Targeted release health-care oil emulsion in colon and preparation method of targeted release health-care oil emulsion

Abstract

The invention relates to a targeted release health-care oil emulsion in colon and a preparation method thereof, and belongs to the technical field of sex component embedding and targeted release, and the targeted release health-care oil emulsion in colon comprises the following components by mass: 70-95 parts of a pectin aqueous solution; and 5-30 parts of health-care oil. The preparation method comprises the following steps: S1, preparing a pectin aqueous solution with the mass concentration of 0.5-3% for later use; s2, adjusting the pH value of the pectin aqueous solution prepared in the step S1 to 2, and then putting the pectin aqueous solution in a refrigerator overnight; s3, taking out the pectin aqueous solution overnight in the step S2, adding the health-care oil into the pectin aqueous solution, and stirring at a high speed by using an ultra-high-speed stirrer; and S4, adding the crude emulsion prepared in the step S3 into a high-pressure homogenizer to prepare the targeted release health-care oil emulsion in the colon. The digestion degree of the health-care oil emulsion in small intestines can be effectively reduced, and the active ingredients in the health-care oil emulsion are improved, so that the health-care oil emulsion is released in a targeted manner at the colon part.

Description

Technical Field

[0001] The invention belongs to the technical field of sexual component embedding and targeted release, and specifically relates to a health-care oil emulsion with targeted release in the colon and a preparation method thereof. Background Art

[0002] Health oil refers to a type of plant oil or animal oil with health benefits. In addition to being rich in unsaturated fatty acids, vitamins, and minerals, health oil also contains a variety of active ingredients and has multiple physiological functions such as antioxidant, anti-inflammatory, and anti-tumor. For example, sea buckthorn oil is rich in vitamin C and vitamin E, and has antioxidant effects. After being consumed, it can play an antioxidant and anti-inflammatory role in the digestive tract, especially helping to relieve colon inflammation. During the digestion process, most of the health oil will be digested and absorbed by the small intestine, which greatly reduces its distribution and physiological activity in the colon. Using a delivery system to target the health oil to the colon can increase its concentration in the colon, exerting local anti-inflammatory effects, promoting repair, and maintaining intestinal health.

[0003] Emulsion encapsulation technology is widely used in the delivery of health oils. By regulating the interface structure and interface digestibility of the emulsion, the controlled release of health oils in the colon can be achieved. Natural pectin is a natural dietary fiber emulsifier with good emulsifying properties. While it remains intact in the upper digestive tract, it is not degraded by digestive enzymes. Therefore, it becomes an ideal raw material for constructing health oil emulsions for targeted small intestine delivery. Some studies use a layer-by-layer assembly method to adsorb pectin on the formed emulsion interface to form a multi-layer protective layer to improve the release effect of the emulsion in the colon; other studies chemically modify pectin to increase its degree of esterification to enhance the release effect of its emulsion in the colon. However, these current technical methods are too complicated and require cumbersome production processes, which increases manufacturing costs and is not conducive to commercial applications.

[0004] In summary, further research and optimization are still needed to develop simpler and more effective methods to construct pectin-stabilized health oil emulsions and target the delivery of health oil in the colon. Summary of the invention

[0005] The main purpose of the present invention is to overcome the deficiencies in the prior art. The present invention provides a health-care oil emulsion with targeted release in the colon and a preparation method thereof, which can simply and effectively construct a health-care oil emulsion with targeted release in the colon and realize the targeted delivery of active ingredients in the health-care oil in the colon.

[0006] In order to achieve the above-mentioned invention object, the present invention provides the following technical solution: a health-care oil emulsion for targeted release in the colon, the composition and mass fraction thereof are: Pectin aqueous solution, 70~95 parts; the mass concentration of pectin aqueous solution is 0.5%~3%; Health care oil, 5-30 parts; the health care oil is one or more of sea buckthorn oil, grape seed oil, camellia oil, millet bran oil, oat oil or linseed oil.

[0007] The reasons why the pectin aqueous solution with a mass concentration of 0.5% to 3% (especially 2% to 3%) stabilizes the sea buckthorn oil emulsion to release active ingredients in the colon: first, the interfacial adsorption layer formed by the pectin aqueous solution with a mass concentration of 0.5% to 3% (especially 2% to 3%) can resist bile salt substitution; second, the interfacial adsorption layer formed by the pectin aqueous solution with a mass concentration of 0.5% to 3% (especially 2% to 3%) can directly inhibit lipase digestion. The two effects synergistically inhibit emulsion digestion, so that the prepared sea buckthorn oil emulsion has the ability to release active ingredients in the colon.

