A natural oil gel bead targeting colon and its preparation method and application

Abstract

The application provides a natural oil gel bead targeting colon and a preparation method and application thereof, and belongs to the technical field of natural oil gel beads. A lecithin aqueous solution is mixed with natural oil to obtain a natural oil emulsion through high-speed shearing; a sodium alginate aqueous solution is mixed with a pectin aqueous solution to obtain a compound solution; the natural oil emulsion is mixed with the compound solution to obtain a mixed solution through high-speed shearing; the mixed solution is added dropwise into a calcium lactate solution, soaked and crosslinked, and then cleaned to obtain the natural oil gel bead. The emulsion containing natural oil is fixed in the crosslinked pectin-sodium alginate-calcium lactate structure, and the natural oil gel bead has the dual characteristics of emulsion and gel. The prepared gel bead has good taste and smell, retains complete and small-loss nutritional ingredients, can prolong the shelf life, and can target the colon.

Description

Technical Field

[0001] This invention belongs to the field of natural oil gel beads technology, and particularly relates to a natural oil gel bead targeting the colon, its preparation method and application. Background Technology

[0002] Natural oils are a class of hydrophobic substances derived from animal and plant tissues, primarily composed of triglycerides, and are an important source of essential fatty acids for the human body. As an indispensable nutrient component, their functions encompass energy supply, transport of fat-soluble vitamins, maintenance of cell membrane structure, and regulation of various physiological metabolisms, finding wide applications in food processing, nutritional supplements, pharmaceuticals, and cosmetics. Among them, n-3 polyunsaturated fatty acids (n-3 PUFAs), including eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), have become a research hotspot in food science, nutrition, and medicine due to their significant physiological activities in cardiovascular protection, anti-inflammation, neurodevelopment, and metabolic regulation.

[0003] Krill oil, as an emerging functional nutritional food ingredient, is rich in phospholipid-type n-3 unsaturated fatty acids, such as EPA and DHA, as well as the natural antioxidant astaxanthin. Compared to regular fish oil, the n-3 fatty acids in krill oil exist in the form of phospholipids, resulting in better bioavailability. Furthermore, the bioavailability of phospholipid-type n-3 is approximately 30% higher than that of triglyceride-type n-3. In addition, krill oil offers numerous health benefits, including anti-inflammatory properties, improved cardiovascular health, and cholesterol reduction. Its high astaxanthin content possesses antioxidant capabilities, helping to reduce oxidative stress levels in the body and working synergistically with n-3 fatty acids to enhance the health benefits of krill oil.

[0004] The fishy smell of krill oil mainly comes from its complex lipid composition and various easily oxidized components. These components readily produce unique volatile compounds during oxidation, leading to unpleasant flavors. Specifically, the fishy-smelling substances include unsaturated esters, amines, trimethylamine, trimethylamine oxide, and dimethyl sulfide. Among these, unsaturated esters and amines are the primary sources of the fishy smell.

[0005] Krill oil is primarily absorbed in the small intestine after ingestion. The phospholipids in krill oil are amphiphilic, meaning they are absorbed almost 100% through cells and do not require liver metabolism, allowing direct absorption into the bloodstream. Krill oil can have even greater effects if absorbed in the colon, such as: anti-inflammatory effects, as the n-3 fatty acids in krill oil work in the colon to reduce inflammatory responses; regulating blood lipids: diabetic patients often have abnormal blood lipid levels, and the n-3 fatty acids in krill oil help regulate these levels; improving insulin sensitivity: krill oil may help reduce insulin resistance and improve insulin sensitivity; gut health: krill oil helps maintain a healthy intestinal lining, prevents intestinal infections, and may improve glycemic control and insulin sensitivity by regulating the gut microbiome.

