Secondary embedded macleaya cordata extract microcapsule and preparation method thereof
By using sodium alginate and chitosan as wall materials in Boluohui extract microcapsules, it was solved by embedding once and then oxidizing and decomposing the Boluohui extract, and its stability and embedding rate were significantly improved.
Patent Information
- Application Number
- CN202510312926.2
- 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 the influence of external temperature, pH, light and additives and is oxidized and decomposed, resulting in low stability and solubility, limiting its clinical application.
Sodium alginate and chitosan were used as wall materials, and the first embedding was carried out by sharp hole solidification method, and then secondary embedding was carried out to form a stable Boluohui extract microcapsule.
The stability of the microcapsule easily oxidized substances is significantly improved, the release of the core material is controlled, the toxic side effect is reduced, and the embedding rate is increased to 89.85%.
Smart Images
Figure CN120093716A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of microcapsule preparation, and in particular to a secondary embedded Macleaya cordata extract microcapsule and a preparation method thereof. Background Art
[0002] The extract of Macleaya cordata is easily affected by external temperature, pH, light and some common additives and undergoes oxidative decomposition. Therefore, its low stability and low solubility limit its clinical application. In recent years, the 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 in recent years. 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, play a sustained release role, and is convenient for storage and transportation, and has a wider range of applications. The effect of secondary embedding is better than that of primary embedding. Secondary embedding can greatly improve the stability of easily oxidized substances in microcapsules, control the release of core materials, and reduce toxic and side effects. Chitosan (CS) and sodium alginate (Na-Alg) are biodegradable ionic polymers, non-toxic, with excellent biocompatibility, good film-forming and spherical properties. Some progress has been made in the preparation of edible microcapsules using them as wall materials for composite microcapsules. Summary of the invention
[0003] The purpose of the present invention is to use sodium alginate and chitosan as wall materials and Macleaya cordata extract as core material to perform secondary embedding of Macleaya cordata extract microcapsules based on primary embedding. ＋ The ionic gelation of the Macleaya cordata extract forms a calcium alginate gel, and the Macleaya cordata extract is embedded in the "egg box" structure of the calcium alginate to achieve embedding. The present invention uses alkaloids as the embedding rate, and conducts single factor analysis on the preparation process from four factors such as sodium alginate concentration, calcium chloride concentration, chitosan concentration, and stirring speed, and screens out the optimal preparation process range to obtain gel microcapsules with regular shape, uniform size, moderate hardness, and full color.
[0004] The present invention provides a method for preparing secondary embedded Macleaya cordata extract microcapsules, 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; (2) Weigh a certain amount of Macleaya cordata extract and dissolve it in anhydrous ethanol, mix the Macleaya cordata solution and the sodium alginate solution in a certain proportion, and stir until uniform; (3) adding the above solution to the calcium chloride solution and then leaving it to stand at room temperature to obtain a primary microcapsule embedding solution; (4) The microcapsules embedded once in (3) are mixed with a chitosan solution of a certain concentration for secondary embedding, the microspheres are collected and finally freeze-dried to obtain the secondary embedded Macleaya cordata extract microcapsules.
[0005] Furthermore, the concentration of sodium alginate is 0.5%, 1%, 2% or 3%.
[0006] Furthermore, the concentration of calcium chloride is 0.5%, 1%, 2% or 3%.
[0007] Furthermore, the chitosan concentration is 0.5%, 1%, 2% or 3%.
[0008] Furthermore, the stirring speed is 200 r / min, 250 r / min, 300 r / min or 350 r / min.
[0009] Furthermore, the sodium alginate concentration was 2%, the calcium chloride concentration was 2.5%, the stirring speed was 250 r / min, and the chitosan concentration was 0.5%.
[0010] Furthermore, in step (4), the microcapsules embedded once in (3) are mixed with a chitosan solution of a certain concentration for secondary embedding, and then placed on an oscillator for oscillation at 200 rpm / min for film-forming reaction for 15 minutes, rinsed with distilled water for 3 times, filtered and collected microspheres, which are microcapsules embedded twice; finally, the microspheres are pre-frozen at -20°C and dried in a freeze dryer for 24 hours to obtain microcapsules of Macleaya cordata extract embedded twice.
[0011] Furthermore, the embedding rate of the secondary embedded Macleaya cordata extract microcapsules reached up to 89.85%.
