Anti-aging and sleep-aiding multifunctional preparation and preparation method thereof

Abstract

The invention provides an anti-aging and sleep-aiding multifunctional preparation and a preparation method thereof.The anti-aging and sleep-aiding multifunctional preparation is added with modified calcium carbonate and a film coating material, and the modified calcium carbonate is obtained by aminating porous calcium carbonate; the film coating material is prepared from the following raw materials in parts by mass through reaction: 3 to 5 parts of acrylic acid, 1 to 2 parts of acrylic ester, 0.1 to 0.2 part of trihydroxypropane trimethacrylate, 0.01 to 0.1 part of an emulsifier and 0.01 to 1 part of an initiator. Amino groups are introduced to the surface of modified calcium carbonate, carboxyl groups are introduced into a film coating material, and the film coating material is tightly coated on the surface of a preparation through mutual combination of charge neutralization effects of the amino groups and the carboxyl groups and a three-dimensional network structure formed by a polymer. The preparation is good in sealing performance, coating performance and stability after being stored for a long time, does not leak materials, and can be dissolved in a gastric acid environment of a human body, so that contents are uniformly and quickly released.

Description

Technical Field

[0001] The present invention relates to the technical field of anti-aging and sleep-aiding preparations, and in particular to a multifunctional anti-aging and sleep-aiding preparation and a preparation method thereof. Background Art

[0002] With the increasing global aging population and rising health awareness, the market for sleep and anti-aging products is growing rapidly. The demand for sleep-aiding, calming, and anti-aging products from a large number of people with sleep disorders and beauty consumers is driving product diversification. Oral tablets, beverages, and inhaled formulations are currently the mainstream forms of sleep and anti-aging products. Products that combine sleep-aiding and anti-aging ingredients with skincare products are also a hot topic of research.

[0003] Existing technologies such as CN109200176A, an anti-aging sleep-aiding wine, CN119385982A, a non-addictive anti-aging sleep-aiding preparation and its preparation method, CN119699589A, a composition containing ergothioneine with sleep-aiding, whitening, anti-aging and anti-inflammatory effects and its application, etc. all use a variety of different substances with sleep-aiding and anti-aging functions to compound, and are applied to beverages, food and other fields, and have achieved certain sleep-aiding and anti-aging effects.

[0004] However, active ingredients such as plant extracts are easily affected by light, heat, oxygen and humidity, and may be degraded or inactivated. Their effects are significantly reduced after long-term storage. To improve stability, the industry often uses microencapsulation technology, using cyclodextrin, liposomes, chitosan and other wall materials to encapsulate active ingredients and isolate them from the external environment. However, this protection mechanism may delay the release of active ingredients, resulting in the product not being able to take effect and be absorbed in time, and is not suitable for anti-aging and sleep-aiding preparations. In addition, most coating technologies still have shortcomings such as unsatisfactory effects, complex processes and high costs, and still need to be further optimized to meet the market demand for efficient and stable sleep-aiding and anti-aging products.

[0005] In summary, a new technical solution is urgently needed to solve the problems existing in the existing technology. Summary of the Invention

[0006] Based on this, the present invention provides a multifunctional anti-aging and sleep-aiding preparation and its preparation method. The present invention introduces amino groups onto the surface of modified calcium carbonate and carboxyl groups into a film coating material. Through the charge neutralization of the amino and carboxyl groups, combined with the three-dimensional network structure formed by the polymer, the film coating material is tightly coated on the surface of the preparation. The preparation of the present invention exhibits excellent sealing, coating, and stability after long-term storage without leakage, and dissolves in the human stomach acid environment, allowing the contents to be released evenly and quickly.

[0007] One object of the present invention is to provide a multifunctional anti-aging and sleep-aiding preparation, which comprises the following components in parts by mass:

[0008]

[0009]

[0010] The modified calcium carbonate is porous calcium carbonate that has been aminated;

[0011] The film coating material is prepared by reacting the following raw materials in parts by mass:

[0012]

[0013] Furthermore, the acrylic acid ester is selected from one or more of methyl methacrylate, ethyl methacrylate or n-butyl acrylate.

[0014] Furthermore, the emulsifier is selected from one or more of sodium lauryl sulfate, octylphenol polyoxyethylene ether-10, sorbitan monolaurate, and polyoxyethylene sorbitan monooleate.

[0015] Furthermore, the initiator is potassium persulfate.

[0016] Another object of the present invention is to provide a method for preparing the above-mentioned multifunctional anti-aging and sleep-aiding preparation, comprising the following steps:

[0017] S1. Blending calcium acetate and ammonium carbonate, stirring and reacting to obtain porous calcium carbonate; blending the porous calcium carbonate with triethanolamine, heating and reacting to obtain modified calcium carbonate;

[0018] S2, blending the emulsifier and water, stirring and mixing, then adding acrylic acid, acrylate and trihydroxypropane trimethacrylate, heating and stirring to obtain a pre-emulsion;

[0019] S3. Under the protection of inert gas, the pre-emulsion and the initiator are mixed, heated and stirred to react, to obtain a film coating material emulsion;

[0020] S4. Evenly blend the components other than the film coating material, press into plain tablets, and then coat with the film coating material emulsion to coat the surface of the plain tablets with the film coating material. After drying, obtain the anti-aging and sleep-aiding multifunctional preparation.

