Double-gel composition, high-temperature-resistant and high-moisture-resistant gel beads capable of protecting lipophilic active ingredients and probiotics as well as preparation method and application of double-gel composition and high-temperature-resistant and high-moisture-resistant gel beads

Abstract

The invention belongs to the technical field of emulsion gel, and particularly relates to a double-gel composition, a high-temperature-resistant and high-moisture-resistant gel bead capable of protecting lipophilic active ingredients and probiotics as well as a preparation method and application of the double-gel composition and the high-temperature-resistant and high-moisture-resistant gel bead. The double-gel composition provided by the invention consists of the low-temperature response gel and the high-temperature response gel, and the gel prepared from the double-gel composition has good tolerance to high temperature and high moisture and can be used for preparing high-temperature-resistant and high-moisture-resistant gel products. The high-temperature-resistant and high-moisture-resistant gel bead provided by the invention is prepared from the double-gel composition and an oil phase containing active ingredients through the steps of shear mixing, dropping pill cooling, crosslinking and the like, the structure of the gel bead is a network gel skeleton structure, and the active ingredients are uniformly distributed in the gel bead. The gel bead has excellent heat resistance, can tolerate heat treatment in a high-moisture environment and under a high-moisture condition, and plays an effective role in protecting active ingredients distributed in a network gel skeleton.

Description

Technical Field

[0001] The invention belongs to the technical field of emulsion gel, and particularly relates to a double gel composition, high temperature and high moisture resistant gel beads capable of protecting lipophilic active ingredients and probiotics, and a preparation method and application thereof. Background Art

[0002] Many lipophilic active substances and probiotic ingredients are usually susceptible to oxidation, degradation and probiotic germination and death in high-moisture environments due to the influence of moisture content and dissolved oxygen in water, which limits their application in food, health food and medicine. Emulsion gel is a system that restricts oil droplets in a three-dimensional solid water network (hydrogel). The formation of the hydrogel network will fix the droplets in the gel structure, thereby preventing the emulsion from flocculation and aggregation, which can greatly improve the stability of the emulsion.

[0003] At present, polysaccharides and protein gels such as sodium alginate and gellan gum are generally used as gel matrices. Emulsion gel beads prepared using polysaccharide cold gelling agents such as sodium alginate and gellan gum can achieve the mechanical properties of the gel by cross-linking with metal cations to form a gel. Although the above-mentioned emulsion gel can achieve the effect of forming a gel-stabilized emulsion, it is difficult to maintain its structural integrity under heat treatment conditions such as high-temperature sterilization, and its mechanical properties such as hardness and elasticity change significantly. Under high-water content processes or storage conditions, the encapsulation ability of the inclusions in the emulsion gel is very poor, and it is generally easy to leak and seep out of grease and encapsulated active ingredients, which is not conducive to the processing and production of products using the emulsion gel, and cannot meet the product quality requirements. Summary of the invention

[0004] In view of the above technical problems, the present invention provides a double gel composition, a high temperature and high moisture resistant gel bead capable of protecting lipophilic active ingredients and probiotics, and a preparation method and application thereof. The gel bead provided by the present invention has a stable structure under high temperature and high moisture conditions, and can protect the active substances loaded therein from leakage under high heat and high moisture environmental conditions.

[0005] In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical solutions: The first aspect of the present invention provides a double gel composition, which is composed of a low-temperature responsive gel and a high-temperature responsive gel, wherein the mass ratio of the low-temperature responsive gel to the high-temperature responsive gel is (5~15):(5~15); the raw material of the low-temperature responsive gel includes gellan gum, and the gellan gum accounts for no less than 20%wt in the low-temperature responsive gel, and the raw material of the high-temperature responsive gel includes at least one of pregelatinized starch, acid-treated starch, hydroxypropyl starch, hydroxypropyl distarch phosphate and oxidized hydroxypropyl starch.

[0006] The double gel composition provided by the present invention is composed of a specific low-temperature responsive gel and a high-temperature responsive gel. The gel made from the double gel composition has good tolerance to both high temperature and high moisture content. It can maintain structural stability not only under high temperature conditions, but also under high moisture conditions and high moisture and high temperature conditions. It can be used to make high temperature and high moisture resistant gel products.

[0007] In the dual gel composition, the raw material types of the low-temperature responsive gel and the high-temperature responsive gel are particularly important. If the raw material of the low-temperature responsive gel is only common sodium alginate, although its basic structure can be kept intact under high temperature conditions, it will stick together under high moisture and high temperature conditions. If other low-temperature responsive gels are used instead, the structure cannot be kept intact after heat treatment. If the high-temperature responsive gel is replaced with other raw materials of heat-responsive gels, the viscosity is easily too high, and it is impossible to prepare a gel product with a good morphology.

[0008] Preferably, the raw materials of the low temperature responsive gel further include at least one of sodium alginate, agar, gelatin, pectin, trehalose, carrageenan, locust bean gum, xanthan gum, gum arabic and guar gum. Gellan gum can be used in combination with the above low temperature responsive gel raw materials to adjust the properties in terms of viscosity, rheology, texture, etc., so that the dual gel composition is suitable for the preparation of different types of gels.

