得易食特性复合凝胶食品的保存温度为2~10℃。
本发明的第二目的在于提供前述方法制得的具有易食特性复合凝胶。
在一种实施方式中,具有易食特性复合凝胶的凝胶强度0.1~1.5N,储能模量在150~260Pa,持水/油率不低于98%。经过3D打印后的制品具有良好的精度和形态。胃半排空时间(t1/2)不高于150min。
本发明的第二目的在于提供具有易食特性复合凝胶在3D打印领域中的应用。
本发明提供的具有易食特性复合凝胶在3D打印中的应用,包括如下步骤:
(1)打印:使用前述具有易食特性复合凝胶为3D打印原料,进行3D打印;
(2)定型:将步骤(1)打印的具有立体形状的凝胶于0~25℃静置10~30min定型,以增加易食特性的复合凝胶的弹性和保水性。
优选方式下,步骤(1)中的3D打印:3D打印机的品牌及型号为时印科技FoodBot-D2,将具有易食特性复合凝胶导入到3D打印机的进料筒中,选择打印模型进行打印,选择喷嘴直径为0.8~1.8mm,打印速度为15~30mm/s,挤出力为2~7N,打印环境温度为4~25℃。
本发明的有益效果是:
1、本发明创造性地提出了一步法乳液填充-蛋白交联的方法,即将复配物料经高压剪切处理,在高压剪切处理过程中同时添加功能性油脂,得到复合凝胶;通过设置合理的压力和剪切时间,控制热变性蛋白颗粒大小与凝胶网络交联程度,利用高压剪切作用破碎海洋优质蛋白并促使蛋白分子交联形成高保水性网络结构,同时将功能性油脂“镶嵌”在复合凝胶网络结构中,不仅实现了脂溶性营养素的包埋,而且提高了复合凝胶的锁水能力,实现高效控制持水/油率超过90%,提高了功能性油脂在易食特性复合凝胶食品中的稳定性;综合调控产品的凝胶强度为0.1~1.5N,储能模量为150~260Pa,在室温下具有易食特性,可以为老年人、吞咽困难患者等特殊人群提供高营养、软质凝胶状易食食品;克服了现有功能食品可能产生的吞咽不畅或食管积留的缺点,解决了功能活性物质在蛋白基凝胶中不稳定等问题。
2、本发明通过将熟鱼肉置于盐溶液中漂洗处理对鱼肉进行预制,有助于降低后续高压剪切的压力,降低能耗,增加凝胶产量。
3、本发明通过大量试验发现,在鱼肉基的营养调控步骤中,与鱼肉复配的膳食纤维的选择对于复合凝胶产品的3D打印性能会产生重大影响:基于本发明方法,只有选用本发明的特定复配组合——预制鱼肉与水、菊粉和大豆膳食纤维,结合特定的配比,制得的复合凝胶才具有良好的3D打印性能,经过3D打印后的制品具有良好的精度和形态;而采用奇亚籽、藜麦粉或魔芋胶所得的复合凝胶不适于3D打印或根本难以成功制备得到凝胶产品。
4、本发明涉及鱼肉基的营养调控,提高了产品的营养特性的同时,制得的复合凝胶具有
良好的3D打印性能,经过3D打印后的制品具有良好的精度和形态,3D打印后仍可维持高的持水/油率。
5、本发明充分提高海洋资源的利用率,可以利用加工剩余一些碎肉、冷冻保存资源为原料制备得到易食食品,提高产品附加值。
6、针对凝胶类增材在3D制造过程中的高效稳定性、特殊质构等方面的要求,以本发明制备的复合凝胶作为3D打印增材,结合3D打印成型技术,满足消费者对食品的营养、滋味和外观需求,提高消费者食欲,实现鱼肉产品的个性化形态定制。
图1是本发明实施例1制备的复合凝胶微观结构图。
图2是本发明实施例1制备的复合凝胶IDDSI测试评估实图。
图3是本发明对比例1制备的复合凝胶IDDSI测试评估实图。
图4是本发明实施例2制备的复合凝胶3D打印制品实图。
图5是本发明实施例3、实施例4、对比例2、对比例3制备的样品经过动态体外消化系统(DIVHS)食糜状态。
图6是本发明实施例4、对比例2、对比例3制备的样品胃排空曲线。
图7是本发明对比例6制备的复合凝胶3D打印制品实图。
图8是本发明对比例7制备的复合膏体3D打印制品实图。
测试方法:
凝胶强度测定方法:使用P/0.5S探头进行穿刺实验,将探头穿透至凝胶深度15mm过程中感应到的最大力(N)认定为样品的凝胶强度。测前速度设置为10.0mm/s,测试速度设置为1.0mm/s,测后速度设置为1.0mm/s,触发力为3.0g。
储能模量按如下方法测定:采用旋转流变仪和平行板夹具(直径为40mm),频率扫描(Oscillation Frequency)模式,在频率为0.1~100rad/s下进行振荡实验,以获得样品储能模量。
持水/油率使用离心法测定:将样品放入10mL离心管中,采用高速冷冻离心机在4℃条件下5000rpm离心10min。去除上清液,记录管中凝胶的重量。计算公式如下:
上式中m0:空离心管质量(g);m1:样品及离心管总质量(g);m2:离心后沉淀及离
心管总质量(g)。
