Dietary nutrition supplement and preparation process thereof

Abstract

The invention belongs to the field of nutritional supplements, and particularly relates to a dietary nutritional supplement and a preparation process thereof. According to the supplement, a double-gel system is constructed, and galangal polysaccharide and vitamin E are entrapped. The preparation method comprises the following steps: S1, dissolving galangal polysaccharide and gelatin in deionized water, heating, stirring, and cooling to obtain hydrogel; s2, dissolving monoglyceride in olive oil, adding vitamin E in the cooling process, and cooling to obtain oleogel; and S3, heating the oil gel, mixing the heated oil gel with the hydrogel according to a volume ratio of 4: 6-6: 4, and carrying out high-speed homogenization and rapid cooling to obtain the double-gel. Hydrogel and oil gel are used for respectively entrapping hydrophilic polysaccharide and hydrophobic vitamin E, so that the problems of poor water solubility and low bioavailability of vitamin E are solved. Experimental results show that the supplement can effectively repair intestinal barrier injury. The invention provides a novel nutritional supplement scheme for improving intestinal health.

Description

Technical Field

[0001] This invention belongs to the field of nutritional supplements, specifically relating to a dietary nutritional supplement and its preparation process. Background Technology

[0002] The gut is a vital digestive and immune organ, and the integrity of the intestinal barrier is crucial for maintaining bodily health. The intestinal barrier is composed of mechanical, chemical, immune, and biological barriers. The mechanical barrier, formed by intestinal epithelial cells and their intercellular tight junction proteins (Occludin and ZO-1), is the first line of defense against harmful substances such as bacteria and endotoxins translocating into the bloodstream. Various factors, such as medications, stress, and poor diet, can lead to intestinal barrier dysfunction, damage to the tight junction structure, and "leaky gut," which is closely related to the development of various local and systemic diseases, such as inflammatory bowel disease, metabolic syndrome, and autoimmune diseases. Therefore, developing dietary supplements that can effectively protect and repair intestinal barrier function is of significant practical importance.

[0003] Currently, supplements on the market that improve gut health mainly consist of probiotics, prebiotics, dietary fiber, and some plant extracts with anti-inflammatory and antioxidant effects. Among these, polysaccharides have been extensively studied due to their prebiotic properties and immunomodulatory activity. Galangal, a traditional medicinal and edible plant, has had its extract, galangal polysaccharide, reported to have potential benefits in anti-inflammatory, antioxidant, and gut microbiota regulation. On the other hand, vitamin E is a fat-soluble antioxidant that neutralizes free radicals, protecting cell membranes, the nervous system, skeletal muscle, and the retina from oxidative damage, thereby delaying aging, reducing cellular oxygen consumption, and improving lipid metabolism.

[0004] However, directly applying these active ingredients to gut health still faces many challenges. First, vitamin E has extremely low water solubility and oral bioavailability, limiting its efficacy. Second, the simple physical mixing of galangal polysaccharides and vitamin E results in unsatisfactory stability, targeted delivery efficiency, and maintenance of bioactivity in the complex gastrointestinal environment. More importantly, existing technologies lack a delivery system capable of simultaneously and effectively delivering both water-soluble polysaccharides and fat-soluble active ingredients, and promoting their synergistic effects in the gut.

[0005] In recent years, gel delivery systems, particularly hydrogels and oleogels, have attracted attention in the food and pharmaceutical fields. Hydrogels are well-suited for encapsulating hydrophilic components, while oleogels are better suited for encapsulating hydrophobic components. However, how to construct a stable and technologically feasible dual-gel system, ensuring that the active ingredients are not only effectively released upon reaching the intestine but also exert their effects, especially regarding the specific function of intestinal barrier repair, remains a challenge and has not yet been reported. Therefore, there is an urgent need to develop novel dietary supplements and their preparation methods that can synergistically repair intestinal barrier function. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention prepares galangal polysaccharides through enzymatic hydrolysis, further screens for vitamin E that exhibits synergistic effects with galangal polysaccharides in intestinal damage repair, and then develops a process to prepare a dual-gel dietary supplement by loading galangal polysaccharides onto a hydrogel and vitamin E onto an oleogel, followed by mixing the hydrogel and oleogel in a specific ratio using a specific process. This provides a dietary supplement with promising market prospects for addressing common intestinal health issues in modern life.