[0012] The present invention also provides a secondary embedded Macleaya cordata extract microcapsule, which is prepared by the above method.
[0013] Beneficial effects: With Macleaya cordata extract as core material, sodium alginate and chitosan as wall materials, Macleaya cordata extract microcapsules are secondary embedded by sharp hole coagulation method. Secondary embedding can greatly improve the stability of easily oxidized substances in microcapsules, control the release of core materials, and reduce toxic and side effects. The best preparation process of the microcapsules of the present invention is 2% sodium alginate concentration, 2.5% calcium chloride concentration, stirring speed 250r / min, chitosan concentration 0.5%, and the alkaloid embedding rate is 89.85%. Scanning electron microscopy observation shows that the microcapsule structure is complete, the surface is uneven and wrinkled, and the effect of secondary embedding is better than that of primary embedding. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 This is the apparent morphology of the microcapsules in the examples.
[0015] Figure 2Scanning electron micrograph of the wet microcapsules of Macleaya cordata extract prepared in Example. DETAILED DESCRIPTION
[0016] 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.
[0017] In the embodiment, sodium alginate and chitosan are used as wall materials, and the Macleaya cordata extract is used as the core material, and secondary embedding of Macleaya cordata extract microcapsules is performed on the basis of primary embedding.
[0018] 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.
[0019] 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.
[0020] 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% Secondary Encapsulation of Macleaya Cordata Extract Microcapsules by Sharp-hole Coagulation Method (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 at 50°C and stir them evenly until they are dissolved.
[0021] (2) Weigh a certain amount of Macleaya cordata extract and dissolve it in 5 M anhydrous ethanol. Mix the Macleaya cordata solution and the sodium alginate solution in a certain proportion and stir until uniform.
[0022] (3) Then, the above solution is added dropwise to the calcium chloride solution using a 10 ml syringe, and then allowed to stand at room temperature for 2 hours. This is the primary encapsulation microcapsule.
[0023] (4) The microcapsules embedded once in (3) were mixed with a chitosan solution of a certain concentration for secondary embedding, and then placed on an oscillator at 200 rpm / min for film-forming reaction for 15 minutes, rinsed with distilled water for 3 times, filtered and collected, and the microspheres were obtained as secondary embedded microcapsules. Finally, the microspheres were pre-frozen at -20°C and dried in a freeze dryer for 24 hours to obtain Macleaya cordata extract microcapsules.
[0024] Taking the embedding rate as an indicator, the effects of four factors, namely, sodium alginate concentration, calcium chloride concentration, chitosan concentration, and stirring speed, on the microcapsule embedding effect were investigated, and an orthogonal experiment was designed. 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 (34) 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), C (stirring speed) and D (chitosan concentration) on the microcapsule embedding efficiency were investigated. The results and analysis are shown in Table 2.
[0027] Table 2
[0028] When the sodium alginate concentration is 2%, the embedding rate is the highest, and then the embedding rate decreases as the sodium alginate concentration increases. When the mass fraction is lower than 2%, the polyanion groups formed by sodium alginate are relatively small, and the charge density of the sodium alginate solution is relatively low, and it cannot effectively combine with chitosan to form a film. When the mass fraction is higher than 2%, the higher mass fraction of sodium alginate will cause the solution viscosity to be too high, the prepared microcapsules are irregular in shape, and the capsule membrane strength is also relatively low, resulting in a reduced embedding rate.
[0029] With the increase of calcium chloride concentration, the embedding rate of Macleaya cordata extract microcapsules showed a trend of first increasing and then decreasing. The embedding effect was best when the calcium chloride concentration was 2%, and then the embedding rate decreased with the increase of calcium chloride concentration. ２＋ The concentration is low, the hardness of the formed microspheres is poor, the shape of the microspheres is poor, and the embedding rate is low.
[0030] With the increase of stirring speed, the embedding rate of Macleaya cordata extract microcapsules showed a trend of first rising and then falling. The embedding effect was best when the stirring speed was 250r / min. When the stirring speed increased, the frequency of friction and collision between the sodium alginate hydrogel microspheres and the rotating hardware increased, and the number of mutual extrusion and collision between the sodium alginate hydrogel microspheres also increased, so the breakage phenomenon was more obvious. The greater the breakage rate, the lower the embedding rate.
[0031] With the increase of chitosan, the microcapsule embedding rate of Macleaya cordata extract showed a downward trend.