[0009] Further preferably, the raw materials of the low temperature responsive gel include at least one of sodium alginate, carrageenan, agar and gellan gum. Sodium alginate, carrageenan and agar have strong heat resistance and can maintain their original properties without significant changes under high temperature heat treatment conditions. Carrageenan and sodium alginate can cross-link with metal ions to further enhance the gel network.

[0010] Preferably, the raw material of the high temperature response type gel also includes at least one of konjac glucomannan, curdlan, acetate starch, octenyl succinate starch, sodium caseinate and soy protein isolate. The gel network formed by the above high temperature response type gel raw material in water is relatively loose, and effective ingredients can not be fully protected when used alone, wherein the viscosity of konjac glucomannan and curdlan increases with the increase of temperature, and when the addition amount is too high, there will be a situation where the viscosity of the glue is too high, which is unfavorable for gel bead molding. Preferably, konjac glucomannan is adopted.

[0011] The second aspect of the present invention provides a method for preparing high temperature and high moisture resistant gel beads, comprising the following operations: The double gel composition is prepared into a gel with water as a hydrogel phase, the hydrogel phase is mixed with an oil phase containing active ingredients by a high-speed shear dispersion technique, and then dripped into a coolant by a cooling drop pill device to prepare gel beads, the gel beads in the coolant are collected and put into a cross-linking liquid for cross-linking, and after the cross-linking is completed, the gel beads are filtered out and rinsed to obtain the gel beads.

[0012] The gel beads prepared by the above preparation method are not a core-shell structure in which the active ingredient is encapsulated by a gel shell, but a network gel skeleton structure in which the active ingredient is evenly distributed. The schematic diagram of its structure is shown in FIG. Figure 1 shown.

[0013] The gel beads prepared by the above preparation method have excellent heat resistance, can maintain structural stability under high temperature conditions of 90°C-125°C, and can withstand high moisture (such as beverages, including but not limited to fruit juice and fruit juice drinks, tea beverages, coffee beverages, energy drinks, dairy beverages, bitter beverages, plant-based beverages, etc.) environments and heat treatment under high moisture conditions, thereby effectively protecting the active ingredients distributed in the network gel skeleton.

[0014] The preparation method first uses high-speed shearing to fully contact and mix the hydrogel phase and the oil phase to create initial conditions for the formation of gel beads, and then promotes the formation of gel beads through a cooling pellet device. The gel beads are then given heat resistance through a cross-linking process, so that the low-temperature responsive gel in the gel bead component is heat-resistant, thereby obtaining gel beads with good tolerance to high temperature and high moisture.

[0015] In the preparation method, the double gel composition is dispersed in water, heated in a water bath at 85-95°C and stirred until completely dissolved, to obtain a hydrogel phase. Further preferably, the mass percentage concentration of the low temperature responsive gel and the high temperature responsive gel in water is 5%-15%. By adjusting the proportion of water, the gel network density of the hydrogel phase can be adjusted.

[0016] Preferably, the mass ratio of the hydrogel phase to the oil phase is (60-90):(10-40).

[0017] Preferably, the oil phase is composed of an active ingredient and a lipid component, and the mass ratio of the active ingredient to the lipid component is (10-95):(5-90). The active ingredient is dispersed in the lipid component to obtain the oil phase.

[0018] Preferably, the lipid component includes at least one of corn oil, medium chain triglycerides, soybean oil, sunflower oil, hydrogenated vegetable oil, cocoa butter, cocoa butter substitute, palm oil, beeswax, stearic acid, coconut oil, walnut oil, olive oil, fish oil, algae oil, linseed oil and tea oil.

[0019] Preferably, the active ingredient comprises a lipophilic active ingredient or a probiotic.

[0020] Exemplarily, the lipophilic active ingredients include, but are not limited to, at least one of curcumin, lycopene, tocopherol, vitamin A, vitamin D, vitamin K, sterols, carotenoids, quercetin, peppermint oil, linoleic acid, α-linolenic acid, lauric acid, DHA algae oil, EPA (deep sea fish oil) and lutein esters.

[0021] Exemplarily, the probiotics include but are not limited to at least one of Lactobacillus plantarum, Lactobacillus salivarius, Lactobacillus acidophilus, Lactobacillus casei, Lactobacillus paracasei, Lactobacillus rhamnosus, Lactobacillus reuteri, Bifidobacterium animalis subsp. lactis, Bifidobacterium adolescentis, Bifidobacterium longum subsp. longum, Bifidobacterium breve, and Weizmannella coagulans.

[0022] Preferably, the high-speed shearing is performed at a speed of 8000-1000 rpm at a temperature not lower than 80°C and without boiling. The shearing temperature during the preparation process mainly affects the overall viscosity of the glue, and the preparation requirements can be met at a temperature of 80°C or above and without boiling.