[0007] On the one hand, a method for preparing a dietary supplement, the method comprising the following steps: S1. Preparation of hydrogel containing galangal polysaccharide: Dissolve galangal polysaccharide in deionized water to obtain galangal polysaccharide aqueous solution; add gelatin to the galangal polysaccharide aqueous solution, heat and stir, and then cool to obtain hydrogel; S2. Preparation of oleogel containing vitamin E: Dissolve monoglycerides in olive oil to form an oil phase mixture; add vitamin E pre-dissolved in olive oil during the cooling process of the oil phase mixture, mix well and cool to obtain oleogel; S3. Preparation of dual gels: The oleogel obtained in step S2 is heated to fluidity and then mixed with the hydrogel obtained in step S1 at a volume ratio. After homogenization, it is rapidly cooled to obtain the dietary supplement.

[0008] Furthermore, in the preparation method, in step S1, the mass percentage of Alpinia galanga polysaccharide in the hydrogel is 0.1%~0.5%.

[0009] Furthermore, in the preparation method, in step S1, the mass percentage of gelatin in the hydrogel is 6%~8%.

[0010] Furthermore, in the preparation method, in step S1, the heating and stirring conditions are: temperature 60~65℃, rotation speed 400~500rpm, and time 2~3h.

[0011] Furthermore, in the preparation method, in step S2, the mass percentage of the monoglyceride in the oleogel is 8%~10%.

[0012] Furthermore, in the preparation method, in step S2, the percentage of vitamin E in the total mass of the dual gel is 0.5% to 2%.

[0013] Furthermore, in the preparation method, in step S3, the volume ratio of the oleogel to the hydrogel is 4:6 to 6:4.

[0014] Furthermore, in the preparation method, the homogenization conditions in step S3 are: rotation speed 10000~12000 rpm, time 5~6 min.

[0015] Furthermore, in the preparation method, in step S3, the rapid cooling is achieved by stirring and cooling in an ice bath at a speed of 200-300 rpm.

[0016] Finally, dietary supplements prepared by the preparation method described in this invention are also provided.

[0017] Compared with the prior art, the technical solution provided by the present invention has at least the following beneficial effects or advantages: (1) This invention combines Alpinia galanga polysaccharide and vitamin E through a dual gel system for the first time. Experiments have shown that the two have a significant synergistic effect in repairing intestinal damage, and the repair effect is far superior to that of a single component, providing an effective solution for solving intestinal barrier dysfunction.

[0018] (2) By constructing a hydrogel-oil gel biphase system, the key technical problem of poor water solubility and low oral bioavailability of vitamin E was successfully solved, and the simultaneous and efficient encapsulation and targeted delivery of lipophilic and hydrophilic active ingredients were achieved.

[0019] (3) This supplement targets common intestinal health problems in modern life and has good market application prospects. Attached Figure Description

[0020] Figure 1 The results show the relative expression levels of tight junction proteins in the colon tissue of mice in different test groups.

[0021] Figure 2 The results show the relative expression levels of tight junction proteins in the colon tissue of mice in different test groups. Detailed Implementation

[0022] The technical solution of the present invention will be described below with reference to the embodiments. However, the present invention is not limited to the following embodiments.

[0023] To enable those skilled in the art to better understand and implement the technical solutions of the present invention, the present invention will be further described below in conjunction with specific embodiments and accompanying drawings. However, the embodiments described are not intended to limit the present invention.

[0024] Unless otherwise specified, the experimental and detection methods described in the following embodiments are conventional methods; unless otherwise specified, the reagents and materials are commercially available.

[0025] Example 1

[0026] This embodiment describes the preparation of Alpinia officinarum polysaccharide.

[0027] This embodiment describes the preparation of a crude polysaccharide solution of Alpinia galanga.