动态体外消化测试:在动态体外消化系统(DIVHS)中对不同样品进行胃肠消化,并制作胃排空曲线进行对比分析。取样品100g与等质量的人工唾液在食品料理机中混合,低速搅拌100s,得到食团。将模拟口腔加工后的食团借助锥形漏斗放入DIVHS,立即启动机电设备。样品进入胃前1min,30mL模拟胃液流入到空胃模型中,模拟空腔消化。模拟胃液(购自上海源叶生物科技有限公司)配比根据中国药典,含有稀盐酸、氯化钠和胃蛋白酶,pH 1.2,其中胃蛋白酶活力为3000U/MG。此后180min,胃部滚轮对胃模型进行按压,胃蠕动装置速率为500mm/min。与此同时,通过蠕动泵的挤压,模拟胃液随分泌至胃模型内,流速如下表所示。随着样品在胃排空的过程中逐渐进入模拟小肠进行消化,模拟肠液流动速率如下表所示。模拟肠液(购自上海源叶生物科技有限公司)配比根据中国药典含有磷酸二氢钾、氢氧化钠和胰蛋白酶(250U/mg),pH 6.8,在此基础上添加胆盐(终浓度为2.6mg/mL)。
表1动态体外消化系统运行参数
样品胃排空曲线测试:
取动态体外消化系统(DIVHS)消化过程中的样品(每15min从胃中取样),冷冻干燥后称量干燥前后消化液的重量。分别计算收集物中干物质含量的比值,即样品消化过程中胃内剩余百分比(retentionpercentage,%)。利用Elashoff幂指模型描述样品的胃排空情况:
y(t)=1-(1-e-kt)β
y(t)=1-(1-e-kt)β
上式中,y(t)为消化tmin时胃内剩余百分比;k为消化过程中每分钟的胃排空率;β为非线性最小二乘法拟合的曲线截距。
胃的半排空时间(t1/2)的计算方式如下,即y(t)为50%时的时间:
实施例1
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将漂洗混合物通过60目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,其中预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:160g:70g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合凝胶:压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与功能性油脂质量比为85kg:15kg。
经测试,所得复合凝胶的凝胶强度约为0.5N,储能模量在166~260Pa,持水/油率约为98%。
如图1所示,复合凝胶具有清晰的蛋白网络结构,且功能性油脂以油滴形式均匀分布在网络中,证明本发明结合步骤S5的一步法乳液填充-蛋白交联技术成功同步实现构建蛋白凝胶网络结构,并将功能性油脂“镶嵌”在网络结构中的效果。
如图2所示,勺子滴落测试及叉子滴落测试表明,复合凝胶在勺子上能够较好地维持其自身形态;叉子下压测试表明,使用微弱的力即可用叉子前端使其破碎,且不会恢复其原有
形状,说明本发明结合步骤S5的一步法乳液填充-蛋白交联技术构建的复合凝胶符合《易食食品》标准中“软质型”特性,可适宜老年、幼儿等对食品质地有特殊需求人群食用。
实施例2
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:120g:120g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合凝胶;压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与功能性油脂质量比为90kg:10kg;
S6、打印:将步骤S5所述复合凝胶作为3D打印原料,进行3D打印:3D打印机的品牌及型号为时印科技FoodBot-D2,将步骤S5所述复合凝胶导入到3D打印机的进料筒中,选择打印模型进行打印,选择喷嘴直径为0.84mm,打印速度为20mm/s,挤出力为2~7N,打印环境温度为25℃。
S7、定型:将步骤S6打印的具有立体形状的复合凝胶于20℃,静置10min定型,以增加复合凝胶的弹性和保水性。
经测试,实施例2的步骤S5所得复合凝胶的凝胶强度约为0.6N,储能模量在150~230Pa,持水/油率约为98%。
如图4所示,实施例2的步骤S5所得复合凝胶可依据设计模型的形状实现3D打印,经过3D打印后的制品具有良好的精度和形态,说明本发明结合步骤S5的一步法乳液填充-蛋白交联技术制备得到的复合凝胶具有作为3D打印增材的能力。
实施例3
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:100(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗3次,每次3min,将混合物通过60目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水混合得复配物料,所述预制鱼肉、水的质量比是1kg:1.4kg;