[0023] Preferably, the cooling liquid is selected from medium chain triglycerides, corn oil, sunflower oil or soybean oil. Further preferably, medium chain triglycerides are used as the circulating cooling liquid. Medium chain triglycerides are relatively stable in nature, have no special flavor, and have a low overall viscosity.

[0024] In the cooling pill device, the gel solution (i.e., a mixture of the hydrogel phase and the oil phase) is maintained at a temperature of 80-99° C. and the cooling temperature is 10-25° C. The cooling pill device can be a circulating cooling pill device with a circulating cooling device.

[0025] Preferably, the cross-linking liquid is a 0.5% to 5%wt calcium chloride aqueous solution or a calcium lactate aqueous solution.

[0026] The third aspect of the present invention provides high temperature and high moisture resistant gel beads, which are prepared according to the above preparation method.

[0027] The fourth aspect of the present invention provides the use of the high temperature and high moisture resistant gel beads in the preparation of products containing lipophilic active ingredients or probiotics, including but not limited to food and health food.

[0028] The beneficial effects of the present invention are: The double gel composition provided by the present invention can be used as the main raw material for preparing gel products, and the gel products made therefrom can maintain structural stability not only under high temperature conditions, but also under high moisture conditions and high moisture and high temperature conditions. The high temperature and high moisture resistant gel beads provided by the present invention are made of the double gel composition, have excellent heat resistance, and can withstand high moisture environments and heat treatment under high moisture conditions, making up for the poor stability of existing emulsion gel beads in heat treatment, and can effectively protect the active ingredients distributed in its network gel skeleton, so that it is stable in the heat treatment process and does not leak out under high moisture storage conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a schematic diagram of the structure of the gel beads of the present invention; Figure 2 The SEM images of the gel beads obtained in Example 2 and Comparative Example 6 in Test Example 1 of the present invention are shown; Figure 3 The distribution of active ingredients in the gel beads obtained in Example 2 of Test Example 1 of the present invention; Figure 4 These are the bacterial activity test results of the gel beads obtained from Example 1, Example 3, Example 4, Example 5, and Comparative Example 4 in Test Example 3 of the present invention. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work fall within the scope of protection of the present invention.

[0031] The conventional method of using gel to protect active ingredients is usually to make gel raw materials and active ingredients into a core-shell structure, that is, the active ingredient is the core and the gel is the shell. However, gel products with a core-shell structure are often unstable to heat and can only withstand temperatures around 45°C, and cannot withstand higher temperatures; and in the case of high water content and high temperature, gel products with a core-shell structure are more likely to be structurally unstable and cannot effectively protect their contents.

[0032] In view of the above problems, an embodiment of the present invention provides a double gel composition: composed of a low-temperature responsive gel and a high-temperature responsive gel, the mass ratio of the low-temperature responsive gel to the high-temperature responsive gel is (5~15):(5~15); the raw material of the low-temperature responsive gel includes gellan gum, and the gellan gum accounts for no less than 20%wt of the low-temperature responsive gel; the raw material of the high-temperature responsive gel includes at least one of pregelatinized starch, acid-treated starch, hydroxypropyl starch, hydroxypropyl distarch phosphate and oxidized hydroxypropyl starch.

[0033] The embodiment of the present invention also provides a method for preparing high temperature and high moisture resistant gel beads, comprising the following operations: The double gel composition is prepared into a gel with water as a hydrogel phase, the hydrogel phase is mixed with an oil phase containing active ingredients by high-speed shear dispersion technology, and then dripped into a coolant through a cooling drop pill device to prepare gel beads, the gel beads in the circulating coolant are collected and put into a cross-linking liquid for cross-linking, and after the cross-linking is completed, the gel beads are filtered out and rinsed to obtain the gel beads.

[0034] The embodiment of the present invention also provides high temperature and high moisture resistant gel beads made according to the above preparation method.

[0035] The embodiments of the present invention also provide the use of the high temperature and high moisture resistant gel beads in the preparation of products containing lipophilic active ingredients or probiotics.

[0036] The scheme of the present invention is described below through specific embodiments.

[0037] The gellan gum used in the following examples is low acyl gellan gum from Zhejiang Jianlong Biotechnology Co., Ltd.; sodium alginate is purchased from Langfang Pengcai Fine Chemical Co., Ltd.; konjac gum is low-viscosity konjac powder from Jiangsu Jiushun Biotechnology Co., Ltd.; agar is purchased from Anhui Chenshan Food Ingredients Co., Ltd.; hydroxypropyl distarch phosphate is purchased from Henan Fengwei Biotechnology Co., Ltd.; acid-treated starch is purchased from Zhucheng Xingmao Corn Development Co., Ltd.; pregelatinized starch is purchased from Suzhou Zhuoxin Biotechnology Co., Ltd.; soy protein isolate is purchased from Linyi Shansong Biological Products Co., Ltd.; sodium caseinate is purchased from Shenzhen Antai Biotechnology Co., Ltd.; curdlan is purchased from Guangzhou Huiding Food Co., Ltd.; carrageenan is purchased from Henan Anrui Biotechnology Co., Ltd.; octenyl succinate starch is purchased from Zhengzhou Wanbo Chemical Products Co., Ltd.; locust bean gum is purchased from Incom, Turkey.