[0028] Galangal powder was obtained by thoroughly pulverizing the galangal using a traditional Chinese medicine pulverizer and passing it through an 80-mesh sieve. It was then stored in a cool, dry place for later use. 500g of galangal powder was weighed and added to 90% ethanol at a material-to-liquid ratio of 1:12 (for example, 1g galangal powder to 12g 90% ethanol). The mixture was refluxed at 80℃ for 1.5 hours, filtered, and the filtrate was collected. The residue was extracted twice more using the same method. The filtrates were combined and concentrated under reduced pressure at 55℃ to 1 / 5 of the original volume. The concentrated filtrate was stored at -20℃ for later use. The residue was dried at 60℃ until the ethanol was completely evaporated and stored at 4℃ for subsequent extraction of galangal polysaccharides. Accurately weigh 100g of the above-mentioned galangal extract residue, add deionized water at a material-to-liquid ratio of 1:18, and treat at 105℃ for 100 minutes to fully gelatinize the starch, obtaining suspension 1. Allow to cool naturally at room temperature, adjust the pH of suspension 1 to 5.5, add 1% (w / w) of α-amylase (sample mass), and enzymatically hydrolyze at 60℃ for 120 minutes to obtain suspension 2. Adjust the pH of suspension 2 to 5.0, add 1% (w / w) of glucoamylase (sample mass) and 1% (w / w) of cellulase (sample mass). The sample was enzymatically hydrolyzed at 55℃ for 16 hours to fully hydrolyze the starch and accelerate the dissolution of galangal polysaccharides, resulting in suspension 3. Suspension 3 was adjusted to pH 7.0 and treated at 105℃ for 2 hours. The filtrate was collected by suction filtration and concentrated under reduced pressure at 55℃. Anhydrous ethanol was then added to bring the ethanol concentration in the system to 80% (v / v). After slow stirring and homogenization, the mixture was allowed to stand at 4℃ for 12 hours, centrifuged at 8000g for 25 minutes, and the precipitate was collected. Deionized water was added to redissolve the precipitate and the volume was adjusted to 50 mL to obtain a crude galangal polysaccharide solution. Papain (1% of the sample content) was added to the above crude galangal polysaccharide solution for enzymatic hydrolysis at 37℃ for 5 hours. Salts were then removed by dialysis. XAD-16 macroporous resin was added, and the mixture was statically adsorbed at 37℃ and 120 rpm for 4 hours to remove small peptides and some pigments. The filtrate was then collected by suction filtration and concentrated under reduced pressure at 55℃ to obtain galangal polysaccharide.

[0029] Example 2

[0030] This embodiment describes the preparation of a bigel containing galangal polysaccharide and vitamin E.

[0031] S1. Preparation of hydrogel containing galangal polysaccharide: 0.1% of galangal polysaccharide by mass was weighed, dissolved in deionized water, and stirred until homogeneous to obtain an aqueous solution of galangal polysaccharide; 6% of gelatin by mass was weighed and added to the aqueous solution of galangal polysaccharide, stirred, and the mixture was heated to 60℃ and stirred at 400 rpm for 3 hours. Afterwards, the mixture was cooled at 4℃ for 12 hours to allow the gelatin to mix, thus obtaining the hydrogel.

[0032] S2. Preparation of oleogel: Weigh out monoglycerides at 8% of the total mass of the oleogel. Dissolve the monoglycerides completely in olive oil at 65°C to form an oil phase mixture in which monoglycerides constitute 8% of the total oil phase mass. During the cooling process of the oil phase mixture, add pre-dissolved vitamin E (weigh out 0.5% of the total mass of the two gels and dissolve it in olive oil beforehand), and mix thoroughly. Cool the mixture to room temperature and then store it in a refrigerator for 24 hours. The oleogel is then obtained.

[0033] S3, Preparation of dual gels: The prepared olegel is heated to 50°C to give it a certain degree of fluidity.

[0034] Accurately measure the oleogel and hydrogel at a volume ratio of 6:4. Slowly add the oleogel to the hydrogel while simultaneously starting a homogenizer and homogenizing at 10,000 rpm for 6 minutes. During homogenization, ensure the two gels are thoroughly mixed to form a preliminary emulsion.

[0035] Rapid cooling: The pre-emulsified mixture was rapidly transferred to an ice bath apparatus and stirred at 200-300 rpm to rapidly cool the mixture. A bigel was obtained. This bigel is labeled #1.

[0036] Example 3

[0037] This embodiment describes the preparation of a bigel containing galangal polysaccharide and vitamin E.

[0038] S1. Preparation of hydrogel containing galangal polysaccharide: 0.2% of galangal polysaccharide by mass was weighed, dissolved in deionized water, and stirred until homogeneous to obtain an aqueous solution of galangal polysaccharide; 7% of gelatin by mass was weighed and added to the aqueous solution of galangal polysaccharide, stirred, and the mixture was heated to 60℃ and stirred at 400 rpm for 3 hours. Afterwards, the mixture was cooled at 4℃ for 12 hours to allow the gelatin to mix, thus obtaining the hydrogel.

[0039] S2. Preparation of oleogel: Weigh out monoglycerides at 10% of the total mass of the oleogel. Dissolve the monoglycerides completely in olive oil at 65°C to form an oil phase mixture in which monoglycerides constitute 10% of the total oil phase mass. During the cooling process of the oil phase mixture, add pre-dissolved vitamin E (weigh out 1% of the total mass of the two gels and dissolve it in olive oil beforehand), and mix thoroughly. Cool the mixture to room temperature and then store it in a refrigerator for 24 hours. The oleogel is then obtained.

[0040] S3, Preparation of dual gels: The prepared olegel is heated to 50°C to give it a certain degree of fluidity.

