Macleaya cordata extract microcapsule and preparation method thereof
By using sodium alginate and calcium chloride to prepare Boluohui extract microcapsules, the problem of easy oxidation and decomposition of Boluohui extract is solved, and the stability and solubility of Boluohui extract is achieved, and its clinical application scope is expanded.
Patent Information
- Application Number
- CN202510312509.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2025-06-06
AI Technical Summary
Boluohui extract is susceptible to external temperature, pH, light and additives and is oxidized and decomposed, resulting in low stability and low solubility, limiting its clinical application.
Sodium alginate is used as the wall material, and by adjusting the concentration of sodium alginate, calcium chloride and core wall ratio, combined with freeze-drying method, Boluohui extract microcapsules with regular shape, uniform size and moderate elasticity are prepared.
The stability and solubility of the Boluohui extract are improved, the better biological activity sustained release effect is achieved, and its application scope is expanded, with an embedding rate up to 75.51%.
Smart Images
Figure CN120093715A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of microcapsule preparation, and in particular to a Macleaya cordata extract microcapsule and a preparation method thereof. Background Art
[0002] Macleaya cordata extract is easily affected by external temperature, pH, light and some common additives and undergoes oxidative decomposition, so its low stability and low solubility limit its clinical application. In recent years, new dosage forms of Macleaya cordata extract prepared mainly include nanoemulsions, microcapsules, solid dispersions and liposomes, among which the preparation of microcapsules has become a hot topic of research in recent years. At present, the methods for preparing Macleaya cordata extract microcapsules include sharp hole method, complex coacervation method, molecular embedding method, spray drying method, etc. The use of microcapsule embedding technology to prepare Macleaya cordata extract into microcapsule form can protect the Macleaya cordata extract to better exert its biological activity and play a sustained release role, and it is convenient for storage and transportation, and has a wider range of applications. Summary of the invention
[0003] The invention aims to prepare Macleaya cordata extract microcapsules with regular shape, uniform size and moderate elasticity by using Macleaya cordata extract as core material and sodium alginate as wall material, by adjusting appropriate sodium alginate concentration, calcium chloride concentration and core-to-wall ratio and adopting freeze-drying conditions.
[0004] The present invention provides a method for preparing microcapsules of Macleaya cordata extract, comprising the following steps: (1) Weigh a certain amount of sodium alginate and calcium chloride respectively and dissolve them in distilled water to make a solution of a certain concentration of sodium alginate and calcium chloride, and then place them in a digital magnetic stirrer at 50°C and stir them evenly until they are dissolved; (2) weighing a Macleaya cordata extract and dissolving it in anhydrous ethanol, mixing the Macleaya cordata solution with the sodium alginate solution in a certain mass ratio, i.e., the core-to-wall ratio, and stirring until uniform; (3) Add the above solution dropwise into the calcium chloride solution using a syringe, and then let it stand at room temperature for 2 hours; (4) washing with distilled water, filtering and collecting the microspheres, i.e., the primary embedded microcapsules, and finally freeze-drying to obtain the Macleaya cordata extract microcapsules.
[0005] Furthermore, in step (1), the concentration of sodium alginate is 0.5%, 1%, 2%, 2.5% or 3%.
[0006] Furthermore, in step (1), the concentration of calcium chloride is 0.5%, 1%, 2%, 2.5% or 3%.
[0007] Furthermore, in step (2), the core-to-wall ratio is 1:1, 1:1.5, 1:2, 2:1 or 1:3.
[0008] Furthermore, the sodium alginate concentration is 2%, the calcium chloride concentration is 2.5%, and the core-to-wall ratio is 1:1.5.
[0009] Furthermore, in step (4), the mixture was rinsed with distilled water for three times, and the freeze-drying conditions were: pre-freezing at -20°C and drying in a freeze dryer for 24 hours.
[0010] Furthermore, the embedding rate of the microcapsules obtained by the method can reach up to 75.51%.
[0011] The invention also provides a Macleaya cordata extract microcapsule, which is prepared by the above method.