[0038] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0039] Unless otherwise specified, other materials, reagents, etc. used in the following examples can be obtained from commercial sources.

[0040] Example 1 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: High-temperature responsive gel acid-treated starch and low-temperature responsive gel (a mixture of sodium alginate and gellan gum in a mass ratio of 8:12) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high-temperature responsive gel, the low-temperature responsive gel and water was 12:5:83; probiotics were dispersed in cocoa butter substitute to obtain an oil phase, and the mass ratio of the probiotics to the cocoa butter substitute was 10:90.

[0041] The oil phase and the hydrogel phase with a mass ratio of 10:90 are subjected to high-speed shearing at 80°C and a rotation speed of 8000rpm, and are drip-cooled using a circulating cooling pellet equipment (the gelatin solution is kept at a temperature of 85-90°C, the gelatin solution output rate is 45mL / min, the circulating pump speed is 10rpm, the flow rate is 3000mL / min, the cooling temperature is 15-20°C, and the circulating coolant is medium-chain triglycerides). The gel beads in the circulating coolant are collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking. After the cross-linking is completed, the gel beads are filtered out and rinsed, and the product is collected after rinsing.

[0042] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the beverage liquid was almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0043] Example 2 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of acid-treated starch and hydroxypropyl distarch phosphate in a mass ratio of 8:2) and a low temperature responsive gel (a mixture of gellan gum and agar in a mass ratio of 3:2) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 10:5:85; DHA algae oil was dispersed and mixed with corn oil to obtain an oil phase, and the mass ratio of DHA algae oil to corn oil was 95:5.

[0044] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 10rpm, the flow rate was 3000mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0045] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) were mixed in a mass ratio of 95:5 (simulating the form of gel bead storage solution) and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the gel bead structure remained intact, the oxidation of algal oil was low, and no leakage was detected.

[0046] Example 3 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: High-temperature responsive gel acid-treated starch and low-temperature responsive gel gellan gum are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high-temperature responsive gel, the low-temperature responsive gel and water is 10:5:87; probiotics are dispersed in cocoa butter substitute to obtain an oil phase, and the mass ratio of the probiotics to the cocoa butter substitute is 10:90.

[0047] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 95-99°C, the gelatin solution output rate was 50mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 20-25°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0048] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) were mixed in a mass ratio of 95:5 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the beverage liquid was almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0049] Example 4 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of acid-treated starch and konjac gum in a mass ratio of 18:2) and a low temperature responsive gel gellan gum are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and the temperature is naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 15:5:80; probiotics are dispersed in hydrogenated vegetable oil to obtain an oil phase, and the mass ratio of the probiotics to the hydrogenated vegetable oil is 10:90.

[0050] The oil phase and the hydrogel phase with a mass ratio of 20:80 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 6rpm, the flow rate was 1800mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 5%wt calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0051] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 95:5 and then heat treated at 95°C for 30 min. There was no obvious change in the beverages, and the gel beads showed adhesion. However, the beverage liquids were almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0052] Example 5 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: The high temperature responsive gel hydroxypropyl distarch phosphate and the low temperature responsive gel gellan gum are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 5:15:80; the probiotics are dispersed in hydrogenated vegetable oil to obtain an oil phase, and the mass ratio of the probiotics to the hydrogenated vegetable oil is 10:90.

[0053] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 90-95°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 20-25°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0054] The morphological characteristics of the gel beads, such as roundness, were poor. The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 95:5 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the beverage liquids were almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0055] Example 6 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: High temperature responsive gel hydroxypropyl distarch phosphate and low temperature responsive gel (a mixture of sodium alginate and gellan gum in a mass ratio of 8:12) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 5:15:80; DHA algae oil was dispersed in medium chain triglycerides to obtain an oil phase, and the mass ratio of DHA algae oil and medium chain triglycerides was 95:5.

[0056] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 50mL / min, the circulating pump speed was 12rpm, the flow rate was 3600mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0057] The morphological characteristics of the gel beads, such as roundness, were poor. The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 95:5 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the oxidation of DHA algae oil was low, and no leakage was detected.

[0058] Example 7 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of acid-treated starch and hydroxypropyl distarch phosphate in a mass ratio of 10:5) and a low temperature responsive gel (a mixture of gellan gum and agar in a mass ratio of 3:2) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 15:5:80; lutein ester was dispersed in sunflower seed oil to obtain an oil phase, and the mass ratio of lutein ester to sunflower seed oil was 15:85.

[0059] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 10rpm, the flow rate was 3000mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0060] The morphological characteristics of the gel beads, such as roundness, were poor. The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 95:5 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, no leakage of lutein esters was detected, and the active ingredients of lutein esters were almost not degraded.

