Probiotic ball as well as preparation method and application thereof

Abstract

The invention relates to the technical field of food, and provides a probiotic ball and a preparation method and application thereof.The probiotic ball is obtained by forming dropping pills from an inner core raw material, a grease layer raw material and a rubber layer raw material through a one-step dropping pill process, cooling the dropping pills and then mixing the dropping pills with a calcium salt-containing solution; in the one-step pill dropping method preparation, the grease layer raw material is in contact with the inner core raw material and the rubber layer raw material, and the curing agent in the grease layer raw material is migrated to the inner core raw material and the interface between the inner core raw material and the grease layer and is crosslinked and cured with sodium alginate in the first water-soluble protective agent, so that the grease layer raw material is obtained. The curing agent in the raw materials of the grease layer migrates to the raw materials of the rubber layer and the interface between the raw materials of the rubber layer and the grease layer, and is cross-linked and cured with sodium alginate in the second water-soluble protective agent. According to the preparation method disclosed by the invention, the specific embedding layer is optimally designed, so that the obtained high-quality probiotic balls have excellent tolerance and good sensory flavor when being used in the preparation process of yoghourt.

Description

Technical Field

[0001] This invention relates to the field of food technology, and in particular to a probiotic ball, its preparation method, and its application. Background Technology

[0002] Probiotics, as live microorganisms with a clear regulatory function on human gut health, have been widely used in food systems such as yogurt and beverages. However, probiotics are extremely sensitive to environmental factors (such as temperature, oxygen, stomach acid, and bile salts) and are easily inactivated during processing, storage, and passage through the human digestive tract. To address this issue, using droplet encapsulation technology to isolate probiotics from adverse external environments is an effective solution. Especially with the popularity of visually appealing beverages such as yogurt, milk, and coffee, probiotic pellets (droplets) with their attractive appearance and chewy texture are highly favored by the market.

[0003] In existing probiotic droplet preparation technologies, in pursuit of high encapsulation rates and high tolerance (acid resistance, heat resistance, shear resistance), conventional practices often rely on adding a hydrophobic oil protective layer or thickening the wall material. However, this approach leads to significant sensory defects, namely, the product is accompanied by a "bland flavor" or an unacceptable "greasy / waxy feel" when consumed, affecting the consumer experience.

[0004] To improve taste, the industry has attempted to introduce water-soluble ingredients as raw materials for the encapsulation layer. However, if the encapsulation layer is entirely composed of water-soluble ingredients, the probiotics within it can easily migrate outwards through the aqueous phase channels. This not only reduces the encapsulation rate but also leads to free exchange of moisture between the inner and outer layers, making the product highly susceptible to moisture absorption and resulting in a loose wall structure that is difficult to maintain stability in high-moisture matrices such as yogurt. Therefore, multi-layered encapsulation layer structures with alternating oil and hydrophilic layers have been proposed. However, while the one-step drop pelleting method integrates key steps such as material mixing, molding, and cooling solidification into a single device and offers high production efficiency, current one-step drop pelleting processes for preparing probiotic pellets use oil as the inner core carrier or have a high proportion of oil in the layer, resulting in limited effectiveness in improving the aforementioned sensory defects.

[0005] Therefore, this invention is proposed. Summary of the Invention

[0006] Research has found that in the process of preparing probiotic capsules using the one-step drop pelleting method, in order to improve the product's tolerance to complex process conditions such as high-temperature sterilization and high-shear stirring, and to prevent its inactivation during product storage or application, it is necessary to strictly control the quality defects of the probiotic-containing capsules, such as excessive weight variation, uneven hardness, poor sphericity, or core eccentricity. Using water-soluble components as the core carrier and oil components as the outer protective layer, the interaction at the water-oil interface plays a crucial role in the successful application of the one-step drop pelleting method and ensuring the quality of the resulting probiotic capsules.

[0007] Based on this, the present invention provides a probiotic ball prepared by a one-step drop pelleting method, its preparation method, and its application. By adding a specific curing agent to the oil layer and sodium alginate to the water-soluble inner core carrier and the rubber layer, the curing agent in the oil layer continuously migrates during the one-step drop pelleting process and after the pellets are formed, and then cross-links and solidifies with the sodium alginate in the water-soluble inner core carrier and the rubber layer. This achieves the preparation of high-quality probiotic balls using the one-step drop pelleting method. These probiotic balls, when used in the preparation of yogurt, exhibit excellent tolerance and good sensory flavor.

[0008] Specifically, in the first aspect, the present invention provides a probiotic ball, which is obtained by forming droplets using an inner core material, an oil layer material, and a rubber layer material through a one-step droplet forming process, cooling the droplets, and then mixing them with a solution containing calcium salts; The core material is used to form the core of the probiotic ball; The grease layer material is used to form a grease layer located on the surface of the inner core; The rubber layer material is used to form a rubber layer located on the surface of the grease layer; The inner core material includes probiotics and uses a first water-soluble protective agent containing sodium alginate as a carrier for the probiotics; the outer layer material includes a second water-soluble protective agent containing sodium alginate. In the one-step droplet preparation method, the grease layer material comes into contact with the inner core material and the rubber layer material. The curing agent in the grease layer material migrates to the inner core material and its interface with the grease layer, and cross-links and cures with sodium alginate in the first water-soluble protective agent. The curing agent in the grease layer material also migrates to the rubber layer material and its interface with the grease layer, and cross-links and cures with sodium alginate in the second water-soluble protective agent. The curing agent is selected from one or more of calcium chloride, calcium lactate, calcium citrate, calcium gluconate, calcium stearyl lactate, and calcium triethyl citrate.