[0008] A method for preparing the colon targeted release health oil emulsion as described above, characterized in that it comprises the following steps: S1. Add pectin powder to pure water and stir at a temperature of 20°C to 30°C, a stirring speed of 100 rpm to 300 rpm, and a stirring time of 6h to 12h. After stirring evenly, prepare a pectin aqueous solution with a mass concentration of 0.5% to 3% for standby use; S2, adjusting the pH value of the pectin aqueous solution prepared in step S1 to 2. When the pH value of the pectin solution is 2, the pectin has the strongest ability to reduce the oil-water interfacial tension, and the particle size constructed at this time is the smallest; then placing in a refrigerator at 4° C. and refrigerating overnight to allow the pectin aqueous solution to fully undergo a hydration reaction; S3, take out the pectin aqueous solution after step S2 overnight, weigh the raw materials according to the mass fractions of the pectin aqueous solution and the health oil, add the health oil to the pectin aqueous solution, use an ultra-high speed stirrer to stir at high speed, the stirring speed is 1000 rpm, the stirring time is 3min, and a crude emulsion is obtained; S4, high-pressure homogenization: Add the crude emulsion prepared in step S3 into a high-pressure homogenizer, set the pressure to 600 bar, and repeat at least three times to obtain a health-care oil emulsion with targeted release in the colon.

[0009] Compared with the prior art, the present invention has the following beneficial effects: The present invention can reduce the particle size of the emulsion and improve the stability of the emulsion by simply adjusting the pH value of the system (pH=2) and the concentration of the pectin aqueous solution (2%~3%). More importantly, this method can effectively reduce the digestion degree of the health oil emulsion in the small intestine, increase the active ingredients in the health oil emulsion, and then release them in a targeted manner in the colon. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 This is a comparison diagram of the interfacial tension curves of pectin aqueous solution and seabuckthorn oil under different pH conditions in Example 1; Figure 2 This is a comparison diagram of the average particle size of the pectin-stabilized seabuckthorn oil emulsion under different pH conditions in Example 1; Figure 3 This is a comparison diagram of particle size and potential of sea buckthorn oil emulsions stabilized by pectin aqueous solutions of different mass concentrations in Example 2; Figure 4 Comparative photos of the appearance changes of seabuckthorn oil emulsions stabilized by pectin aqueous solutions of different mass concentrations during storage at 4° C. in Example 2; Figure 5 This is a comparison diagram of the particle size changes of sea buckthorn oil emulsions stabilized by pectin aqueous solutions of different mass concentrations during storage at 4°C in Example 2; Figure 6 This is a comparison diagram of the microstructure of sea buckthorn oil emulsion stabilized by pectin aqueous solutions of different mass concentrations before and after small intestine digestion in Example 2; Figure 7 is a comparison chart of fatty acid release rates during in vitro simulated digestion of seabuckthorn oil emulsions stabilized by pectin aqueous solutions of different mass concentrations in Example 2; Figure 8 This is a comparative diagram of the bioavailability of β-carotene (Figure A) and α-tocopherol (Figure B) during the simulated in vitro digestion of seabuckthorn oil emulsions stabilized by pectin aqueous solutions of different mass concentrations in Example 2; Fig. 9 This is a comparison chart of the pectin adsorption per unit area on the interface of the health oil emulsion after in vitro simulated digestion; Fig.10 This is a comparison chart of fatty acid release rates of different health oil emulsions in the presence of lipase alone. DETAILED DESCRIPTION

[0011] The present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. Example 1

[0012] A method for preparing a health-care oil emulsion for targeted release in the colon, characterized in that it comprises the following steps: S1. Add 1 g of pectin powder to 99 g of pure water and stir at a temperature of 25 ° C., a stirring speed of 300 rpm, and a stirring time of 12 h. After stirring evenly, a pectin aqueous solution with a mass concentration of 1% is prepared for standby use; S2, using hydrochloric acid, citric acid, malic acid, ascorbic acid or phosphoric acid to adjust the pH values ​​of the pectin aqueous solution prepared in step S1 to 1, 2, 3, 4, 5, 6, 7 respectively, and then placing the seven groups of pectin aqueous solutions in a refrigerator at 4° C. overnight to allow the pectin aqueous solution to fully undergo hydration reaction; S3, taking out 7 groups of pectin aqueous solutions after overnight storage in step S2, and weighing 90 g of each, then adding 10 g of sea buckthorn oil to each group of pectin aqueous solutions, using an ultra-high speed stirrer to stir at a high speed of 1000 rpm for 3 min to obtain a crude emulsion; S4, high-pressure homogenization: the crude emulsion prepared in step S3 is added into a high-pressure homogenizer, the pressure is set to 600 bar, and the process is repeated at least three times to obtain 7 groups of health-care oil emulsions with targeted release in the colon.