[0061] Example 8 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of pregelatinized starch and hydroxypropyl starch in a mass ratio of 3:2) and a low temperature responsive gel (a mixture of gellan gum and gelatin in a mass ratio of 1:4) were dispersed in water, heated in a water bath at 85°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 5:5:90; oil-soluble curcumin was dispersed in soybean oil to obtain an oil phase, and the mass ratio of curcumin to soybean oil was 10:90.

[0062] The oil phase and the hydrogel phase with a mass ratio of 40:60 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 15-20°C, and the circulating coolant was soybean oil). The gel beads in the circulating coolant were collected and put into a 2.5%wt calcium chloride aqueous solution for cross-linking. After the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0063] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the gel beads became sticky, and no leakage of curcumin was detected.

[0064] Example 9 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of hydroxypropyl starch and curdlan in a mass ratio of 9:1) and a low temperature responsive gel (a mixture of gellan gum and pectin in a mass ratio of 6:1) were dispersed in water, heated in a water bath at 85°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 15:10:75; lycopene was dispersed in hydrogenated vegetable oil to obtain an oil phase, and the mass ratio of lycopene dispersed in the hydrogenated vegetable oil was 15:85.

[0065] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 8rpm, the flow rate was 2400mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0066] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 125°C for 30 minutes. The structure of the gel beads remained intact, the beverages showed no obvious changes, and lycopene was not detected in the beverages. Example 10 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of acid-treated starch and oxidized hydroxypropyl starch in a mass ratio of 1:1) and a low temperature responsive gel (a mixture of gellan gum, xanthan gum, and guar gum in a mass ratio of 5:2:2) were dispersed in water, heated in a water bath at 95°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 5:5:90; tocopherol was mixed with cocoa butter to obtain an oil phase, and the mass ratio of tocopherol to cocoa butter was 45:55.

[0067] The oil phase and the hydrogel phase with a mass ratio of 10:90 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 6rpm, the flow rate was 1800mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 3%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0068] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. The structure of the gel beads remained intact, the beverages showed no obvious changes, and tocopherol was not detected in the beverages. Embodiment 11 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of oxidized hydroxypropyl starch and acetate starch in a mass ratio of 4:1) and a low temperature responsive gel (a mixture of gellan gum, trehalose, and gum arabic in a mass ratio of 3:5:1) were dispersed in water, heated in a water bath at 95°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel, and water was 10:5:85; EPA was mixed with palm oil and walnut oil to obtain an oil phase, and the mass ratio of EPA, palm oil, and walnut oil was 20:20:55.

[0069] The oil phase and the hydrogel phase with a mass ratio of 20:80 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 12rpm, the flow rate was 3600mL / min, the cooling temperature was 20-25°C, and the circulating coolant was corn oil). The gel beads in the circulating coolant were collected and put into a 2% calcium lactate aqueous solution for cross-linking. After the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0070] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. The structure of the gel beads remained intact, the beverages had no obvious bad flavor, and the oxidation and acid value in the beverages were low. Example 12 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of hydroxypropyl distarch phosphate, octenyl succinate starch, and soy protein isolate in a mass ratio of 5:1:1) and a low temperature responsive gel (a mixture of gellan gum and carrageenan in a mass ratio of 1:1) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel, and water was 5:10:85; probiotics were dispersed in coconut oil to obtain an oil phase, and the mass ratio of the probiotics to coconut oil was 10:90.

[0071] The oil phase and the hydrogel phase with a mass ratio of 35:65 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooling was performed using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 10rpm, the flow rate was 3000mL / min, the cooling temperature was 15-20°C, and the circulating coolant was sunflower oil), the gel beads in the circulating coolant were collected and put into a 4.5% calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0072] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the beverage liquids were almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0073] Embodiment 13 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of pregelatinized starch and sodium caseinate in a mass ratio of 3:1) and a low temperature responsive gel (a mixture of gellan gum and locust bean gum in a mass ratio of 1:4) were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 15:15:70; probiotics were mixed with beeswax and stearic acid to obtain an oil phase, and the mass ratio of probiotics, beeswax and stearic acid was 20:50:10.

[0074] The oil phase and the hydrogel phase with a mass ratio of 25:75 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 90-95°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2.5% calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0075] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, the beverage liquids were almost sterile, and there was no obvious change in the bacterial activity inside the gel beads.

[0076] Embodiment 14 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: Disperse the high-temperature responsive gel oxidized hydroxypropyl starch and the low-temperature responsive gel gellan gum in water, heat and stir in a water bath at 95°C until the gel is completely dissolved, and cool naturally to obtain a hydrogel phase, and the mass ratio of the high-temperature responsive gel, the low-temperature responsive gel and water is 5:15:80; mix vitamin A, vitamin D, vitamin K, carotenoids and olive oil to obtain an oil phase, and the mass ratio of vitamin A, vitamin D, vitamin K, carotenoids and olive oil is 1:1:1:2:10.