[0009] This invention addresses the functional requirements of the inner core and outer layer of probiotic pellets by employing a differentiated cross-linking design based on the interaction mechanism between sodium alginate and calcium. The curing agent in the oil layer and the calcium-containing solution exhibit completely different release methods and cross-linking processes due to their different phase states (oil-dispersed / water-soluble). During the dripping process, the curing agent in the oil layer gradually diffuses into the inner core material through the oil-water interface, progressively cross-linking with the sodium alginate in the inner core to form a loose gel network, suitable for the gentle encapsulation requirements of probiotics. The calcium in the calcium-containing solution immediately comes into direct contact with the outer layer material after dripping, enabling immediate cross-linking of the sodium alginate in the outer layer material to form a dense gel network, constructing an acid-resistant barrier. In other words, this difference in calcium source composition is a functional design feature of this invention, achieving a functional division between "live bacteria protection" and the "environmental barrier" function of the outer layer by controlling the cross-linking intensity gradient through phase regulation.

[0010] Meanwhile, this invention achieves precise layering of the microsphere structure through differentiated control of crosslinking timing: the crosslinking of the inner core is carried out simultaneously with the microsphere drop forming (during the drop addition process), ensuring the synergistic controllability of the inner core gel network and the microsphere morphology and particle size, and avoiding damage to live bacteria due to crosslinking stress; the crosslinking of the rubber layer is carried out after the drop forming is completed (post-curing reinforcement), and the reaction only occurs on the surface of the microsphere, without interfering with the already formed inner core structure, while achieving rapid densification of the rubber layer.

[0011] Regarding the crosslinking of the rubber layer, after dripping, the rubber layer and the calcium salt mixture undergo immediate crosslinking to form a dense outer layer. In the subsequent process, the curing agent in the grease layer slowly migrates to the side of the rubber layer closer to the inner core, implementing supplementary mild crosslinking, so that the rubber layer forms a composite structure with different degrees of crosslinking. This not only solves the brittle cracking defect of the rubber layer caused by conventional single aqueous calcium crosslinking, but also ensures the acid resistance barrier function, achieving a balance between structural density and toughness.

[0012] In the three-layer structure designed in this invention, the middle oil layer is a dense hydrophobic layer, forming a "water-oil" thermodynamic barrier that prevents probiotics from migrating across phases, thus maintaining a relatively stable encapsulation rate. The outer rubber layer primarily blocks the penetration of acidic substances, and the middle oil layer also prevents the inner core from direct contact with external acidic solutions, extending the acid resistance time of the inner core's aqueous phase in maintaining a neutral environment. Furthermore, the middle oil layer also provides oxygen barrier and moisture protection.

[0013] Preferably, the calcium salt is selected from one or a combination of two or more of calcium chloride, calcium lactate, calcium citrate, calcium gluconate, calcium stearoyl lactate, and calcium triethyl citrate.

[0014] According to the probiotic balls provided by the present invention, the mass ratio of the inner core material to the oil layer material is 1:(0.5~1.5); for example, it can be any value or a range of values ​​formed by any values ​​from 1:0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1.0, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5.

[0015] And / or, the mass ratio of the grease layer material to the rubber layer material is 1:(1~3), for example, it can be any value or a range of values ​​formed by any values ​​among 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, and 1:3.

[0016] The mass ratios of the above-mentioned raw materials were determined by considering the stoichiometry, reaction kinetics, spatial distribution, structural stability of the embedded spheres, probiotic protection, and process feasibility of the calcium cross-linking reaction. Within the above range, the cross-linking reaction that promotes probiotic encapsulation mainly occurs at the oil-water interface (the core material and the rubber layer material are aqueous phases, while the oil layer material is an oil phase). The mass ratio of the oil layer directly affects the calcium content. 2+ The release rate, diffusion path, and interfacial reaction environment are crucial factors. The core components of the inner core and outer shell materials are ionic hydrophilic colloids (such as sodium alginate, agar, and gellan gum). These colloids have reaction sites on their molecular chains that can crosslink with calcium, forming a three-dimensional gel network through ionic bridging. This is the core of capsule encapsulation. Furthermore, the calcium-crosslinked gel layer acts as an acid-resistant barrier, while the lipid layer provides a bile salt-resistant hydrophobic barrier. The mass ratio of these two layers needs to be adjusted based on the degree of calcium crosslinking to achieve complementary barrier functions.

[0017] Preferably, the curing agent is a combination of a first curing agent and a second curing agent, wherein the first curing agent is selected from one or more of calcium chloride, calcium lactate, calcium citrate, and calcium gluconate; and the second curing agent is selected from calcium stearyl lactate and / or calcium triethyl citrate. More preferably, the mass ratio of the first curing agent to the second curing agent is 1:(10~40), for example, it can be any value or a numerical range composed of any values ​​from 1:10, 1:15, 1:20, 1:25, 1:30, 1:35, and 1:40.