[0006] Currently, krill oil is mainly available as a health supplement, with softgels being the most common form. These softgels are convenient to carry and consume, effectively preserving the nutritional components and extending shelf life. Krill oil powder, produced through processes like spray drying, is also readily added to other foods or health supplements. However, there are currently no krill oil products specifically targeting the colon. Summary of the Invention

[0007] In view of this, one of the objectives of the present invention is to provide a method for preparing natural oil gel beads.

[0008] The second objective of this invention is to provide natural lipid gel beads for targeting the colon prepared by the aforementioned preparation method.

[0009] A third objective of this invention is to provide the application of the natural oil gel beads or the preparation method in the preparation of food, health products, and drug delivery systems.

[0010] To achieve the above-mentioned objectives, the present invention provides the following technical solution: This invention provides a method for preparing natural oil gel beads, comprising the following steps: Lecithin was dissolved in water to obtain a 1wt%~5wt% lecithin aqueous solution. The lecithin aqueous solution was mixed with natural oils and sheared at high speed to obtain a natural oil emulsion. Sodium alginate was dissolved in water to obtain a sodium alginate aqueous solution of 1wt%~5wt%; Dissolve pectin in water to obtain a 1wt%~5wt% pectin aqueous solution; A sodium alginate aqueous solution and a pectin aqueous solution were mixed to obtain a compound solution; The natural oil emulsion is mixed with the compound solution and subjected to high-speed shearing to obtain the mixed solution; Dissolve calcium lactate in water to obtain a calcium lactate solution of 1wt%~5wt%; The mixed solution was added dropwise to a calcium lactate solution, soaked and cross-linked, and then washed to obtain natural oil gel beads.

[0011] Preferably, the natural oil includes krill oil.

[0012] Preferably, the volume ratio of lecithin aqueous solution to natural oil is 1 to 9:1.

[0013] Preferably, the volume ratio of sodium alginate aqueous solution to pectin aqueous solution is (3:7) to (7:3).

[0014] Preferably, the volume ratio of the natural oil emulsion to the compound solution is (3:7) to (7:3).

[0015] Preferably, the high-speed shearing speed is 5000~20000 rpm and the shearing time is 1~6 min.

[0016] Preferably, the mixed solution is added dropwise 5-15 cm above the calcium lactate solution, and the soaking and cross-linking time is 1-9 min.

[0017] Preferably, the method further includes: mixing natural oleogel beads with a mixed solution, dripping the natural oleogel beads encapsulating the mixed solution into a calcium lactate solution, soaking and cross-linking the beads, and then washing them.

[0018] The present invention also provides natural lipogel beads for targeting the colon prepared by the aforementioned preparation method.

[0019] The present invention also provides the application of the natural oil gel beads or the preparation method thereon in the preparation of food, health products and drug delivery systems.

[0020] Compared with the prior art, the present invention has the following beneficial effects: This invention provides a method for preparing the aforementioned natural oil gel beads. The method involves immobilizing emulsion droplets containing natural oils within a cross-linked sodium alginate-calcium lactate structure, thus possessing both emulsion and gel properties. Pectin, as a key gelling component, remains stable in the acidic environment of the stomach and small intestine, successfully transporting nutrients to the colon. In the specific environment of the colon, the structure of the gel beads changes, allowing for precise release of nutrients. This targeted sustained-release mechanism not only prolongs the duration of action of krill oil in the digestive tract but also effectively prevents the destruction of nutrients by gastric acid and digestive enzymes, significantly improving the bioavailability of krill oil.

[0021] This invention provides natural oil gel beads targeting the colon, using only lecithin as an emulsifier and natural oils as the oil source for emulsification, thus preparing an emulsion. This method is convenient and safe. The natural oil gel beads provided by this invention have a significantly reduced fishy smell and a pleasant taste and aroma. The nutritional components are well preserved with minimal loss, and the natural oil nutrients are protected to a certain extent, extending the shelf life. Compared to capsules, the natural oil gel beads of this invention are easier to swallow, improving palatability and compliance for special populations such as children, the elderly, and patients with swallowing difficulties, thus opening up new directions for the design and development of oral nutritional dosage forms. Attached Figure Description