[0012] Beneficial effects: The present invention prepares microcapsules of Macleaya cordata extract by ion gelation of sodium alginate and calcium chloride. Experiments have confirmed that the sodium alginate concentration mainly determines the shape of the microcapsules, the calcium chloride concentration mainly affects the hardness and taste of the microcapsules, and the core-to-wall ratio mainly affects the loading amount of the microcapsules. When the sodium alginate concentration is 2%, the calcium chloride concentration is 2.5%, and the core-to-wall ratio is 1:1.5, the embedding rate is the highest, which is 75.51%. At the same time, freeze drying is adopted to finally obtain microcapsules with regular shape, uniform size and moderate elasticity. BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Figure 1 This is the apparent morphology of the Macleaya cordata extract microcapsules of the example.
[0014] Figure 2 Scanning electron micrograph of the wet microcapsules of Macleaya cordata extract prepared in Example. DETAILED DESCRIPTION
[0015] The sodium alginate and calcium chloride used in the examples were purchased from Shanghai Maclean Biochemical Technology Co., Ltd.; the Maclean extract was purchased from Meikeda Biological Company; and anhydrous ethanol was purchased from Shandong Keyuan Biochemical Co., Ltd. Digital magnetic stirrer, oscillator, and electronic balance were purchased from Zhengzhou Huate Instrument Equipment Co., Ltd.; 10 ml syringe: commercially available; pH meter was purchased from Mettler-Toledo Instrument (Shanghai) Co., Ltd.; freeze dryer was purchased from SIM, USA; UV spectrophotometer was purchased from Shanghai Yiheng Scientific Instrument Co., Ltd.; scanning electron microscope was purchased from Hitachi, Japan.
[0016] The embodiment of the present invention uses Macleaya cordata extract as core material and sodium alginate as wall material, and prepares Macleaya cordata extract microcapsules with regular shape, uniform size and moderate elasticity by adjusting appropriate sodium alginate concentration, calcium chloride concentration and core-to-wall ratio.
[0017] The embedding rate refers to the mass percentage of the embedded core material to the total core material added during the reaction. It is an important parameter to measure the embedding capacity of the wall material. Theoretically, the higher the embedding rate, the better the embedding effect. Therefore, this experiment screened the best preparation process by calculating the embedding rate.
[0018] Embedding efficiency determination method Surface alkaloid content: Weigh 0.5 g of wet Macleaya cordata extract microcapsules, add 10 mL of anhydrous ethanol, vortex oscillate for 1 min, then centrifuge at 3000 r / min for 5 min to remove the supernatant, filter through a 0.22 μm organic filter membrane, and measure the absorbance at 415 nm; calculate the alkaloid content on the surface of the microcapsules.
[0019] Total alkaloid content: Weigh 0.5g of wet Macheulandia extract microcapsules, add 10mL of anhydrous ethanol, ultrasonicate for 20min at 40°C and 100w, centrifuge at 3000r / min for 5min, filter through a 0.22μm organic filter membrane, and measure the absorbance at 415nm; calculate the total alkaloid content in the microcapsules. Calculation formula: Encapsulation rate = [1-surface alkaloid content ÷ total alkaloid content] × 100% 1. Microencapsulation method of Macleaya cordata extract Example
[0020] (1) Weigh a certain amount of sodium alginate and calcium chloride respectively and dissolve them in distilled water to make a solution of a certain concentration of sodium alginate and calcium chloride. Then place them in a digital magnetic stirrer and stir them evenly at 50°C until they are dissolved.
[0021] (2) Weigh the Macleaya cordata extract and dissolve it in anhydrous ethanol, mix the Macleaya cordata solution with the sodium alginate solution in a certain mass ratio, i.e., the core-to-wall ratio, and stir until uniform.
[0022] (3) The above solution was then added dropwise to the calcium chloride solution using a syringe, and then allowed to stand at room temperature for 2 hours.
[0023] (4) Rinse with distilled water for 3 times, filter and collect the microspheres, which are the primary embedded microcapsules. Finally, pre-freeze the microspheres at -20°C and dry them in a freeze dryer for 24 hours to obtain the Macleaya cordata extract microcapsules.
[0024] Taking the embedding rate as an indicator, the three factors of sodium alginate concentration, calcium chloride concentration and core-to-wall ratio were investigated. An orthogonal experiment was designed to study the effect of microcapsule embedding. The factors and levels of the orthogonal experiment are shown in Table 1.