[0018] Preferably, the probiotics are selected from at least one of Lactobacillus plantarum, Lactobacillus curvatureensis, Bifidobacterium, Lactobacillus bulgaricus, Streptococcus thermophilus, Lactobacillus rhamnosus, Lactobacillus acidophilus, Lactobacillus casei / paracasei, Leuconostoc mesenteroides, Lactobacillus fermentum, Lactobacillus gasseri, Lactobacillus johnsonii, Lactobacillus helveticus, Lactobacillus reuteri, Lactobacillus salivarius, Bacillus coagulans, Lactococcus lactis, Lactobacillus sakei, Pediococcus lactis, Pediococcus pentosus, Bacillus coagulans BC 30, Bacillus coagulans BC 99, and Bacillus coagulans BC 208.

[0019] According to the probiotic balls provided by the present invention, the raw material of the oil layer further includes oil, and the mass ratio of the curing agent to the oil is (0.1~5):100, for example, it can be any value or a numerical range composed of any values ​​from 0.1:100, 0.5:100, 1.0:100, 1.5:100, 2.0:100, 2.5:100, 3.0:100, 3.5:100, 4.0:100, 4.5:100, 5.0:100.

[0020] If the amount of curing agent is too low, the molecular chain cross-linking will be insufficient, resulting in poor gel strength and easy swelling; if the amount of curing agent is too high, the gel will become brittle and shrink due to excessive cross-linking, and may even develop white bloom.

[0021] Preferably, the oil is selected from one or more of peanut oil, soybean oil, sunflower oil, corn oil, rapeseed oil, glycerin, MCT, butter, cream, and rice bran oil.

[0022] More preferably, the grease comprises a mixture of semi-solid and solid greases. Here, semi-solid and solid refer to the state of the grease at room temperature (25°C). The mass ratio of the semi-solid to solid grease is 3:1, and can be any value or a range of values.

[0023] According to the probiotic balls provided by the present invention, the sodium alginate content in the first water-soluble preservative is 10-20% by mass, for example, it can be any value or a range of any values ​​from 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, and 20%. When the sodium alginate content is too low, it is not conducive to improving the live bacteria encapsulation rate, easily accelerates the inactivation of probiotics, and the interface between the inner core and the oil layer is not tightly bound, easily resulting in "layering" or "off-center core". When the sodium alginate content is too high, it is not conducive to flavor release and easily causes uneven particle size of the probiotic balls.

[0024] To ensure uniform droplet forming, the viscosity of the core material is preferably between 4000 and 4500 mPa·s.

[0025] According to the probiotic balls provided by the present invention, the mass content of probiotics in the inner core material is 1×10⁻⁶. 6 ~1×10 13 CFU / g, for example, can be 1×10 6 CFU / g, 1×10 7 CFU / g, 1×10 8 CFU / g, 1×10 9 CFU / g, 1×10 10 CFU / g, 1×10 11 CFU / g, 1×10 12 CFU / g, 1×10 13 Any value in CFU / g or a range of values ​​consisting of any values.

[0026] According to the probiotic balls provided by the present invention, the sodium alginate content in the second water-soluble protective agent is 8-15% by mass, for example, it can be any value or a range of any values ​​among 8%, 9%, 10%, 11%, 12%, 13%, 14%, and 15%; the calcium salt content in the calcium salt-containing solution is 0.5-5% by mass, for example, it can be any value or a range of any values ​​among 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, and 5.0%.

[0027] If the sodium alginate content in the second water-soluble protective agent is too low, a complete cross-linked network cannot be formed. The droplets will be difficult to solidify in the calcium chloride solution, or the formed "crystals" will be soft, easily collapsed, and shatter upon contact. Furthermore, the encapsulation stability is poor, leading to easy swelling and leakage, and an inability to effectively encapsulate core substances (such as probiotics and flavor components). If the content is too high, it will lead to excessive cross-linking, resulting in hard, brittle crystals with a dry texture, poor chewiness, and even a "vitrified" feel. It will also cause the viscosity of the rubber layer material to be too high, resulting in uneven droplets, easy adhesion, and the formation of air bubbles or cracks inside after solidification. Additionally, if the cross-linking reaction of calcium chloride is too vigorous, the rapid film formation on the surface leads to insufficient internal penetration of calcium ions, resulting in a "hard outside, soft inside" layering phenomenon.

[0028] According to the probiotic balls provided by the present invention, the first water-soluble protective agent further includes substance A; substance A is selected from one or more combinations of gellan gum, agar, gelatin, konjac gum, pectin, carrageenan, gum arabic, locust bean gum, xanthan gum, guar gum, peach gum, red algae gum, and glycerin.

[0029] According to the probiotic balls provided by the present invention, the second water-soluble protective agent further includes substance B; said substance B is selected from one or more combinations of gellan gum, agar, gelatin, konjac gum, pectin, carrageenan, gum arabic, locust bean gum, xanthan gum, guar gum, peach gum, red algae gum, and glycerin.

[0030] The interaction of these substances can enhance gel strength and structural stability, crosslinking uniformity, and thermal stability.

[0031] Preferably, by weight, the core material includes 1-6 parts of probiotics, 40-200 parts of a first water-soluble preservative, and 794-959 parts of purified water; Preferably, by weight, the first water-soluble protective agent comprises 5-16 parts sodium alginate, 12-20 parts gellan gum, 10-18 parts agar, 8-20 parts gelatin, 3-10 parts konjac gum, 0.5-10 parts pectin, 0.5-15 parts carrageenan, 0.5-10 parts gum arabic, 0.5-10 parts locust bean gum, 0.5-10 parts xanthan gum, 0.1-10 parts guar gum, 0.1-10 parts peach gum, 0.1-10 parts red algae gum, and 9-15 parts glycerin.