[0032] When the chitosan concentration is 0.5%, the microcapsule embedding effect of Macleaya cordata extract is the best.
[0033] From Table 2, we can see that A 1 B 2 C 3 D 2 The embedding rate of the group was the highest, at 89.85%. D (4.50) > R C (3.42)>R A (2.93)>R B (2.17), the order of influence of each factor on the embedding rate of microcapsules is: D>C>B>A, that is, chitosan concentration> stirring speed> calcium chloride concentration> sodium alginate concentration. The best process condition combination for preparing microcapsules of Macleaya cordata extract by sharp hole coagulation method is: A 1 B 2 C 3 D 2 Therefore, the optimal process conditions for preparing Macleaya cordata extract microcapsules are: sodium alginate concentration 2%, calcium chloride concentration 2.5%, stirring speed 250r / min, chitosan concentration 0.5%, under which the microcapsule product embedding rate can reach 89.85%.
[0034] The morphology and performance of the Macleaya cordata extract microcapsules obtained in the examples were measured.
[0035] 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. Figure 1 a is a wet microcapsule of Macleaya cordata extract; Figure 1 b is the freeze-dried microcapsule; Figure 1 a. Figure 1b It can be seen that the microcapsules before and after drying are in the form of yellow spherical particles with uniform size and color, smooth surface, no adhesion, and the texture of the dried microcapsules is harder. However, due to the sudden drop in freeze-drying temperature, the particles of the dried microcapsules are smaller than those before drying.
[0036] 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.
[0037] The prepared Macleaya cordata extract wet microcapsules were tested by using an electron scanning electron microscope. Figure 2 . Figure 2 a. Figure 2 b. Figure 2 c are scanning electron micrographs of the microcapsules after freeze-drying; Figure 2 c The left side is the microcapsule embedded once, and the right side is the microcapsule embedded twice; Figure 2 a. Figure 2 b. Figure 2 c It can be seen that the prepared Macleaya cordata extract microcapsule products have complete structures, most of which are spherical, with uneven surfaces and obvious surface wrinkles. The shrinkage phenomenon after the first embedding is more serious than that after the second embedding. This may be because the shell of the microcapsule is harder and more tightly packed after the second embedding, making it difficult for water to enter the internal structure of the microcapsule, and the water loss is less, so the effect of the second embedding is better than that of the first embedding, which is also a feature of the sharp hole method microcapsule.
Claims
1. A method for preparing secondary embedded Macleaya cordata extract microcapsules, 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; (2) Weigh a certain amount of Macleaya cordata extract and dissolve it in anhydrous ethanol, mix the Macleaya cordata solution and the sodium alginate solution in a certain proportion, and stir until uniform; (3) adding the above solution to the calcium chloride solution and then leaving it to stand at room temperature to obtain a primary microcapsule embedding solution; (4) The microcapsules embedded once in (3) are mixed with a chitosan solution of a certain concentration for secondary embedding, the microspheres are collected and finally freeze-dried to obtain the secondary embedded Macleaya cordata extract microcapsules.
2. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: The concentration of sodium alginate is 0.5%, 1%, 2% or 3%.
3. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: The concentration of calcium chloride is 0.5%, 1%, 2% or 3%.
4. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: The chitosan concentration was 0.5%, 1%, 2% or 3%.
5. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: The stirring speed is 200r / min, 250r / min, 300r / min or 350r / min.
6. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: The sodium alginate concentration is 2%, the calcium chloride concentration is 2.5%, the stirring speed is 250r / min, and the chitosan concentration is 0.5%.
7. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 1, characterized in that: Step (4) The microcapsules embedded once in (3) are mixed with a chitosan solution of a certain concentration for secondary embedding, and then placed on an oscillator for oscillation at 200 rpm / min for film-forming reaction for 15 minutes, rinsed with distilled water for 3 times, filtered and collected microspheres, which are microcapsules embedded twice; finally, the microspheres are pre-frozen at -20°C and dried in a freeze dryer for 24 hours to obtain microcapsules of Macleaya cordata extract embedded twice.
8. The method for preparing a secondary embedded Macleaya cordata extract microcapsule according to claim 6, characterized in that: The embedding rate of the secondary embedded Macleaya cordata extract microcapsules reaches up to 89.85%.
9. A secondary embedded Macleaya cordata extract microcapsule prepared by the method according to any one of claims 1 to 8.