[0022] Figure 1 The preparation process of natural oil gel beads; Figure 2 The krill oil gel beads prepared in Example 15; Figure 3 The krill oil gel beads prepared in Example 16; Figure 4 The results of the experiment simulating gastrointestinal fluid with krill oil gel beads prepared in Example 15 are shown. Detailed Implementation

[0023] This invention provides a method for preparing natural oil gel beads, comprising the following steps: dissolving lecithin in water to obtain a 1wt%~5wt% lecithin aqueous solution; mixing the lecithin aqueous solution with natural oils and performing high-speed shearing to obtain a natural oil emulsion; dissolving sodium alginate in water to obtain a 1wt%~5wt% sodium alginate aqueous solution; dissolving pectin in water to obtain a 1wt%~5wt% pectin aqueous solution; mixing the sodium alginate aqueous solution and the pectin aqueous solution to obtain a compound solution; mixing the natural oil emulsion with the compound solution and performing high-speed shearing to obtain a mixed solution; dissolving calcium lactate in water to obtain a 1wt%~5wt% calcium lactate solution; adding the mixed solution dropwise to the calcium lactate solution, soaking and cross-linking, and washing to obtain natural oil gel beads. The preparation process is as follows: Figure 1 As shown.

[0024] Sodium alginate is a natural polysaccharide, while calcium lactate is a water-soluble calcium salt. Both act as cross-linking agents during the formation of gel beads, giving them better stability and mechanical properties. Gel beads made from these two materials exhibit good pH sensitivity, displaying different swelling characteristics under different gastrointestinal environments. Pectin is a commonly used thickener and gelling agent in food, possessing good biocompatibility and biodegradability. In the gastrointestinal tract, pectin gel beads remain stable in gastric acid and the small intestine, while their structure changes under the pH conditions of the colon, enabling targeted and sustained release of nutrients. This characteristic gives pectin gel beads a significant advantage in colonic targeted delivery.

[0025] In the preparation method of the present invention, the natural oil preferably includes krill oil. The lecithin is preferably soluble in water under heating conditions, preferably water bath heating, preferably at a temperature of 55-65°C, more preferably at 60°C, and preferably for 25-35 minutes, more preferably 30 minutes; the concentration of the lecithin aqueous solution is preferably 1.5wt%-4.5wt%, more preferably 2wt%-4wt%, more preferably 2.5wt%-3.5wt%; the concentration of the sodium alginate aqueous solution is preferably 1.5wt%-4.5wt%, more preferably 2wt%-4wt%, more preferably 2.5wt%-3.5wt%; the concentration of the pectin aqueous solution is preferably 1.5wt%-4.5wt%, more preferably 2wt%-4wt%, more preferably 2.5wt%-3.5wt%, and if the pectin is difficult to dissolve in water, it is preferable to refrigerate it at 4°C for 24 hours to obtain the pectin aqueous solution; the concentration of the calcium lactate solution is preferably 1.5wt%-4.5wt%, more preferably 2wt%-4wt%, more preferably 2.5wt%-3.5wt%. This invention has found that the concentrations of sodium alginate aqueous solution, pectin aqueous solution, and calcium lactate solution directly affect whether gel beads can solidify. The preparation method provided by this invention can obtain gel beads with good solidification effect.

[0026] In the preparation method of this invention, the volume ratio of lecithin aqueous solution to natural oil is preferably 1 to 9:1, and in some examples it can be 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1 or 9:1. The volume ratio of sodium alginate aqueous solution to pectin aqueous solution is preferably (3:7) to (7:3), and in some examples it can be 3:7, 4:6, 5:5, 6:4 or 7:3. The volume ratio of natural oil emulsion to compound solution is preferably (3:7) to (7:3), and in some examples it can be 3:7, 4:6, 5:5, 6:4 or 7:3. This invention has found that if the content of natural oil is too high, it cannot solidify, and if the content is too low, it cannot meet the market demand for natural oil gel beads.