[0032] Preferably, the raw materials of the rubber layer, by weight, include: 1-6 parts of probiotics, 45-120 parts of a second water-soluble protective agent, and 850-950 parts of purified water; Preferably, by weight, the second water-soluble protective agent comprises 12-20 parts gellan gum, 10-18 parts agar, 5-16 parts sodium alginate, 8-20 parts gelatin, 3-10 parts konjac gum, 0.1-1 parts pectin, 0.1-1 parts carrageenan, 0.1-1 parts gum arabic, 0.1-1 parts locust bean gum, 0.1-1 parts xanthan gum, 0.1-1 parts guar gum, 0.1-1 parts peach gum, 0.1-1 parts red algae gum, and 9-15 parts glycerin.

[0033] According to the probiotic balls provided by the present invention, the oil layer raw material further includes a sweetener, which is selected from one or more combinations of ammonium glycyrrhizate, monopotassium glycyrrhizate, tripotassium glycyrrhizate, stearyl glycyrrhizate, sucralose, and acesulfame potassium.

[0034] By adding oil-soluble sweeteners that meet the GB 2760-2024 standard, the "greasiness" and "blandness" of lipid matrices can be specifically improved. From the perspective of sensory threshold regulation, the sweetness of the sweetener can synergize with the "fatty" sensation of fat, reducing the duration of the oral cavity's perception of "greasy aftertaste". Sensory evaluation has verified that it can shorten the aftertaste retention time.

[0035] Preferably, the raw material for the oil layer comprises, by weight, 9950-1050 parts of oil, 0.3-30 parts of curing agent, and 0.01-5 parts of sweetener; Preferably, by weight parts, the oils include 100-200 parts peanut oil, 100-200 parts soybean oil, 100-200 parts sunflower oil, 100-200 parts corn oil, 100-200 parts rapeseed oil, 0.1-10 parts glycerin, 100-200 parts MCT, 100-200 parts butter, 10-50 parts light cream, and 10-50 parts rice bran oil.

[0036] In this invention, MCT refers to medium-chain triglycerides, of which caprylic triglycerides account for 50-80% and decanoic triglycerides account for 20-50%.

[0037] Preferably, the curing agent comprises, by weight, 0.3-5 parts calcium chloride, 0.3-5 parts calcium lactate, 0.3-5 parts calcium citrate, 0.3-5 parts calcium gluconate, 0.3-30 parts calcium stearyl lactate, and 0.3-30 parts calcium triethyl citrate.

[0038] Preferably, the sweetener comprises, by weight parts, 0.1 to 0.5 parts of glycyrrhizic acid stearate, 0.1 to 0.3 parts of stearate stevioside, 0.01 to 0.05 parts of mogroside palmitate, and 0.1 to 0.5 parts of erythritol stearate.

[0039] Secondly, the present invention also provides a method for preparing probiotic balls as described above, comprising: forming droplets using an inner core material, an oil layer material, and a rubber layer material in a one-step droplet process, cooling the droplets, and then mixing them with a solution containing calcium salts; The core material forms the core of the probiotic ball; The grease layer material forms a grease layer located on the surface of the inner core; The rubber layer material forms a rubber layer located on the surface of the grease layer; The inner core material includes probiotics and uses a first water-soluble protective agent containing sodium alginate as a carrier for the probiotics; the outer layer material includes a second water-soluble protective agent containing sodium alginate. In the one-step droplet preparation method, the grease layer material comes into contact with the inner core material and the rubber layer material. The curing agent in the grease layer material migrates to the inner core material and its interface with the grease layer, and cross-links and cures with sodium alginate in the first water-soluble protective agent. The curing agent in the grease layer material also migrates to the rubber layer material and its interface with the grease layer, and cross-links and cures with sodium alginate in the second water-soluble protective agent. The curing agent is selected from one or more of calcium chloride, calcium lactate, calcium citrate, calcium gluconate, calcium stearyl lactate, and calcium triethyl citrate.

[0040] Specifically, in a single dripping process, the oil layer material encapsulates the inner core material, while the outer aqueous phase solidifies instantly (e.g., through calcium cross-linking), forming a dense "oil phase barrier + gel network." This avoids the problems of inner phase leakage and core material loss found in conventional step-by-step processes, effectively ensuring the probiotic encapsulation rate, which is significantly superior to conventional processes. Furthermore, the single dripping directly forms a three-layer structure: "inner aqueous phase (probiotics + colloid) - oil phase - outer aqueous phase." The calcium cross-linked gel layer acts as an acid-resistant barrier, while the oil layer provides a bile salt-resistant hydrophobic barrier. The two layers complement each other's barrier functions through the degree of calcium cross-linking. In this three-layer structure, the oil phase uniformly coats the inner aqueous phase, resulting in more stable resistance to gastric acid and bile salts.

[0041] Preferably, the oil pump used to transport the grease layer raw material rotates at a speed of 200~240 r / min, for example, it can be any value or a range of values ​​composed of 200 r / min, 210 r / min, 220 r / min, 230 r / min, and 240 r / min.

[0042] Preferably, the speed of the adhesive pump used to transport the core material is 300~350 r / min, for example, it can be any value or a range of values ​​composed of 300 r / min, 310 r / min, 320 r / min, 330 r / min, 340 r / min, and 350 r / min.