[0077] The oil phase and the hydrogel phase with a mass ratio of 35:65 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 90-95°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 3.5% calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0078] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. There was no obvious change in the beverages, the structure of the gel beads remained intact, and the leakage of vitamin A, vitamin D, vitamin K, and carotenoids was not detected.

[0079] Embodiment 15 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of hydroxypropyl distarch phosphate and oxidized hydroxypropyl starch in a mass ratio of 3:2) and a low temperature responsive gel gellan gum are dispersed in water, heated in a water bath at 95°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 15:10:75; sterols, quercetin, peppermint oil and linseed oil are mixed to obtain an oil phase, and the mass ratio of sterols, quercetin, peppermint oil and linseed oil is 2:2:5:15.

[0080] The oil phase and the hydrogel phase with a mass ratio of 20:80 were subjected to high-speed shearing at 85°C and a rotation speed of 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 20-25°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 4.0% calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0081] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 min. There was no obvious change in the beverages, the structure of the gel beads remained intact, and no leakage of sterols, quercetin, and peppermint oil was detected.

[0082] Example 16 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: High temperature responsive gel (a mixture of acid-treated starch and hydroxypropyl starch in a mass ratio of 2:1) and low temperature responsive gel gellan gum are dispersed in water, heated in a water bath at 85°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 10:15:75; linoleic acid, α-linolenic acid, lauric acid and tea oil are mixed to obtain an oil phase, and the mass ratio of linoleic acid, α-linolenic acid, lauric acid and tea oil is 3:3:3:20.

[0083] The oil phase and the hydrogel phase with a mass ratio of 25:75 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2.5% calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0084] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 min. There was no obvious change in the beverages, the structure of the gel beads remained intact, and no leakage of linoleic acid, α-linolenic acid, and lauric acid was detected.

[0085] Embodiment 17 This embodiment provides a high temperature and high moisture resistant gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of acid-treated starch and hydroxypropyl distarch phosphate in a mass ratio of 2:1) and a low temperature responsive gel (a mixture of gellan gum and agar in a mass ratio of 5:1) were dispersed in water, heated in a water bath at 85°C with stirring until the gel was completely dissolved, and the temperature was naturally cooled to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 10:15:75; probiotics were mixed with fish oil and algae oil to obtain an oil phase, and the mass ratio of probiotics, fish oil and algae oil was 10:55:35.

[0086] The oil phase and the hydrogel phase with a mass ratio of 40:60 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 6rpm, the flow rate was 1800mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 3%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0087] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. The structure of the gel beads remained intact, the beverage liquids were almost sterile, and there was no obvious change in the bacterial activity inside the gel beads. Comparative Example 1 This comparative example provides a gel bead, and the preparation method thereof is as follows: A high temperature responsive gel (a mixture of hydroxypropyl distarch phosphate and acid-treated starch in a mass ratio of 15:5) and a low temperature responsive gel sodium alginate are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 20:2:78; DHA algae oil is mixed with medium chain triglycerides to obtain an oil phase, and the mass ratio of DHA algae oil and medium chain triglycerides is 95:5.

[0088] The oil phase and the hydrogel phase with a mass ratio of 10:90 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 10rpm, the flow rate was 3000mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0089] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) were mixed in a mass ratio of 10:90 and then heat-treated at 95°C for 30 min. The beverages became noticeably turbid, the gel beads melted, adhered, and aggregated, and had an obvious unpleasant flavor when taken.

[0090] Comparative Example 2 This comparative example provides a gel bead, and the preparation method thereof is as follows: First, disperse the high-temperature responsive gel acid-treated starch and the low-temperature responsive gel (a mixture of gelatin and gellan gum in a mass ratio of 17:3) in water, heat and stir in a water bath at 90°C until the gel is completely dissolved, and cool naturally to obtain a hydrogel phase. The mass ratio of the high-temperature responsive gel, the low-temperature responsive gel and water is 1:20:79. Mix DHA algae oil with medium-chain triglycerides to obtain an oil phase. The mass ratio of DHA algae oil and medium-chain triglycerides is 95:5.

[0091] The oil phase and the hydrogel phase with a mass ratio of 20:80 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 90-95°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 12rpm, the flow rate was 3600mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2%wt calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out and rinsed, and the product was collected after rinsing.

[0092] The gel beads were mixed with different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) in a mass ratio of 10:90 and then heat-treated at 95°C for 30 min. The gel beads melted, adhered, and aggregated, and the beverage became noticeably turbid and had a distinct unpleasant flavor when taken.

[0093] Comparative Example 3 This comparative example provides a gel bead, and the preparation method thereof is as follows: High temperature responsive gel acid-treated starch and low temperature responsive gel sodium alginate are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 5:5:90; DHA algae oil is mixed with corn oil to obtain an oil phase, and the mass ratio of DHA algae oil to corn oil is 95:5.

[0094] The oil phase and the hydrogel phase with a mass ratio of 10:90 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 50mL / min, the circulating pump speed was 8rpm, the flow rate was 2400mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 1.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0095] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) were mixed in a mass ratio of 10:90 and then heat-treated at 95°C for 30 min. The beverages became noticeably turbid, the gel beads melted, adhered, and aggregated, and had an obvious unpleasant flavor when taken.