[0027] In the preparation method of this invention, the high-speed shearing speed is preferably 5000~20000 rpm, more preferably 8000~15000 rpm, and even more preferably 10000~12000 rpm; the shearing time is preferably 1~6 min, more preferably 1.5~4.5 min, and even more preferably 2~3 min. Shearing with a high-speed shearing machine ensures complete and uniform mixing. The size of the gel beads can be changed by controlling the diameter of the outlet tube and the dripping speed. The diameter of the outlet tube is preferably 0.1~0.3 mm, and the dripping speed is preferably 0.5~3 s / drop; the diameter of the gel beads is preferably 0.2~3.0 mm, more preferably 0.5~2.0 mm. This invention can prepare gel beads of different particle sizes simply by adjusting the diameter of the outlet tube and the dripping speed, without the need for complex equipment or multi-step processes; the obtained gel beads have good particle size uniformity, which can significantly reduce problems such as uneven gel bead size, adhesion, and tailing, resulting in high batch-to-batch consistency. The preparation method of the present invention is simple to operate and low in cost: it does not require expensive equipment such as microfluidics and high-pressure homogenization, and is suitable for laboratory pilot-scale and large-scale preparation.

[0028] In the preparation method of the present invention, the mixed solution is preferably added dropwise at a position 5-15 cm above the calcium lactate solution, more preferably at a position 8-10 cm above the calcium lactate solution; the soaking and crosslinking time is preferably 1-9 min, more preferably 2-5 min.

[0029] The preparation method of the present invention further includes: mixing natural oil gel beads with a mixed solution, dripping the natural oil gel beads encapsulating the mixed solution into a calcium lactate solution, soaking and cross-linking, and then washing. The present invention mixes the natural oil gel beads with the mixed solution, preferably dripping them into the calcium lactate solution one particle at a time, which can further improve the sensory evaluation and stability of the natural oil gel beads.

[0030] The present invention also provides natural lipogel beads for targeting the colon prepared by the aforementioned preparation method.

[0031] The present invention also provides the application of the natural oil gel beads or the preparation method thereon in the preparation of food, health products and drug delivery systems.

[0032] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0033] Example 1 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4℃ for 24 hours to obtain a 3wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 3:7, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was dissolved in water by stirring to obtain a 5 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube at a drip rate of 1 s / drop) from a height of 5 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 10.74%.

[0034] Example 2 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4℃ for 24 hours to obtain a 3wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 3:7, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was dissolved in water by stirring to obtain a 5 wt% calcium lactate solution. The mixed solution was then slowly added dropwise (using a 0.3 mm diameter outlet tube at a rate of 1 drop per second) from a height of 15 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 10.74%.

[0035] Example 3 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube and a drip rate of 1 second / drop) from a height of 5cm above the surface of the calcium lactate solution. After soaking and cross-linking for 1 minute, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0036] Example 4 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube at a drip rate of 1 second / drop) from a height of 15cm above the surface of the calcium lactate solution. After soaking and cross-linking for 1 minute, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0037] Example 5 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube and a drip rate of 1 second / drop) from a height of 5cm above the surface of the calcium lactate solution. After soaking and cross-linking for 9 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0038] Example 6 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube at a drip rate of 1 second / drop) from a height of 15cm above the surface of the calcium lactate solution. After soaking and cross-linking for 9 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0039] Example 7 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 5 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 5 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube and a drip rate of 1 s / drop) from a height of 10 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 9 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0040] Example 8 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 5 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 1:1 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 3:7, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube and a drip rate of 1 second / drop) from a height of 10cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 10.74%.

[0041] Example 9 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4℃ for 24 hours to obtain a 3wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 3:7 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 3:7, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube and a drip rate of 1 second / drop) from a height of 10cm above the surface of the calcium lactate solution. After soaking and cross-linking for 1 minute, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 10.74%.