[0043] Preferably, the speed of the adhesive pump used to transport the rubber layer raw material is 420~470 r / min, for example, it can be any value or a range of values ​​composed of 420 r / min, 430 r / min, 440 r / min, 450 r / min, 460 r / min, and 470 r / min.

[0044] Preferably, the dripping temperature used in the one-step pelleting method is 85~90℃, for example, it can be any value or a range of values ​​among 85℃, 86℃, 87℃, 88℃, 89℃, and 90℃.

[0045] Preferably, the heating cycle of the dropper used in the one-step droplet method is 55~65s, for example, it can be any value or a range of values ​​composed of 55s, 56s, 57s, 58s, 59s, 60s, 61s, 62s, 63s, 64s, and 65s.

[0046] Preferably, the heating time used in the one-step pelleting method is 45~55s, for example, it can be any value or a range of values ​​among 45s, 46s, 47s, 48s, 49s, 50s, 51s, 52s, 53s, 54s, and 55s.

[0047] Preferably, the temperature for cooling the droplets is 10~30℃, for example, it can be any value or a range of values ​​among 10℃, 15℃, 20℃, 25℃, and 30℃.

[0048] Preferably, the calcium salt-containing solution is obtained by mixing calcium salt with water.

[0049] Preferably, the temperature at which the cooled pellets are mixed with the calcium salt solution is 20-30°C, and the time is less than 30 minutes.

[0050] Thirdly, the present invention also provides a food product, the food product including yogurt or jam; the food product also includes probiotic balls as described above, and the probiotic balls prepared by the preparation method described above.

[0051] As an example, the probiotic balls can be added directly to the yogurt base, or they can be mixed with jam first and then added to the yogurt base.

[0052] The probiotic balls, their preparation method, and applications provided by this invention optimize the design of a specific encapsulation layer. In the one-step droplet preparation process, the curing agent in the oil layer raw material undergoes cross-linking and curing with the sodium alginate in the inner core raw material and the rubber layer raw material. This results in high-quality probiotic balls that exhibit excellent tolerance and good sensory flavor when used in the preparation of yogurt. Detailed Implementation

[0053] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0054] Where specific techniques or conditions are not specified in the embodiments, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels. The models or parameters of some of the raw materials involved in the embodiments of this invention are shown below: Probiotics: Bacillus coagulans BC 99, with a live count of 9 × 10⁻⁶. 8 CFU / serving

[0055] Intestinal sustained-release membrane solution: 0~5wt% concentration of intestinal sustained-release membrane solution.

[0056] The structure of the three-layer dripper in the one-step pelleting equipment is as follows: the outermost dripper has a diameter of 5.1 mm.

[0057] Example 1A Probiotic Balls This embodiment provides a method for preparing probiotic balls, the steps of which are as follows: (1) Ingredients (1.1) Preparation of core raw materials The composition of the core material by weight is as follows: 936 parts water, 20 parts gellan gum, 11 parts agar, 9 parts sodium alginate, 3 parts konjac gum, 15 parts glycerin, and 3 parts bacterial powder.

[0058] The preparation process of the core material is as follows: All raw materials except water and probiotics are added to water at 60°C and stirred continuously for 30 minutes. Probiotics are then added, and the mixture is dispersed using a disperser at 1500 rpm for 15 minutes to obtain the core material. The mixture is then kept at this temperature for later use. The viscosity of this core material is 4500 mPa·s.

[0059] (1.2) Preparation of oil layer raw materials The composition of the oil layer raw material by mass parts is as follows: Oils: 220 parts soybean oil, 220 parts sunflower oil, 220 parts MCT, 220 parts butter, 50 parts rice bran oil, 50 parts light cream, 20 parts glycerin.

[0060] Curing agent: 1 part calcium chloride, 10 parts calcium lactate stearyl ester, 6 parts calcium triethyl citrate.

[0061] Sweeteners: 0.3 parts glycyrrhizic acid stearate, 0.15 parts stearate stevioside, 0.05 parts mogroside palmitate, and 0.3 parts erythritol stearate.

[0062] The preparation process of the grease layer raw material is as follows: heat the grease to 65°C to melt and mix it to form an oil liquid, and add a curing agent and a sweetener to the oil liquid to obtain the grease layer raw material.

[0063] (1.3) Rubber layer raw materials The composition of the rubber layer raw material by weight is as follows: Weigh out 941 parts of RO water, 25 parts of gellan gum, 15 parts of agar, 7 parts of sodium alginate, and 12 parts of glycerin.

[0064] The preparation process of the rubber layer raw material is as follows: after the second water-soluble protective agent is dry-mixed, it is added to RO water and stirred to dissolve. The temperature is raised to 95℃ and maintained for 30 minutes to obtain the rubber layer raw material, which is then kept at this temperature for later use. The viscosity of this core raw material is 4000 mPa·s.

[0065] (1.4) Solutions containing calcium salts The preparation process of the calcium salt-containing solution is as follows: calcium salt (calcium chloride) is mixed with RO water to obtain the calcium salt-containing solution. The calcium salt content in the solution is 1% by mass.

[0066] (2) The core material, grease layer material and rubber layer material in step (1) are used to form a three-layer structure with a diameter of 7.0 mm by using a three-layer dropper of a one-step dropper. The dropper is dropped into cooling oil (MCT) at a temperature of 10~15℃.