S4、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切
处理过程中同时添加亚麻籽油,得到复合凝胶:压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与亚麻籽油质量比为90kg:10kg。
对实施例3制得的复合凝胶进行动态体外消化测试,结果如图5所示,消化0min时,在镜下观察到实施例3具有紧密的结构,样品的平均粒度小于15μm。随着消化时间的延长,样品中颗粒粒度逐渐减小,且可以在鳕鱼微纤维表面观察到空隙。消化末期(180min),可以观察到实施例3消化食糜粒度显著减小,经计算分析其平均粒度为5.86μm。
实施例4
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:100(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗10次,每次5min,将混合物通过100目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:160g:70g;
S4、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加亚麻籽油,得到复合凝胶:压力为40MPa,每100g复配物料对应高压剪切处理时间为9min;复配物料与亚麻籽油质量比为90kg:10kg。
对实施例4制得的复合凝胶进行胃排空曲线测试,对实施例4制得的复合凝胶进行动态体外消化测试,如图5所示,消化0min时,在镜下观察到实施例4具有紧密的结构,消化末期(180min),可以观察到实施例4消化食糜粒度降至为5.36μm。
根据图6胃排空曲线计算得出实施例4的胃半排空时间(t1/2)约为93.80min。
经测试,实施例1-4所得复合凝胶兼具低凝胶强度(凝胶强度在0.1~1.5N或储能模量在150~260Pa)、高持水/油性的复合凝胶(持水/油率大于等于90%)。所得的复合凝胶在室温下具有易食特性,可以为老年人、吞咽困难患者等特殊人群提供高营养、软质凝胶状易食食品。还可做为3D打印增材借助3D打印技术实现个性化形态定制。
对比例1
参照实施例1,区别仅在于,将步骤S5的高压剪切处理替换为高速剪切处理。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过60目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:160g:70g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、高速剪切:将步骤S3所述复配物料与S4所述的功能性油脂高速剪切(剪切速率为3000rpm/min,时间为9min),复配物料与功能性油脂质量比为85kg:15kg,以试图制备复合凝胶。
结果发现,步骤S5得到的复合材料呈浆料状,根本无法成功制备得到凝胶。即使对高速剪切的剪切速率、时间等参数进行优化,也根本无法成功制备得到凝胶。
经测试,所得复合浆料的储能模量在1.2~12Pa,持水/油率约为65%。
如图3所示,高速剪切制备得到的复合材料具有流动性,呈浆料状,在勺子倾斜后多数样品掉落,并在勺子表面残留较多样品(明显挂壁特性);该样品能够轻易流动穿过叉子齿间的缝隙,表明样品在吞咽过程中可能在口腔中有一定的残留,这不利于老年等患有吞咽障碍人群食用。
对比例2
参照实施例4,区别仅在于:鱼肉基的营养调控时省略菊粉和大豆膳食纤维的添加,采用高速剪切处理替代高压剪切处理。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:100(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗10次,每次5min,将混合物通过100目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水混合得复配物料,所述预制鱼肉、水的质量比是1kg:1.4kg;
S4、高速剪切:将步骤S3所述复配物料与亚麻籽油高速剪切(剪切速率为3000rpm/min,时间为9min),复配物料与亚麻籽油质量比为90kg:10kg,以试图制备复合凝胶,但样品状态具有流动性与对比例1相近,且不具有凝胶性状。
如图5所示,消化0min时,在镜下观察到对比例2具有明显的鱼肉纤维颗粒,粒度大于40μm,消化末期(180min),可以观察到对比例2消化食糜粒度降至为14.99μm。