[0042] Example 10 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 3:7 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 1 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube at a drip rate of 1 s / drop) from a height of 10 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0043] Example 11 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 7:3 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 1 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube at a drip rate of 1 s / drop) from a height of 10 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0044] Example 12 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 5 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 3 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 7:3 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 5 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube at a drip rate of 1 s / drop) from a height of 10 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0045] Example 13 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 5 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 7:3 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube and a drip rate of 1 second / drop) from a height of 5cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0046] Example 14 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a water bath at 60°C for 30 minutes to obtain a 4.6 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 5.89 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 3 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 5 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 7:3 to obtain a compound solution. Krill oil emulsion and compound solution were mixed at a volume ratio of 1:1, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 5.89 min) to obtain a mixed solution. Calcium lactate was added to water and stirred to dissolve, obtaining a 3wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3mm diameter outlet tube at a rate of 1 second / drop) from a height of 15cm above the surface of the calcium lactate solution. After soaking and cross-linking for 5 minutes, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content of these gel beads was 17.9%.

[0047] Example 15 A method for preparing natural oil gel beads, comprising the following steps: Lecithin was added to water and heated in a 60°C water bath for 30 minutes to obtain a 3.2 wt% lecithin aqueous solution. After cooling, the lecithin aqueous solution was mixed with krill oil, with krill oil accounting for 35.8%. The mixture was sheared using a high-speed shearing machine at a shearing speed of 10,000 rpm for 3.9 minutes to obtain a krill oil emulsion. Sodium alginate was dissolved in water to obtain a 4.38 wt% sodium alginate aqueous solution; pectin was added to water and stirred to dissolve. If it was difficult to dissolve, it was placed at 4°C and refrigerated for 24 hours to obtain a 2.84 wt% pectin aqueous solution; the sodium alginate aqueous solution and the pectin aqueous solution were mixed at a volume ratio of 57.7:42.3 to obtain a compound solution. The krill oil emulsion and the compound solution were mixed at a volume ratio of 45.5:54.5, stirred evenly, and then sheared using a high-speed shearing machine (10000 rpm, 3.9 min) to obtain the mixed solution. Calcium lactate was dissolved in water by stirring to obtain a 2.5 wt% calcium lactate solution. The mixed solution was slowly added dropwise (using a 0.3 mm diameter outlet tube at a drip rate of 1 s / drop) from a height of 8 cm above the surface of the calcium lactate solution. After soaking and cross-linking for 2.55 min, the solution was removed and washed with purified water to remove surface ions, thus obtaining krill oil gel beads. The krill oil content in these gel beads was 16.289%. The obtained krill oil gel beads are shown below. Figure 2 As shown.

[0048] Example 16 A method for preparing natural oil gel beads differs from that in Example 15 in that: The obtained krill oil gel beads were added to a mixed solution, coating their surface with a sodium alginate-pectin mixture. Individual beads were then dropped into a calcium lactate solution for cross-linking. After soaking, the beads were removed and washed with purified water to remove surface ions. The resulting krill oil gel beads are shown below. Figure 3 As shown.

[0049] Comparative Example 1 A method for preparing natural oil gel beads differs from Example 15 in that the concentration of the sodium alginate aqueous solution is 0.5 wt%. The krill oil content in the gel beads is 16.289%.

[0050] Comparative Example 2 A method for preparing natural oil gel beads differs from Example 15 in that the concentration of the sodium alginate aqueous solution is 6 wt%. The krill oil content in the gel beads is 16.289%.

[0051] Comparative Example 3 A method for preparing natural oil gel beads differs from Example 15 in that the concentration of the pectin aqueous solution is 0.5 wt%. The krill oil content in the gel beads is 16.289%.

[0052] Comparative Example 4 A method for preparing natural oil gel beads differs from Example 15 in that the concentration of the pectin aqueous solution is 6 wt%. The krill oil content in the gel beads is 16.289%.