[0067] The mass ratio of the inner core material, the grease layer material, and the rubber layer material is 2:2:4. The oil pump speed is 220 r / min, the glue pump speed is 430 r / min, the dripper temperature is 85~90℃, the dripper heating cycle is 60s, and the heating time is 50s.

[0068] (3) Mix the pellets from step (2) with the calcium salt solution from step (1) and contact them at 25°C for 30 minutes to allow the outer rubber protective layer to fully harden and obtain a semi-finished product.

[0069] (4) The semi-finished product obtained in step (3) is placed in a 2wt% intestinal slow-release membrane solution and left to stand for 30 minutes. Then, it is washed, filtered and packaged in sequence to obtain probiotic balls.

[0070] Example 2A This embodiment provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, the only difference being that the oil is a liquid oil, and its specific composition is as follows: 300 parts soybean oil, 300 parts sunflower oil, 280 parts MCT, 50 parts rice bran oil, 50 parts light cream, and 20 parts glycerin.

[0071] Example 3A This embodiment provides a method for preparing probiotic balls. The steps are basically the same as those in Example 1A. The only difference is that in step (2), the mass ratio of the inner core material, the oil layer material, and the rubber layer material is 2:3:4, the oil pump speed is 320 r / min, and the rubber pump speed is 430 r / min.

[0072] Example 4A This embodiment provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the curing agent is replaced by calcium chloride in equal mass.

[0073] Example 5A This embodiment provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the curing agent is replaced by 10.5 parts of calcium stearyl lactate and 6.5 parts of calcium triethyl citrate.

[0074] Examples 6A~8A This embodiment provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that: In Example 6A, the calcium chloride in the oil layer raw material was replaced with calcium lactate by mass.

[0075] In Example 7A, the calcium chloride in the oil layer raw material was replaced by calcium citrate.

[0076] In Example 8A, the calcium chloride in the oil layer raw material was replaced with calcium gluconate by mass.

[0077] Comparative Example 1A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that sodium alginate is not added to the core material.

[0078] Comparative Example 2A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the oil layer raw material does not contain a curing agent.

[0079] Comparative Example 3A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the oil is a semi-solid oil, and its specific composition is as follows: 320 parts butter, 320 parts coconut oil, 320 parts palm oil, 40 parts chocolate.

[0080] Comparative Example 4A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the oil layer raw material does not contain sweeteners.

[0081] Comparative Example 5A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A, except that the oil layer raw materials are replaced with corn syrup in equal quantities. The preparation process of the corn syrup is as follows: 500 parts corn syrup, 150 parts maltodextrin, 30 parts starch, 8 parts pectin, 5 parts gelatin, and 15 parts gum arabic are dissolved in 292 parts purified water to obtain a sugar solution with a viscosity of 100-300 mPa·s.

[0082] Comparative Example 6A This comparative example provides a method for preparing probiotic balls, the steps of which are basically the same as those in Example 1A. The only difference is that in step (2), the mass ratio of the inner core material, the oil layer material, and the rubber layer material is 2:1:4, the oil pump speed is 120r / min, and the rubber pump speed is 430r / min.

[0083] Example 1B Probiotic Cone Jam This embodiment provides a method for preparing probiotic confectionery, the steps of which are as follows: First, add the pretreated probiotic balls to the target jam base, which has been cooled to 15-20°C, at a ratio of 15-20% (w / w). Mix using a paddle mixer (40-50 rpm) for 5-8 minutes until evenly distributed. Then, use a plunger pump filling machine at a filling temperature of 15-20°C to fill bottles (200g / bottle) → seal → invert for sterilization (85-90°C, 15 minutes) → cool.

[0084] Example 1C Yogurt This embodiment provides a method for preparing yogurt, the steps of which are as follows: (1) Standardization of raw milk Raw milk undergoes purification, degassing, standardization, and sterilization separation.

[0085] This process requires a protein content of 3.0% and a microbial content of <50 CFU.

[0086] (2) Chemical processing Heat the raw milk to 40-45℃, then add protein powder, starch, stabilizer and other ingredients in sequence, while controlling the high shear speed at 2500r / min and stirring and dispersing for 10min.

[0087] (3) Sterilization All materials are sterilized at 121℃ for 4 seconds.

[0088] (4) Homogeneous The material is heated to 60°C and homogenized under a pressure of 200 bar.

[0089] (5) Fermentation Add the starter culture at 42℃ and continue fermenting for 5.5 hours. When the pH value is between 4.3 and 4.55 and the acidity is >70°T, the fermentation ends.

[0090] (6) Delaying milk production Maintain a speed of 25-40 rpm and continue stirring for 2-5 minutes to complete the demulsification and stirring process.

[0091] (7) Aseptic mixing and filling The yogurt base obtained in step (6) is aseptically mixed with the probiotic ball jam obtained in Example 1B and packaged to obtain yogurt containing probiotic balls.

[0092] Examples 2B~8B Probiotic Cone Jam This is essentially the same as Example 1B, except that the probiotic balls used are those prepared in Examples 2A to 8A. The correspondence is shown in the table below.

[0093] Table 1

[0094] Example 2C~8C Yogurt This is essentially the same as Example 1C, except that the probiotic ball jam uses probiotic balls prepared in Examples 2B to 8B. The correspondence is shown in the table below.