[0096] Comparative Example 4 This comparative example provides a gel bead, and the preparation method thereof is as follows: The high temperature responsive gel hydroxypropyl distarch phosphate and the low temperature responsive gel gellan gum were dispersed in water, heated in a water bath at 90°C with stirring until the gel was completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water was 5:5:90; the probiotics were dispersed in medium chain triglycerides to obtain an oil phase, and the mass ratio of the probiotics to the medium chain triglycerides was 10:90.

[0097] The oil phase and the hydrogel phase with a mass ratio of 10:90 were subjected to high-speed shearing at 80°C and 8000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 15rpm, the flow rate was 4500mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 0.5%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0098] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, and plant-based drinks) were mixed in a mass ratio of 10:90 and then heat treated at 95°C for 10 min. The beverages became noticeably turbid, the gel beads melted, adhered, and aggregated, and bacteria were present in the beverage liquid.

[0099] Comparative Example 5 This comparative example provides a gel bead, and the preparation method thereof is as follows: High temperature responsive gel (a mixture of konjac gum and curdlan in a mass ratio of 15:5) and low temperature responsive gel sodium alginate are dispersed in water, heated in a water bath at 90°C with stirring until the gel is completely dissolved, and cooled naturally to obtain a hydrogel phase, and the mass ratio of the high temperature responsive gel, the low temperature responsive gel and water is 15:5:80; DHA algae oil and medium chain triglycerides are mixed to obtain an oil phase, and the mass ratio of DHA algae oil and medium chain triglycerides is 95:5.

[0100] The oil phase and the hydrogel phase with a mass ratio of 10:90 were subjected to high-speed shearing at 80°C and a rotation speed of 1000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 80-85°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 6rpm, the flow rate was 1800mL / min, the cooling temperature was 10-15°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 5%wt calcium lactate aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0101] The gel beads and different beverages (juice and juice drinks, tea drinks, coffee drinks, energy drinks, dairy drinks, bitter drinks, plant-based drinks) were mixed in a mass ratio of 10:90 and then heat treated at 95°C for 30 minutes. The beverages became noticeably turbid and had a noticeable bad flavor. The gel beads melted, adhered, and aggregated, and the DHA algae oil leaked.

[0102] Comparative Example 6 This comparative example provides a gel bead, and the preparation method thereof is as follows: Disperse the low-temperature responsive gel (a mixture of gellan gum and agar in a mass ratio of 3:2) in water, heat and stir in a water bath at 90°C until the gel is completely dissolved, and cool naturally to obtain a hydrogel phase with a ratio of 15:85; disperse DHA algae oil and mix it with corn oil to obtain an oil phase with a mass ratio of DHA algae oil to corn oil of 95:5.

[0103] The oil phase and the hydrogel phase with a mass ratio of 30:70 were subjected to high-speed shearing at 80°C and a rotation speed of 10000rpm, and drip-cooled using a circulating cooling pellet equipment (the gelatin solution was kept at a temperature of 85-90°C, the gelatin solution output rate was 45mL / min, the circulating pump speed was 10rpm, the flow rate was 3000mL / min, the cooling temperature was 15-20°C, and the circulating coolant was medium-chain triglycerides), the gel beads in the circulating coolant were collected and put into a 2%wt calcium chloride aqueous solution for cross-linking, and after the cross-linking was completed, the gel beads were filtered out for rinsing, and the product was collected after rinsing.

[0104] Test Example 1 High-resolution images of the surface morphology of the gel beads obtained in Example 2 and the gel beads obtained in Comparative Example 6 were obtained by scanning electron microscopy (SEM). Figure 2 and Figure 3 As shown, Figure 2 Figure b shows the surface microstructure of the gel beads in Example 2, and Figure a shows the surface microstructure of the gel beads obtained in Comparative Example 6. The gel structure shown in Comparative Example 6 is relatively loose and cannot protect the active ingredients. The gel structure shown in Example 2 is relatively dense and can effectively protect the active ingredients and effectively prevent the dissolution of the active ingredients and the invasion of factors that affect the active ingredients. Figure 3 This is the distribution of the active ingredient in Example 2.

[0105] Test Example 2 After the gel beads in Example 2, Example 6, Comparative Example 1, Comparative Example 3, and Comparative Example 5 were heat treated in AD calcium milk, the temperature was naturally reduced to 25°C, and the gel beads required for the experiment were fished out from each AD calcium milk for appearance and fishy smell (from DHA algae oil), and an appropriate amount of AD calcium milk was taken for sensory evaluation, and then a portion of the samples (i.e., a mixture of gel beads and AD calcium milk) were stored at 25°C for 60 days of room temperature stability, and another portion of the samples were stored at 40°C for 30 days of accelerated stability. The stability of the gel beads in AD calcium milk was judged by the fishy smell at the end of the stability study. The results are shown in Table 1. The gel beads of the three comparative examples all showed poor stability after heat treatment, and the contents leaked. The gel beads of Example 2 and Example 6 showed good stability after heat treatment, and the contents were basically not leaked. After 60 days of room temperature storage and 30 days of storage at 40°C, the gel beads still maintained good stability in AD calcium milk.