[0053] Comparative Example 5 A method for preparing natural oil-based gel beads differs from Example 15 in that: an aqueous solution of sodium alginate and an aqueous solution of pectin are mixed at a volume ratio of 10:90 to obtain a compound solution. The gel beads contain 16.289% krill oil.

[0054] Comparative Example 6 A method for preparing natural oil gel beads differs from Example 15 in that: sodium alginate aqueous solution and pectin aqueous solution are mixed at a volume ratio of 80:20 to obtain a compound solution. The krill oil content in this gel bead is 16.289%.

[0055] Comparative Example 7 A method for preparing natural oil gel beads differs from Example 15 in that: krill oil emulsion and a compound solution are mixed at a volume ratio of 10:90. The krill oil content in the gel beads is 3.58%.

[0056] Comparative Example 8 A method for preparing natural oil gel beads differs from Example 15 in that: krill oil emulsion and a compound solution are mixed at a volume ratio of 80:20. The krill oil content in the gel beads is 28.64%.

[0057] Comparative Example 9 A method for preparing natural oil gel beads differs from Example 15 in that the concentration of the calcium lactate solution is 0.5 wt%. The krill oil content in the gel beads is 16.289%.

[0058] Comparative Example 10 A method for preparing natural oil-based gel beads differs from Example 15 in that the mixed solution is slowly added dropwise to the calcium lactate solution at a height of 1 cm above the surface. The gel beads contain 16.289% krill oil.

[0059] Comparative Example 11 A method for preparing natural oil gel beads differs from Example 15 in that the mixed solution is slowly added dropwise to the calcium lactate solution at a height of 20 cm above the surface of the calcium lactate solution.

[0060] Comparative Example 12 A method for preparing natural oil gel beads differs from that in Example 15 in that: the beads are soaked and crosslinked for 0.5 min before being removed.

[0061] Comparative Example 13 A method for preparing natural oil gel beads differs from that in Example 15 in that: the beads are removed after soaking and cross-linking for 15 minutes.

[0062] Experimental Example 1 Properties of krill oil gel beads prepared by different methods.

[0063] The krill oil gel beads prepared in Examples 1 to 16 and Comparative Examples 1 to 13 were used as samples for sensory evaluation, stability evaluation, encapsulation efficiency verification and simulated digestion experiments.

[0064] 1. Sensory evaluation: The odor, color and gloss, size and appearance, uniformity and texture of krill oil gel beads prepared by different methods were evaluated. Each sample was evaluated three times, and the average value of the three evaluation results was recorded. The evaluation criteria are shown in Table 1, and the evaluation results are shown in Table 2.

[0065] Table 1 Sensory Evaluation Criteria for Krill Oil Gel Beads

[0066] Table 2 Sensory evaluation results of krill oil gel beads

[0067] 2. Stability evaluation: Fifty krill oil gel beads were placed in a 10 mL centrifuge tube, water was added to a final volume of 5 mL, and the mixture was stored at room temperature for 7 days. At the beginning and end of the experiment, samples of the soaking solution were taken to detect the degree of emulsion seepage. The absorbance of an equal volume of sample at a wavelength of 534 nm was measured using an ELISA reader to determine the turbidity of the solution and assess its stability. The results are shown in Table 3.