[0095] Table 2

[0096] Comparative examples 1C~6C This is essentially the same as Example 1C, except that the probiotic balls used are those prepared in Comparative Examples 1A to 6A. The corresponding relationships are shown in the table below.

[0097] Table 3

[0098] Test Example 1 (1) Encapsulation rate of probiotic balls Test method: Calculate the total amount of material in a single tank (N0) and the amount of waste discharged during the dripping process in a single tank (N1), and calculate the dripping rate. The formula is: Dripping rate (%) = (N0-N1) / N0×100%.

[0099] (2) Live bacteria count of probiotic balls Test method: Crush 50 samples and dissolve them in 50ml of oil. Test the number of viable bacteria in the capsules after the product's shelf life (30 days) according to GB 4789.35. The storage conditions during the shelf life are: storage temperature 2~6℃ (optimal 4℃), dry and well-ventilated (relative humidity ≤75%), and protected from light.

[0100] (3) The hardness of probiotic balls Test method: The hardness of the probiotic balls was tested using an SMS texture analyzer. The descent speed before the test was 2 mm / sec, the test speed was 1 mm / sec, the rise speed after the test was 10.00 mm / sec, the trigger force was 5 g, and the deformation was 85%. Ten balls were tested for each sample, and the average value was taken.

[0101] (4) Breakage rate during the preparation of probiotic balls Test method: Randomly select 100 pellets from each embodiment and comparative example during the processing, i.e., the semi-finished product obtained in step (3). Calculation method: Breakage rate = n1 / 100×100%: where n1 is the number of broken pellets in the semi-finished product.

[0102] (5) Eccentricity of probiotic balls Test method: 100 probiotic pellets were randomly selected from each example and comparative example. Calculation method: Eccentricity = m / 100 × 100%; where m is the number of eccentric particles in the probiotic pellet. Definition of eccentric particles: The distance between the inner core and the outer rubber layer is less than 0.1 cm, and the position of the inner core does not change when vibrated or shaken.

[0103] The test results are shown in Table 4 below.

[0104] Table 4

[0105] Generally, some waste is generated during the encapsulation process of probiotic pellets, and the encapsulation rate is a key indicator for evaluating the efficiency of the pellet encapsulation process. The data above shows that factors such as the cross-linking and curing of the inner core, the semi-solid oil in the oil layer, and the mass ratio of each layer play a crucial role in achieving a high encapsulation rate in the one-step pelleting process of this invention. Correspondingly, when cross-linking and curing cannot occur between the inner core material and the oil layer material, the protective effect on the probiotics is reduced, leading to a significant decrease in viable bacteria count, an increase in breakage rate, and an increase in eccentricity. If the oil layer material is replaced with corn syrup of equal mass, the protection of the oil layer is lost, causing probiotic migration and a decrease in viable bacteria count. When the mass ratio is unreasonable, the protective effect of the oil layer is limited, and the high eccentricity leads to a decrease in viable bacteria count. If the oil is semi-solid, it is semi-solid at room temperature and has low shear resistance; under room temperature and low temperature conditions, the internal pressure of the probiotic pellets is high, resulting in a high breakage rate.

[0106] Test Example 2 (1) Heat resistance Test method: 100 probiotic pellets were randomly selected from each example and comparative example and placed in a 250ml beaker. 100ml of distilled water was added, and the mixture was sterilized in an autoclave at 100℃ for 10 minutes. The unbroken pellet rate was then calculated. The unbroken pellet rate was calculated as n² / 100 × 100%, where n² was the number of unbroken pellets.

[0107] (2) Shear resistance Test method: 100 probiotic pellets were randomly selected from each example and comparative example and placed in a 250ml beaker. 100ml of distilled water was added, and the mixture was treated at 700r / min for 20min. The unbroken pellet rate was then calculated. The unbroken pellet rate was calculated as n3 / 100 × 100%, where n3 was the number of unbroken pellets.

[0108] (3) Acid resistance Test method: 100 probiotic pellets from each example and comparative example were randomly selected and placed in 250ml beakers. 100ml of a pH 3.0 aqueous solution prepared using lactic acid was added. After one month, the unbroken pellet rate was calculated. The unbroken pellet rate was calculated as n4 / 100 × 100%, where n4 was the number of unbroken pellets.

[0109] The test results are shown in Table 5.

[0110] Table 5

[0111] The heat resistance, shear resistance, and acid resistance of probiotic balls in downstream applications have a key impact on the quality of the final product. As can be seen from the above data, the heat resistance, shear resistance, and acid resistance of probiotic balls are mainly related to the composition of the colloidal protective agent and the cross-linking and curing effect of the curing agent in the oil protective layer. When the cross-linking and curing effect is weak, the protective layer of the probiotic balls is not strong enough, the undamaged rate is low, and the heat resistance decreases.

[0112] Test Example 3 Sensory Evaluation Test subjects: Yogurt randomly selected from each example and comparative example.

[0113] Testing Method: Fifty sensory evaluators were invited to taste the above-mentioned yogurt sample containing probiotic balls. The evaluators gave the sample an overall rating based on their preference, on a scale of 0 to 5, where 0 indicates strong dislike, 3 indicates acceptable, and 5 indicates strong liking. The average rating from the 50 sensory evaluators was used as the sensory score for the sample. The sensory scores are shown in Table 6.