[0013] The interfacial tensions of pectin aqueous solution and seabuckthorn oil under 7 different pH conditions in Example 1 are as follows: Figure 1 As shown in the figure, it can be seen that when pH = 2, pectin has the strongest ability to reduce the oil-water interfacial tension, the interfacial tension between the pectin aqueous solution and the oil phase is the lowest, and the particle size of the sea buckthorn oil emulsion stabilized by pectin is the smallest (see Appendix Figure 2 ). Example 2

[0014] A method for preparing a health-care oil emulsion for targeted release in the colon, characterized in that it comprises the following steps: S1, adding pectin powder to pure water and stirring, the stirring temperature is 25 ° C, the stirring speed is 300 rpm, the stirring time is 12 h, and after stirring evenly, 4 groups of pectin aqueous solutions with mass concentrations of 0.5%, 1%, 2% and 3% are prepared for standby use; S2, using hydrochloric acid, citric acid, malic acid, ascorbic acid or phosphoric acid to adjust the pH of the four groups of pectin aqueous solutions prepared in step S1 to 2, and then placing the four groups of pectin aqueous solutions in a refrigerator at 4° C. overnight to allow the pectin aqueous solutions to fully undergo hydration reaction; S3, taking out 7 groups of pectin aqueous solutions after overnight storage in step S2, and weighing 90 g of each, then adding 10 g of sea buckthorn oil to each group of pectin aqueous solutions, using an ultra-high speed stirrer to stir at a high speed of 1000 rpm for 3 min to obtain a crude emulsion; S4, high-pressure homogenization: the crude emulsion prepared in step S3 is added into a high-pressure homogenizer, the pressure is set to 600 bar, and the process is repeated at least three times to obtain 4 groups of health-care oil emulsions with targeted release in the colon.

[0015] The particle sizes of the four groups of pectin aqueous solutions with different mass concentrations stabilized with seabuckthorn oil emulsions prepared in Example 2 and the changes in appearance and particle size during storage are shown in Figure 2. Figures 3-5As shown, it can be seen that when the concentration of the pectin aqueous solution is 0.5% and 1%, the particle size of the emulsion is larger. After storage at 4°C for 7 weeks, the emulsion shows certain oil separation and stratification, which leads to changes in the emulsion particle size and the emulsion is unstable. When the concentration of the pectin aqueous solution is 2% and 3%, the seabuckthorn oil emulsion particle size is smaller (below 1000 nm). After storage for 7 weeks, the emulsion does not stratify, and the seabuckthorn oil emulsion particle size remains basically unchanged. The health oil emulsion has a high stability.

[0016] It can be seen from Example 1 and Example 2 that the health oil emulsion with targeted release in the colon prepared under the conditions of 2% mass concentration of pectin aqueous solution in step S1 and pH=2 in step S2 has the best performance, and a verification test is carried out as follows.

[0017] 1. Emulsion digestion conditions: After the health oil emulsion and simulated saliva are mixed in proportion, the pH of the system is adjusted to 7, and the mixture is stirred at 200 rpm in a 37-degree water bath for 5 minutes to simulate oral digestion; the digestion product is further mixed with simulated gastric juice in a volume ratio of 2:1, the pH is adjusted to 2, and the mixture is stirred at 100 rpm in a 37-degree water bath for 1 hour to simulate gastric digestion; the digestion product is placed in a beaker, the pH is adjusted to 7, bile salts, calcium chloride, lipase and protease are added, and the mixture is reacted in a 37-degree constant temperature water bath for 2 hours to simulate the small intestinal digestion process, and a constant pH automatic titrator is used for titration to maintain the digestive fluid at pH = 7.

[0018] 2. Test indicators: microstructure of the emulsion before and after digestion, fatty acid release rate of the emulsion during small intestinal digestion, and bioaccessibility of β-carotene and tocopherol.