[0068] Table 3. Stability of krill oil gel beads

[0069] According to the data in Tables 2 and 3, the krill oil gel beads obtained by the preparation method of the present invention have no obvious unpleasant odor, are acceptable, have a uniform and bright orange color, are clear and glossy, are small, spherical in shape, have a full appearance, smooth surface, no protrusions or bubbles, are uniform in size, have a dense texture, good elasticity, and are not easily damaged. The krill oil gel beads obtained by the present invention have obvious sensory advantages and stability. In Example 16, the krill oil gel beads obtained in Example 15 were further coated with a sodium alginate pectin mixed solution and then crosslinked again, which further improved the sensory evaluation and stability of the krill oil gel beads. In Comparative Example 1, the concentration of sodium alginate aqueous solution was reduced, resulting in the problem of non-coagulation; in Comparative Example 2, the concentration of sodium alginate solution was increased, but it did not improve the properties of the gel beads. Comparative Examples 3 and 4 changed the concentration of pectin solution, but their effects were not as good as those of Example 15. In Comparative Example 5, the reduced proportion of sodium alginate and pectin significantly decreased sensory evaluation and stability. In Comparative Example 6, the increased proportion of sodium alginate and pectin resulted in poorer sensory evaluation and stability compared to Example 15. Comparative Example 7 had a low krill oil content in its gel beads, failing to meet market demand. Comparative Example 8 had excessive krill oil emulsion, leading to a failure to solidify. Comparative Example 9 experienced a failure to solidify when the calcium lactate solution concentration was reduced. Comparative Example 10 experienced a failure to drip the mixed solution into the calcium lactate solution when the drop height was reduced. Comparative Example 11 showed that increasing the drop height resulted in irregularly shaped gel beads that were prone to breakage. Comparative Example 12 showed that reducing the soaking cross-linking time prevented complete solidification of the gel beads, while Comparative Example 13 extended the soaking cross-linking time, increasing time costs, and both the stability and sensory evaluation of the gel beads decreased with prolonged cross-linking time.

[0070] 3. Determination of encapsulation efficiency: Accurately weigh 5.0 g of freshly prepared krill oil gel beads and blot dry with filter paper. Add 30 mL of n-hexane, gently shake and wash for 2 min, then immediately filter. Remove the solvent by rotary evaporation at 40℃, dry and weigh to obtain the surface oil mass (Wsurface). Grind the gel beads after removing the surface oil, add 50 mL of petroleum ether (boiling range 30~60℃), and extract by shaking at 25℃ for 2 h. Filter and repeat the extraction twice with the residue. Combine the filtrates, evaporate the solvent, dry and weigh to obtain the extracted oil mass (Wextract). Calculate the encapsulation efficiency using the following formula: Encapsulation efficiency (EE%) = W_extracted / W_theoretical × 100%. Where W_theoretical is the mass of krill oil added during the preparation of the krill oil gel beads. The results are shown in Table 4.

[0071] Table 4 Encapsulation efficiency of krill oil gel beads

[0072] As shown in Table 4, the encapsulation efficiency of the krill oil gel beads prepared by this invention can all reach over 80%. Example 15 yielded krill oil gel beads with an encapsulation efficiency of 92.79%. In Example 16, the krill oil gel beads obtained in Example 15 were further encapsulated with a sodium alginate-pectin mixture and then crosslinked again, further improving the encapsulation efficiency. Compared with Example 15, Comparative Examples 1-6 and 8-13 changed the parameters in the preparation process, all of which significantly affected the encapsulation efficiency of the krill oil gel beads. While Comparative Example 7 improved the encapsulation efficiency by reducing the krill oil content, it still could not meet market demands.

[0073] 4. Simulated Digestion Experiment: Using the krill oil gel beads prepared in Example 15 as experimental samples, a simulated digestion experiment was conducted by simulating gastrointestinal digestion in vitro, and a release curve was determined.

[0074] The stomach environment was prepared by mixing food samples with simulated gastric juice SGF at a 1:1 volume ratio. Twenty krill oil gel beads were placed in 10 mL of purified water as the food sample. 7.5 mL of simulated gastric juice SGF electrolyte stock solution, 1.6 mL of pepsin solution, and 5 μL of calcium chloride solution (0.3 M) were added. The pH of the system was adjusted to 3.0 with 1 M HCl solution, and a trace amount of purified water was added to bring the volume to 20 mL. The mixture was incubated for 2 h in a shaker at 150 r / min and 37 ℃, with the conical flask mouth sealed with plastic wrap to prevent evaporation. Samples were taken every 30 min, and the absorbance of an equal volume of sample at 534 nm was measured using a microplate reader to determine the turbidity and assess the digestion of the gel beads. An equal volume of simulated gastric juice digestion solution was added immediately after each sampling to maintain a constant volume.