根据图6胃排空曲线计算得出对比例2的胃半排空时间(t1/2)分别约为103.76min。
对比例3
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:100(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗10次,每次5min,将混合物通过100目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复
配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:160g:70g;
S4、高速剪切:将步骤S3所述复配物料与亚麻籽油高速剪切,得复配浆料:剪切速率为3000rpm/min,时间为9min;复配物料与亚麻籽油质量比为90kg:10kg;以试图制备复合凝胶,但样品状态具有流动性与对比例1相近,且不具有凝胶性状。
如图5所示,消化0min时,在镜下观察到对比例3具有明显的鱼肉纤维颗粒,粒度大于对比例2,消化末期(180min),可以观察到对比例3消化食糜粒度降至为10.13μm。根据图6胃排空曲线计算得出对比例3的胃半排空时间(t1/2)分别约为107.80min。
对比例4
参照实施例2,区别仅在于:采用传统的先混合物料再高压剪切处理替代一步法乳液填充-蛋白交联处理。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:120g:120g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、传统高压剪切:先将步骤S3所述复配物料和步骤S4所述的功能性油脂充分混合,再经过高压剪切处理,以试图得到复合凝胶:压力为40MPa,每100g复配物料对应高压剪切处理时间为9min;复配物料与功能性油脂质量比为90kg:10kg。
研究发现:复配物料和功能性油脂先混合再高压剪切处理,样品在处理过程中发生了结团现象,造成仪器堵塞,无法获得凝胶状产品。
对比例5
参照实施例2,区别仅在于:先将预制鱼肉、水、菊粉和大豆膳食纤维复合物料高压剪切制备蛋白凝胶,再与油脂通过高压剪切以试图制备复合凝胶。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:120g:120g;
S4、高压剪切:将步骤S3所述每100g复配物料在40MPa压力下高压剪切处理5min,
得蛋白凝胶;
S5、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S6、复合凝胶的制备:将步骤S4所述的蛋白凝胶和步骤S5所述的功能性油脂混合,在转速为3000rpm/min下高速剪切处理4min,复配物料与功能性油脂质量比为90kg:10kg。
研究发现:复配物料先经过高压剪切处理,再和功能性油脂剪切处理制备得到的样品呈白色膏状,且出现分层现象,且持水/油率低于95%。
对比例6
参照实施例2,区别仅在于:先将大豆膳食纤维替换为奇亚籽。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和奇亚籽混合得复配物料,所述预制鱼肉、水、菊粉和奇亚籽的质量比是1kg:1.4kg:120g:120g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合凝胶;压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与功能性油脂质量比为90kg:10kg。
S6、打印:将步骤S5所述复合凝胶作为3D打印原料,进行打印;
S7、定型:将步骤S6打印的具有立体形状的复合凝胶于20℃,静置10min定型,以增加复合凝胶的弹性和保水性。
经测试,对比例6的步骤S5所得复合凝胶的凝胶强度持水/油率约为98%。然而,复合凝胶在经过3D打印喷嘴过程中,发生了水分析出现象(如图7所示),经过3D打印后的制品虽具有设计模型的形态但不稳定。
对比例7
参照实施例2,区别仅在于:先将大豆膳食纤维替换为藜麦粉,定型时采用适宜的温度和静置时间。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和藜麦粉混合得复配物料,所述预制鱼肉、水、菊粉和藜麦粉的质量比是1kg:1.4kg:120g:120g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合膏体;压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与功能性油脂质量比为90kg:10kg。