[0019] 3. Digestion test results When the mass concentration of pectin aqueous solution was 0.5% and 1%, the particle size of the emulsion droplets of pectin-stabilized seabuckthorn oil was significantly reduced after digestion in the small intestine, while when the mass concentration of pectin aqueous solution was 2% and 3%, the particle size of the emulsion did not change significantly after digestion in the small intestine (e.g. Figure 6 As shown in Figure 2 ); Moreover, as the mass concentration of pectin aqueous solution increases, the fatty acid release rate of seabuckthorn oil emulsion and the bioavailability of active ingredients gradually decrease. When the mass concentration of pectin aqueous solution is 3%, the fatty acid release rate of the emulsion after digestion is only about 30% (as shown in Figure 2 ). Figure 7 As shown in Figure 2), only less than 20% of β-carotene and tocopherol were released (as shown in Figure 2). Figure 8 as shown).

[0020] The above results show that when the mass concentration of pectin aqueous solution increases to 2%~3%, the prepared sea buckthorn oil emulsion shows a lower digestion and release rate during in vitro small intestinal digestion, and has the effect of targeted colon release of active ingredients.

[0021] The changes in the amount of pectin adsorbed per unit area on the emulsion interface before and after digestion were detected. Fig. 9 It can be seen that when the mass concentration of pectin aqueous solution is 0.5% and 1%, the amount of pectin adsorbed on the emulsion interface is low, and the amount of pectin adsorbed will further decrease after emulsion digestion; as the pectin concentration increases, the amount of pectin adsorbed per unit area on the emulsion interface gradually increases. When the mass concentration of pectin aqueous solution increases to 2% and 3%, the pectin adsorption on the interface remains basically unchanged after emulsion digestion.

[0022] The above results show that when the mass concentration of the pectin aqueous solution increases to 2%~3%, the amount of pectin adsorbed on the emulsion interface is large, and it can resist the replacement of bile salts during digestion. In addition, the digestion of the emulsion in the presence of lipase only (without bile salts) was tested. It can be seen that when the mass concentration of the pectin aqueous solution increases to 2%~3%, the release rate of fatty acids is low, indicating that high concentrations of pectin can inhibit the digestion of lipase.

[0023] In summary, under pH 2 conditions, when the mass concentration of pectin aqueous solution increases to 2%~3%, the pectin on the interface of seabuckthorn oil emulsion can directly inhibit lipase digestion on the one hand, and resist bile salt substitution on the other hand, which ultimately makes the prepared seabuckthorn oil emulsion show a lower digestibility during in vitro small intestinal digestion, reduces the digestion and absorption of the active ingredients by the small intestine, and has the effect of targeted colon release of active ingredients.

[0024] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed by the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention shall be based on the protection scope of the claims.

Claims

1. A health-care oil emulsion for targeted release in the colon, characterized in that: The composition and mass fraction of the health-care oil emulsion for targeted release in the colon are as follows: Pectin aqueous solution, 70~95 parts; the mass concentration of pectin aqueous solution is 0.5%~3%; Health care oil, 5-30 parts; the health care oil is one or more of sea buckthorn oil, grape seed oil, camellia oil, millet bran oil, oat oil or linseed oil.

2. A method for preparing the colon targeted release health oil emulsion as claimed in claim 1, characterized in that: The following steps are involved: S1. Add pectin powder to pure water and stir at a temperature of 20°C to 30°C, a stirring speed of 100 rpm to 300 rpm, and a stirring time of 6h to 12h. After stirring evenly, prepare a pectin aqueous solution with a mass concentration of 0.5% to 3% for standby use; S2, adjusting the pH value of the pectin aqueous solution prepared in step S1 to 2, and then placing it in a refrigerator at 4° C. and refrigerating it overnight to allow the pectin aqueous solution to fully undergo a hydration reaction; S3, take out the pectin aqueous solution after step S2 overnight, weigh the raw materials according to the mass fractions of the pectin aqueous solution and the health oil, add the health oil to the pectin aqueous solution, use an ultra-high speed stirrer to stir at high speed, the stirring speed is 1000 rpm, the stirring time is 3min, and a crude emulsion is obtained; S4, high-pressure homogenization: Add the crude emulsion prepared in step S3 into a high-pressure homogenizer, set the pressure to 600 bar, and repeat at least three times to obtain a health-care oil emulsion with targeted release in the colon.

Images