[0041] Accurately measure the oleogel and hydrogel at a volume ratio of 5:5. Slowly add the oleogel to the hydrogel while simultaneously starting a homogenizer and homogenizing at 12,000 rpm for 5 minutes. During homogenization, ensure that the two gels are thoroughly mixed to form a preliminary emulsion.

[0042] Rapid cooling: The pre-emulsified mixture was rapidly transferred to an ice bath apparatus and stirred at 300 rpm to rapidly cool the mixture. A bigel was obtained. This bigel is labeled as #2.

[0043] Example 4

[0044] This embodiment describes the preparation of a bigel containing galangal polysaccharide and vitamin E.

[0045] S1. Preparation of hydrogel containing galangal polysaccharide: 0.5% of galangal polysaccharide by mass was weighed, dissolved in deionized water, and stirred until homogeneous to obtain an aqueous solution of galangal polysaccharide; 8% of gelatin by mass was weighed and added to the aqueous solution of galangal polysaccharide, stirred, and the mixture was heated to 65℃ and stirred at 500 rpm for 2 hours. Afterwards, the mixture was cooled at 4℃ for 12 hours to allow the gelatin to mix, thus obtaining the hydrogel.

[0046] S2. Preparation of oleogel: Weigh out monoglycerides at 9% of the total mass of the oleogel. Dissolve the monoglycerides completely in olive oil at 65°C to form an oil phase mixture in which monoglycerides constitute 9% of the total oil phase mass. During the cooling process of the oil phase mixture, add pre-dissolved vitamin E (weigh out 2% of the total mass of the two gels and dissolve it in olive oil beforehand), and mix thoroughly. Cool the mixture to room temperature and then store it in a refrigerator for 24 hours. The oleogel is then obtained.

[0047] S3, Preparation of dual gels: The prepared olegel is heated to 50°C to give it a certain degree of fluidity.

[0048] Accurately measure the oleogel and hydrogel at a volume ratio of 4:6. Slowly add the oleogel to the hydrogel while simultaneously starting a homogenizer and homogenizing at 11,000 rpm for 6 minutes. During homogenization, ensure the two gels are thoroughly mixed to form a preliminary emulsion.

[0049] Rapid cooling: The pre-emulsified mixture was rapidly transferred to an ice bath apparatus and stirred at 300 rpm to rapidly cool the mixture. A bigel was obtained. This bigel is labeled as #3.

[0050] Comparative Example 1 The hydrogel containing galangal polysaccharides prepared in step S1 of Example 3 was used as a contrast agent. It is labeled as contrast agent #1.

[0051] Comparative Example 2 The vitamin E-containing oleogel prepared in step S2 of Example 3 was used as a contrast agent. It is labeled as contrast agent #2.

[0052] Test case This embodiment tests the gut microbiota repair capabilities of the 1#~3# double gels prepared in Examples 2~4 and the 1#~2# contrast agents prepared in Comparative Examples 1~2.

[0053] (1) Establishing an experimental model Forty-two male SPF-grade Kunming mice (27±2g, 7 weeks old) were randomly divided into seven groups (control group, model group, double gel test groups 1#~3#, and control groups with contrast agents 1#~2#, with six mice in each group). The test and control groups were fed 0.5g / kg of the gel in the morning and administered 75mg / kg adenine solution and 300mg / kg potassium oxonate solution by gavage in the afternoon. The model group was administered 0.1mL / 10g physiological saline by gavage in the morning and 75mg / kg adenine solution and 300mg / kg potassium oxonate solution by gavage in the afternoon. The control group was administered 0.1mL / 10g physiological saline by gavage in both the morning and afternoon. Except for the above treatments, all mice were normally fed and allowed free access to food for 21 consecutive days. After 21 days, colonic tissue and cecal contents were collected.

[0054] (2) Determine the relative expression levels of tight junction protein and atresia band 1 in the colon tissue of mice under each treatment. Tight junction proteins are important indicators of maintaining the integrity of the intestinal barrier. Tight junction protein (Occludin) and atresia band 1 (ZO-1) are common tight junction proteins that play a key role in maintaining intestinal barrier function and other physiological barriers.