[0114] Test Method: Fifty sensory evaluators were invited to taste the probiotic balls in the above-mentioned yogurt. The evaluators rated the flavor acceptability on a scale of 0 to 5, where 0 indicates strong rejection, 3 indicates acceptable, and 5 indicates strong acceptance. The average score of the 50 sensory evaluators was used as the sensory score for the sample. The sensory scores are shown in Table 6.

[0115] Table 6

[0116] The data above shows that the strength and presence of cross-linking curing agents in the core and oil layer directly affect sensory evaluation and flavor acceptance; whether sweeteners are added to the oil layer inside the probiotic balls also affects sensory evaluation and flavor acceptance. When cross-linking curing is weak or absent, the probiotic balls have a soft, chewy texture and lack elasticity, resulting in lower preference and flavor acceptance scores; similarly, when no sweeteners are added to the probiotic balls, preference and flavor acceptance scores are also low.

[0117] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A probiotic sphere, characterized in that, is obtained by using an inner core raw material, an oil layer raw material and a rubber layer raw material to form drop pills by one-step drop pill method, and then mixing the drop pills with a solution containing calcium salt after cooling; The inner core raw material is used to form the inner core of the probiotic ball; The oil layer raw material is used to form an oil layer on the surface of the inner core; The rubber layer raw material is used to form a rubber layer on the surface of the oil layer; The inner core raw material includes probiotics and uses a first water-soluble protective agent containing sodium alginate as a carrier of the probiotics; the rubber layer raw material includes a second water-soluble protective agent containing sodium alginate; In the preparation of the one-step drop pill method, the curing agent in the oil layer raw material migrates to the inner core raw material and the interface between the oil layer and the inner core, and crosslinks and cures with the sodium alginate in the first water-soluble protective agent; the curing agent in the oil layer raw material migrates to the rubber layer raw material and the interface between the oil layer and the rubber layer, and crosslinks and cures with the sodium alginate in the second water-soluble protective agent; The curing agent is selected from one or a combination of two or more of calcium chloride, calcium lactate, calcium citrate, calcium gluconate, calcium stearoyl lactate and triethyl citrate calcium.

2. The probiotic sphere according to claim 1, characterized in that, The mass ratio of the inner core raw material to the oil layer raw material is 1:(0.5-1.5); And / or, the mass ratio of the oil layer raw material to the rubber layer raw material is 1:(1-3).

3. The probiotic sphere according to claim 1, wherein The oil layer raw material further includes oil, and the mass ratio of the curing agent to the oil is (0.1-5):

100.

4. The probiotic sphere according to claim 1, wherein The mass content of sodium alginate in the first water-soluble protective agent is 10-20%.

5. The probiotic sphere of claim 1, wherein, The mass content of probiotic bacteria in the inner core raw material is 1 x 10 6 ~1 x 10 13 CFU / g.

6. The probiotic sphere of claim 1, wherein, The mass content of sodium alginate in the second water-soluble protective agent is 8-15%; and the mass content of calcium salt in the solution containing calcium salt is 0.5-5%.

7. The probiotic sphere of claim 1, wherein, The first water-soluble protective agent further includes a substance A; the substance A is selected from one or a combination of two or more of gellan gum, agar, gelatin, konjac gum, pectin, carrageenan, gum arabic, locust bean gum, xanthan gum, guar gum, peach gum, red algae gum and glycerol; And / or, the second water-soluble protective agent further includes a substance B; the substance B is selected from one or a combination of two or more of gellan gum, agar, gelatin, konjac gum, pectin, carrageenan, gum arabic, locust bean gum, xanthan gum, guar gum, peach gum, red algae gum and glycerol.

8. The probiotic balls according to any one of claims 1 to 7, characterized in that, The oil layer raw material further includes a sweetener, and the sweetener is selected from one or a combination of two or more of ammonium glycyrrhizinate, monopotassium glycyrrhizinate, tripotassium glycyrrhizinate, stearyl glycyrrhizinate, sucralose and acesulfame potassium.

9. A process for the preparation of the probiotic spheres according to any one of claims 1 to 8, characterized in that, Comprise: is obtained by using an inner core raw material, an oil layer raw material and a rubber layer raw material to form drop pills by one-step drop pill method, and then mixing the drop pills with a solution containing calcium salt after cooling; The inner core raw material forms the inner core of the probiotic ball; The oil layer raw material forms an oil layer on the surface of the inner core; The rubber layer raw material forms a rubber layer on the surface of the oil layer; The inner core raw material includes probiotics and uses a first water-soluble protective agent containing sodium alginate as a carrier of the probiotics; the rubber layer raw material includes a second water-soluble protective agent containing sodium alginate; In the one-step drop pill method, the oil layer raw material is in contact with the inner core raw material and the rubber layer raw material, the curing agent in the oil layer raw material migrates to the interface between the inner core raw material and the oil layer and is cross-linked and cured with sodium alginate in the first water-soluble protective agent, and the curing agent in the oil layer raw material migrates to the interface between the rubber layer raw material and the oil layer and is cross-linked and cured with sodium alginate in the second water-soluble protective agent. The curing agent is selected from one or a combination of two or more of calcium chloride, calcium lactate, calcium citrate, calcium gluconate, calcium stearoyl lactate, and calcium triethyl citrate.

10. A food product, characterized by, The probiotic pill of any one of claims 1-8 or the probiotic pill prepared by the method of claim 9.

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