[0025] Table 1
[0026] On the basis of the single factor test results, the L9 (33) orthogonal test was used to further optimize the microencapsulation process of Macleaya cordata extract. The effects of A (sodium alginate concentration), B (calcium chloride concentration) and C (core-to-wall ratio) on the microcapsule embedding efficiency were investigated. The results and analysis are shown in Table 2.
[0027] Table 2 Orthogonal test results
[0028] With the increase of sodium alginate concentration, the embedding rate of Macleaya cordata extract microcapsules showed a trend of first increasing and then decreasing. When the sodium alginate concentration was 2%, the embedding rate was the highest, and then the embedding rate decreased with the increase of sodium alginate concentration. When the sodium alginate concentration was greater than 2%, the viscosity of the solution system was too high, the resistance and adhesion of the solution to dripping increased, and large gels were easily formed, which was not conducive to the microspheres. Formation, thus affecting the embedding effect of microspheres.
[0029] With the increase of calcium chloride concentration, the embedding rate of Macleaya cordata extract microcapsules showed a trend of first rising and then falling, but the trend was not obvious. When the calcium chloride concentration was low, the shell of the microcapsules was relatively soft, so it was easy to break with the stirring of the rotor during the preparation process, resulting in a low embedding rate; when the mass fraction of calcium chloride increased to 2%, the embedding rate of the microcapsules reached the best matching state, and continued to increase its mass fraction, the probability of contact between the wall materials increased, the probability of contact between the core material and the wall material became relatively small, the adhesion performance decreased, and the embedding rate decreased.
[0030] With the increase of core-to-wall ratio, the embedding efficiency of Macleaya cordata extract microcapsules first increased and then decreased. The embedding effect is most obvious when the core-to-wall ratio is 1:2.
[0031] From Table 2, we can see that A 1 B 2 C 2 The embedding rate of the group was the highest, at 75.51%. C (2.64) > R A (2.19)>R B (0.94), the order of influence of each factor on the embedding rate of microcapsules is: C>A>B, that is, core-to-wall ratio>sodium alginate concentration>calcium chloride concentration>. The best process condition combination for preparing microcapsules of Macleaya cordata extract by sharp hole coagulation method is: A 1 B 2 C 2 Therefore, the optimal process conditions for preparing Macleaya cordata extract microcapsules are: sodium alginate mass fraction 2%, calcium chloride concentration 2.5%, core-to-wall ratio 1:1.5. Under these conditions, the embedding rate of the microcapsule product can reach 75.51%.
[0032] The morphology and performance of the Macleaya cordata extract microcapsules obtained in the examples were measured.
[0033] Surface morphology of microcapsules The particle size of the microcapsule is determined by the size of the added droplet. In this experiment, a 10mL syringe needle was used for droplet addition. The resulting wet capsules were relatively large, and the surface morphology could be directly observed and photographed. Figure 1 This is the apparent morphology of the microcapsules in the examples.
[0034] Figure 1 a is a wet microcapsule of Macleaya cordata extract; Figure 1 b is the freeze-dried microcapsule; Figure 1 c is the baked microcapsule. Figure 1 b It can be seen that the freeze-dried microcapsules are in the form of yellow spherical particles with uniform size and color, a smooth surface, no adhesion, and a hard texture. Figure 1 c is Figure 1 The microcapsule particles dried at 40°C based on the wet microcapsules prepared in a are brown in shape with different sizes and an uneven surface after drying, but the texture is harder than that of the freeze-dried microcapsules. This is because the microcapsules are subjected to heat due to baking, resulting in surface ruptures.
[0035] Scanning electron microscope (SEM) observation The microcapsule particles prepared in the example were glued to the SEM sample stage with double-sided conductive adhesive, and their external structure was observed with a scanning electron microscope after the surface was treated with gold spraying. The voltage acceleration was 20 kV.