[0106] Table 1 Stability and fishy smell of gel beads and sensory evaluation of beverages

[0107] Test Example 3 The gel beads in Example 1, Example 3, Example 4, Example 5 and Comparative Example 4 were naturally cooled to 25°C after completing the heat treatment in AD calcium milk and stored at 25°C. On the 0th day, the 7th day, the 14th day and the 21st day, the gel beads required for the experiment were fished out from the AD calcium milk for bacterial activity detection, and the remaining gel beads continued to remain in the AD calcium milk. The bacterial activity detection method is: shake and mix the sample with physiological saline containing 5% Tween 80 and 1% sodium citrate, dilute it in a gradient, and inoculate it on MRS agar medium. The total colony count was calculated after anaerobic culture at 37°C for 48 hours (YQX-T anaerobic incubator, Shel Lab Inc., Cornelius, OR, USA). All diluents and consumables used in the culture were sterilized at 121°C for 20 minutes in advance. The results are as shown in the figure. Figure 4 As shown, compared with the examples, the bacterial activity of Comparative Example 4 decreased significantly faster, indicating that the probiotics in the gel beads leaked and the gel beads failed to provide good protection for the contents.

[0108] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A double gel composition, characterized in that: The invention is composed of a low-temperature responsive gel and a high-temperature responsive gel, wherein the mass ratio of the low-temperature responsive gel to the high-temperature responsive gel is (5-15):(5-15); the raw material of the low-temperature responsive gel comprises gellan gum, and the gellan gum accounts for no less than 20%wt of the low-temperature responsive gel; the raw material of the high-temperature responsive gel comprises at least one of pregelatinized starch, acid-treated starch, hydroxypropyl starch, hydroxypropyl distarch phosphate and oxidized hydroxypropyl starch.

2. The double gel composition according to claim 1, characterized in that The raw materials of the low temperature responsive gel further include at least one of sodium alginate, agar, gelatin, pectin, trehalose, carrageenan, locust bean gum, xanthan gum, gum arabic and guar gum; and / or The raw materials of the high temperature responsive gel also include at least one of konjac gum, curdlan gum, acetate starch, octenyl succinate starch, sodium caseinate and soy protein isolate.

3. A method for preparing high temperature and high moisture resistant gel beads, characterized in that: The following operations are included: The double gel composition according to claim 1 or 2 is gelled with water as a hydrogel phase, the hydrogel phase and the oil phase containing the active ingredient are mixed by high-speed shear dispersion technology, and then dripped into a coolant through a cooling pill device to form gel beads, the gel beads in the coolant are collected and put into a cross-linking liquid for cross-linking, and after the cross-linking is completed, the gel beads are filtered out and rinsed to obtain the gel beads.

4. The preparation method according to claim 3, characterized in that: The mass percentage concentration of the low temperature responsive gel and the high temperature responsive gel in water is 5% to 15%; and / or The mass ratio of the hydrogel phase to the oil phase is (60-90):(10-40).

5. The preparation method according to claim 3 or 4, characterized in that: The oil phase is composed of active ingredients and lipid components, and the mass ratio of the active ingredients to the lipid components is (10-95): (5-90).

6. The preparation method according to claim 5, characterized in that: The lipid component comprises at least one of corn oil, medium chain triglycerides, soybean oil, sunflower oil, hydrogenated vegetable oil, cocoa butter, cocoa butter substitute, palm oil, beeswax, stearic acid, coconut oil, walnut oil, olive oil, fish oil, algae oil, linseed oil and tea oil; and / or The active ingredient includes a lipophilic active ingredient or a probiotic; preferably, the lipophilic active ingredient includes at least one of curcumin, lycopene, tocopherol, vitamin A, vitamin D, vitamin K, sterols, carotenoids, quercetin, peppermint oil, linoleic acid, α-linolenic acid, lauric acid, DHA algae oil, EPA and lutein esters.

7. The preparation method according to claim 3, characterized in that: The high-speed shearing is performed at a speed of 8000-1000 rpm at a temperature not lower than 80° C.; and / or The cooling liquid is selected from medium chain triglycerides, corn oil, sunflower oil or soybean oil; and / or The cross-linking liquid is a 0.5% to 5%wt calcium chloride aqueous solution or a calcium lactate aqueous solution.

8. The preparation method according to claim 7, characterized in that: The circulating coolant is medium chain triglyceride.

9. A high temperature and high moisture resistant gel bead, characterized in that: The gel beads are prepared according to the preparation method according to any one of claims 1 to 8.

10. Use of the high temperature and high moisture resistant gel beads according to claim 9 in the preparation of products containing lipophilic active ingredients or probiotics.

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