[0055] 20 mg of colon tissue was added to RIPA strong lysis buffer containing 1:100 PMSF and 1:50 phosphatase inhibitor. After grinding, the tissue was lysed at 4°C for 20 min, followed by centrifugation at 12,000 rpm for 20 min at 4°C, and the supernatant was collected. The concentration of each sample was then determined using a protein quantification kit, and after adjustment to ensure consistency, 5×SDS loading buffer was added. The protein was then denatured at 100°C for 10 min. Proteins were separated by SDS-PAGE electrophoresis, and then transferred to a nitrocellulose membrane. After blocking at room temperature for 1 h, the membrane was incubated overnight at 4°C with primary antibody GAPDH, tight junction protein, and atresia band 1 (antibody dilution 1:1000). Subsequently, the membrane was incubated with the corresponding secondary antibody (dilution 1:3000) at room temperature for 1 h before being immersed in ultrasensitive ELC working solution. Imaging was performed using a chemiluminescence system, and grayscale analysis was performed using ImageJ software. The final data are presented as the ratio of target protein grayscale to internal control GAPDH grayscale. The relative expression levels of tight junction protein and atresia band 1 in mouse colon tissue were measured as follows: Figure 1 ,like Figure 2 As shown.

[0056] Depend on Figure 1 and Figure 2 It can be seen that, compared with the control group, the relative expression levels of tight junction protein (Occludin) and atresia band 1 (ZO-1) in the model group were significantly reduced, indicating that the mouse intestinal barrier damage model was successfully established by gavage administration of adenine and potassium oxonate, which led to the destruction of the intestinal tight junction structure, demonstrating the reliability of the experimental system.

[0057] Compared with the model group, the expression levels of two tight junction proteins in the 1#~3# double gel groups were significantly increased, bringing them close to the levels of the normal control group. This indicates that the double gel groups exhibited significant and effective intestinal barrier repair capabilities and could effectively reverse the intestinal damage caused by the model.

[0058] The contrast agent 1 (galangal polysaccharide hydrogel) showed a certain enhancement effect on the two proteins compared with the model group, indicating that galangal polysaccharide has a certain intestinal protective effect, but the effect was significantly different from that of the two-gel comparison.

[0059] Compared with the model group, the contrast agent 2 (vitamin E oleogel) showed no increase in either protein, indicating that vitamin E oleogel alone does not have the function of repairing intestinal damage in this intestinal injury model.

[0060] This demonstrates that vitamin E and galangal polysaccharides have a synergistic effect on intestinal damage repair in this model. The No. 2 and No. 3 double gels showed the best intestinal damage repair effects. This invention provides a new technical solution for improving intestinal health and has promising market application prospects.

[0061] As described above, the basic principles, main features, and advantages of the present invention have been well described. The above embodiments and specifications are merely descriptions of preferred embodiments of the present invention, and the present invention is not limited to the above embodiments. Various changes and improvements made to the technical solutions of the present invention by those skilled in the art without departing from the spirit and scope of the present invention should fall within the protection scope defined by the present invention.

Claims

1. A method for preparing a dietary supplement, characterized in that, Includes the following steps: S1. Preparation of hydrogel containing galangal polysaccharide: Dissolve galangal polysaccharide in deionized water to obtain galangal polysaccharide aqueous solution; add gelatin to the galangal polysaccharide aqueous solution, heat and stir, and then cool to obtain hydrogel; S2. Preparation of oleogel containing vitamin E: Dissolve monoglycerides in olive oil to form an oil phase mixture; add vitamin E pre-dissolved in olive oil during the cooling process of the oil phase mixture, mix well and cool to obtain oleogel; S3. Preparation of dual gels: The oleogel obtained in step S2 is heated to fluidity and then mixed with the hydrogel obtained in step S1 at a volume ratio. After homogenization, it is rapidly cooled to obtain the dietary supplement.

2. The preparation method according to claim 1, characterized in that, In step S1, the mass percentage of the galangal polysaccharide in the hydrogel is 0.1% to 0.5%.

3. The preparation method according to claim 1, characterized in that, In step S1, the mass percentage of gelatin in the hydrogel is 6% to 8%.

4. The preparation method according to claim 1, characterized in that, In step S1, the heating and stirring conditions are: temperature 60~65℃, rotation speed 400~500rpm, and time 2~3h.

5. The preparation method according to claim 1, characterized in that, In step S2, the monoglyceride has a mass percentage of 8% to 10% in the oleogel.

6. The preparation method according to claim 1, characterized in that, In step S2, the percentage of vitamin E in the total mass of the dual gel is 0.5% to 2%.

7. The preparation method according to claim 1, characterized in that, In step S3, the volume ratio of the oleogel to the hydrogel is 4:6 to 6:

4.

8. The preparation method according to claim 1, characterized in that, In step S3, the homogenization conditions are: rotation speed 10000~12000 rpm, time 5~6 min.

9. The preparation method according to claim 1, characterized in that, In step S3, the rapid cooling is achieved by stirring and cooling in an ice bath at a speed of 200-300 rpm.

10. A dietary supplement, characterized in that, It is prepared by any one of claims 1 to 9.

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