[0075] The intestinal environment was prepared by mixing gastric chyme and simulated intestinal fluid (SIF) in a 1:1 volume ratio to simulate intestinal digestion solution. To 20 mL of gastric chyme (the chyme remaining after the in vitro simulated gastrointestinal digestion experiment), 11 mL of simulated intestinal fluid SIF electrolyte stock solution, 5.0 mL of trypsin solution, 2.5 mL of bile salt solution, and 40 μL of calcium chloride solution (0.3 M) were added. The pH of the system was adjusted to 7.0 with 1 M NaOH solution, and then a trace amount of pure water was added to bring the volume of the mixture to 40 mL. The mixture was incubated in a shaker at 150 r / min and 37 ℃ for 26 h, with the mouth of the conical flask sealed with plastic wrap to prevent liquid evaporation. Samples were taken every 30 min for the first two hours, then every 8 h for a total of two samplings, and then every 4 h for a total of two samplings. The absorbance of an equal volume of sample at 534 nm was measured using a microplate reader to determine the turbidity of the solution and assess the digestion status of the gel beads. Immediately after each sampling, an equal volume of simulated intestinal digestive fluid was added to maintain a constant volume.

[0076] according to Figure 4 The experimental results show that the krill oil gel beads obtained in Example 15 were not completely digested after 6 hours under simulated digestion conditions in vitro, indicating that they can reach the colon and have colon-targeting properties. The longer the time until complete digestion, the better the targeting properties. The krill oil gel beads of the present invention have a longer time in the gastrointestinal tract, indicating that the krill oil release rate is slow and can achieve colon-targeting effects.

[0077] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing natural oil gel beads, characterized in that, Includes the following steps: Lecithin was dissolved in water to obtain a 1wt%~5wt% lecithin aqueous solution. The lecithin aqueous solution was mixed with natural oils and sheared at high speed to obtain a natural oil emulsion. Sodium alginate was dissolved in water to obtain a sodium alginate aqueous solution of 1wt%~5wt%; Dissolve pectin in water to obtain a 1wt%~5wt% pectin aqueous solution; A sodium alginate aqueous solution and a pectin aqueous solution were mixed to obtain a compound solution; The natural oil emulsion is mixed with the compound solution and subjected to high-speed shearing to obtain the mixed solution; Dissolve calcium lactate in water to obtain a calcium lactate solution of 1wt%~5wt%; The mixed solution was added dropwise to a calcium lactate solution, soaked and cross-linked, and then washed to obtain natural oil gel beads.

2. The preparation method according to claim 1, characterized in that, The natural oils include krill oil.

3. The preparation method according to claim 1, characterized in that, The volume ratio of lecithin aqueous solution to natural oil is 1~9:

1.

4. The preparation method according to claim 1, characterized in that, The volume ratio of sodium alginate aqueous solution to pectin aqueous solution is (3:7) to (7:3).

5. The preparation method according to claim 1, characterized in that, The volume ratio of natural oil emulsion to compound solution is (3:7) to (7:3).

6. The preparation method according to claim 1, characterized in that, The high-speed shearing speed is 5000~20000 rpm, and the shearing time is 1~6 min.

7. The preparation method according to claim 1, characterized in that, The mixed solution was added dropwise 5-15 cm above the calcium lactate solution, and the soaking and cross-linking time was 1-9 min.

8. The preparation method according to any one of claims 1 to 7, characterized in that, Also includes: Mix natural oleogel beads with a mixed solution, then drop the natural oleogel beads containing the mixed solution into a calcium lactate solution, soak and crosslink them, and then wash them.

9. A natural oil-based gel bead targeting the colon, characterized in that, It is prepared by any one of the preparation methods of claims 1 to 8.

10. The preparation method according to any one of claims 1 to 8 or the natural oil gel beads according to claim 9 in the preparation of food, health products and drug delivery systems.

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