[0036] The prepared Macleaya cordata extract wet microcapsules were tested by using an electron scanning electron microscope. Figure 2 , Figure 2 a. Figure 2 b is a scanning electron microscopic image of freeze-dried microcapsules in Example; Figure 2 c is a scanning electron microscope image of the microcapsules after baking in the embodiment. Figure 2 a. Figure 2 As shown in Figure b, the structure of the prepared Macleaya extract microcapsule product is complete, most of them are spherical, with an uneven surface and obvious surface wrinkles. The microcapsules in Figure c are severely shrunken after high-temperature drying, which is due to the external heat. Scanning electron microscopy observation showed that the freeze-dried microcapsules had a complete structure, an uneven surface, and wrinkles. The surface of the baked microcapsules was severely shrunken. Therefore, the freeze-drying method used in this application is better for drying microcapsules.
[0037] This application mainly prepares Macleaya cordata extract microcapsules by ion gelation of sodium alginate and calcium chloride. The effects of sodium alginate concentration, calcium chloride concentration and core-wall ratio on the appearance of microcapsules were investigated. The microcapsules with regular morphology, uniform size and moderate elasticity were obtained as indicators. The optimal preparation process conditions were screened by single-factor experiments. It was confirmed that the sodium alginate concentration mainly determines the appearance of microcapsules, the calcium chloride concentration mainly affects the hardness and taste of microcapsules, and the core-wall ratio mainly affects the loading amount of microcapsules. On the basis of the single-factor experiment, the sodium alginate concentration, calcium chloride concentration and core-wall ratio were orthogonally tested with three factors and three levels with the embedding rate as an indicator, and the optimal process conditions were obtained. When the sodium alginate concentration was 2%, the calcium chloride concentration was 2.5%, and the core-wall ratio was 1:1.5, the embedding rate was the highest, which was 75.51%, and the core-wall ratio, sodium alginate concentration and calcium chloride concentration increased in turn. The freeze-dried microcapsules were observed to have a complete structure, an uneven surface and wrinkles by scanning electron microscopy. The surface of the microcapsules shrank severely after baking. Therefore, the freeze-drying method was used to dry the microcapsules in this experiment, which had a better effect. At the same time, the preparation of microcapsules of Macleaya cordata extract provides a reference for the further development and utilization of Macleaya cordata alkaloids.
Claims
1. A method for preparing microcapsules of Macleaya cordata extract, characterized in that: The following steps are involved: (1) Weigh a certain amount of sodium alginate and calcium chloride respectively and dissolve them in distilled water to make a solution of a certain concentration of sodium alginate and calcium chloride, and stir them evenly until they are dissolved; (2) weighing a Macleaya cordata extract and dissolving it in anhydrous ethanol, mixing the Macleaya cordata solution with the sodium alginate solution in a certain mass ratio, i.e., the core-to-wall ratio, and stirring until uniform; (3) adding the above solution to the calcium chloride solution and then allowing to stand at room temperature; (4) washing with distilled water, filtering and collecting the microspheres, i.e., the primary embedded microcapsules, and finally freeze-drying to obtain the Macleaya cordata extract microcapsules.
2. The method for preparing a Macleaya cordata extract microcapsule according to claim 1, characterized in that: In step (1), the concentration of sodium alginate is 0.5%, 1%, 2%, 2.5% or 3%.
3. The method for preparing a Macleaya cordata extract microcapsule according to claim 1, characterized in that: In step (1), the concentration of calcium chloride is 0.5%, 1%, 2%, 2.5% or 3%.
4. The method for preparing a Macleaya cordata extract microcapsule according to claim 1, characterized in that: In step (2), the core-to-wall ratio is 1:1, 1:1.5, 1:2, 2:1 or 1:
3.
5. The method for preparing a Macleaya cordata extract microcapsule according to claim 1, characterized in that: The sodium alginate concentration was 2%, the calcium chloride concentration was 2.5%, and the core-to-wall ratio was 1:1.
5.
6. The method for preparing a Macleaya cordata extract microcapsule according to claim 1, characterized in that: In step (4), rinse with distilled water three times, and freeze-drying conditions are: pre-freeze at -20°C and dry in a freeze dryer for 24 hours.
7. The method for preparing a Macleaya cordata extract microcapsule according to claim 5, characterized in that: The embedding rate of the microcapsules obtained by the method can reach up to 75.51%.
8. A Macleaya cordata extract microcapsule prepared by the method according to any one of claims 1 to 7.