S6、打印:将步骤S5所述复合膏体作为3D打印原料,进行3D打印;
S7、定型:将步骤S6打印的具有立体形状的复合膏体于4℃,静置10min定型,以增加复合膏体的弹性和保水性。
经测试,对比例7的步骤S5所得所得复合膏体的持水/油率约为98%,但不具有凝胶状。复合膏体经过3D喷嘴挤出后,打印制品不具有设计模型的形状,发生坍塌现象(如图8所示)。
对比例8
参照实施例2,区别仅在于:先将大豆膳食纤维替换为魔芋胶。
S1、熟化:取解冻鳕鱼碎肉加热熟化,得熟鱼肉;
S2、鱼肉预制:将步骤S1所得熟鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,在60℃环境中漂洗5次,每次1min,将混合物通过80目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和魔芋胶混合得复配物料,所述预制鱼肉、水、菊粉和魔芋胶的质量比是1kg:1.4kg:120g:120g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合膏体;压力为40MPa,每100g复配物料对应高压剪切处理预计时间为9min,复配物料与功能性油脂质量比为90kg:10kg。
研究发现:复配物料经高压剪切处理过程中发生停滞现象,可能是魔芋胶和鱼肉在剪切过程中发生交联,流动性降低,造成高压剪切处理过程中机器停滞,无法获得凝胶状产品。
对比例9
参照实施例1,区别仅在于:使用未经熟化后的碎鱼肉。
S1、鱼肉解冻:取鳕鱼碎肉在4℃环境中解冻12h,得鱼肉;
S2、鱼肉预制:将步骤S1所得鱼肉按照料液比为1:50(g/mL)与0.1%NaCl溶液混合,
在60℃环境中漂洗5次,每次1min,将漂洗混合物通过60目尼龙滤布过滤得预制鱼肉;
S3、鱼肉基的营养调控:将步骤S2所述的预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,其中预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:1.4kg:160g:70g;
S4、油脂的功能化:将亚麻籽油、类胡萝卜素按质量比为1kg:0.01g混合,得功能性油脂;
S5、一步法乳液填充-蛋白交联:将步骤S3所述复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合样品:压力为40MPa,每100g复配物料对应高压剪切处理时间为9min,复配物料与功能性油脂质量比为85kg:15kg。
研究发现:复合样品经高压剪切处理后即使经过冷藏处理,样品仍不具有凝胶状态。
Claims (10)
- 一种基于高压剪切诱导制备具有易食特性复合凝胶的方法,其特征在于,包括如下步骤:S1、熟化:取原料鱼的鱼肉加热熟化,得熟鱼肉;S2、鱼肉预制:将步骤S1所得熟鱼肉与盐溶液混合,漂洗,过滤得预制鱼肉;S3、鱼肉基的营养调控:将步骤S2所得预制鱼肉与水、菊粉和大豆膳食纤维混合得复配物料,所述预制鱼肉、水、菊粉和大豆膳食纤维的质量比是1kg:(1~3)kg:(0~200)g:0~150)g;S4、油脂的功能化:将液态油脂与脂溶性营养素混合,得到功能性油脂;S5、一步法乳液填充-蛋白交联:将步骤S3所得复配物料经高压剪切处理,在高压剪切处理过程中同时添加步骤S4所述的功能性油脂,得到复合凝胶;压力为20~100MPa,每100g复配物料对应高压剪切处理时间为4~15min,复配物料与功能性油脂的质量比为(85~90)g:(15~10)g。
- 根据权利要求1所述的方法,其特征在于,步骤S2中熟鱼肉与盐溶液的料液比为:1:10~1:1000g/mL。
- 根据权利要求1或2所述的方法,其特征在于,盐溶液为0.01%~0.2%NaCl溶液。
- 根据权利要求1-3中任一项所述的方法,其特征在于,步骤S2中漂洗温度为40~70℃,漂洗3-10次,每次1~5min。
- 根据权利要求1所述的方法,其特征在于,步骤S1中原料鱼为鳕鱼或鲟鱼;加热熟化是在60~100℃加热5~30min。
- 根据权利要求1所述的方法,其特征在于,步骤S4中的脂溶性营养素包括维生素E、类胡萝卜素中的至少一种。
- 根据权利要求1所述的方法,其特征在于,步骤S4中的液态油脂包括亚麻籽油。
- 根据权利要求1所述的方法,其特征在于,步骤S4中液态油脂与脂溶性营养素的混合比为1kg:(0.005~0.3)g。
- 权利要求1-8任一所述的方法制得的具有易食特性复合凝胶。
- 权利要求9所述的具有易食特性复合凝胶在3D打印领域中的应用。
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