[0021] Furthermore, in step S1, the molar ratio of calcium acetate to ammonium carbonate is 1:(0.5-1.5).

[0022] Furthermore, in step S1, the mass ratio of the porous calcium carbonate to triethanolamine is 1:(10-15).

[0023] Furthermore, in step S1, the heating temperature is 70-90°C.

[0024] Furthermore, in step S2, the heating temperature is 40-60°C.

[0025] Furthermore, in step S3, the heating temperature is 70-90°C.

[0026] The present invention has the following beneficial effects:

[0027] The present invention first produces porous calcium carbonate by co-mixing calcium acetate and ammonium carbonate. This is then co-mixed with triethanolamine under heating to introduce amino groups onto the surface of the porous calcium carbonate, forming a modified calcium carbonate. The modified calcium carbonate is then mixed with other components and pressed into plain tablets. Simultaneously, a film coating emulsion is prepared using water as the dispersion medium via pre-emulsified seed emulsion polymerization, introducing reactive groups such as carboxyl groups into the film coating. When the emulsion is used to coat the plain tablets, the amino groups on the surface of the modified calcium carbonate bind to the carboxyl groups in the film coating through charge neutralization. Simultaneously, the polymer chains entangle to form a three-dimensional network, tightly enveloping the film coating onto the surface of the formulation, forming a dense film. This mechanism of action offers dual advantages: first, the porous structure and amino treatment of the modified calcium carbonate enhance its binding and compatibility with the film coating, promoting uniform adhesion to the formulation surface. Second, the resulting film exhibits excellent sealing properties, effectively shielding the active ingredients from the effects of external factors such as light, heat, oxygen, and humidity, inhibiting particle agglomeration and phase separation, and ensuring formulation stability. Test results show that the formulation of the present invention exhibits no significant change in appearance after long-term storage, minimal loss in hardness, and meets specified friability requirements. It exhibits excellent sealing, coating, stability, and no leakage, effectively resolving the prior art issue of active ingredients being susceptible to external influences and lacking stability. Furthermore, the formulation dissolves in the presence of human gastric acid, promoting uniform and rapid release of the contents while balancing storage stability and effectiveness. Test results indicate that the primary efficacy of the present invention is in promoting sleep onset, improving overall sleep quality, enhancing next-day mental well-being, and promoting gastrointestinal conditioning, with attendant benefits such as enhancing appetite and brightening skin tone. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 A histogram showing the percentages of preliminary test results is shown.

[0029] Figure 2 A histogram showing the percentage of test results for the expanded population is shown.

[0030] Figure 3 A histogram of the results of repeated validation tests is shown.

[0031] Figure 4 A histogram showing the percentages of test results for the long term test is shown.

[0032] Figure 5A line graph showing the percentage of test results for the long term test. DETAILED DESCRIPTION

[0033] In order to more clearly illustrate the technical solutions of the present invention, the following examples are given. Unless otherwise stated, the raw materials, reactions and post-processing methods mentioned in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0034] The terms "preferred," "preferably," "more preferred," and the like, used herein, refer to embodiments of the invention that may provide certain benefits under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.

[0035] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.

[0036] The present invention uses the following raw materials:

[0037] Sodium carboxymethyl starch: purchased from Wuhan Nengren Pharmaceutical Chemical Co., Ltd.

[0038] Hydroxypropyl methylcellulose: SH-E3, purchased from Anhui Shanhe Pharmaceutical Excipients Co., Ltd.

[0039] Emulsifier: sodium lauryl sulfate.

[0040] Initiator: potassium persulfate.

[0041] Ziziphus jujuba seed extract, valerian extract, and chamomile extract were purchased from Shaanxi Jiahe Biotechnology Co., Ltd.

[0042] Casein: Food grade casein was purchased from Shandong Aicai Biotechnology Co., Ltd.

[0043] The water in the present invention is all deionized water.

[0044] The "parts" in the present invention refer to parts by mass.

[0045] Example 1

[0046] A multifunctional anti-aging and sleep-aiding preparation, comprising the following components in parts by mass:

[0047]

[0048] The modified calcium carbonate is porous calcium carbonate that has been aminated;

[0049] The film coating material is prepared by reacting the following raw materials in parts by mass:

[0050]

[0051]

[0052] The preparation method of the above-mentioned multifunctional anti-aging and sleep-aiding preparation comprises the following steps:

[0053] S1. Calcium acetate and ammonium carbonate are respectively prepared into 0.5 mol / L aqueous solutions. Under the condition of rapid stirring, the ammonium carbonate aqueous solution is poured into the calcium acetate aqueous solution (calcium acetate: ammonium carbonate = 1:1, n / n), stirred for 10 min, allowed to stand for aging for 0.5 h, filtered, washed, and dried to obtain porous calcium carbonate; the porous calcium carbonate is blended with triethanolamine (porous calcium carbonate: triethanolamine = 1:11, m / m), reacted at 80° C. for 1 h, filtered, washed, and dried to obtain modified calcium carbonate;

[0054] S2. Add the emulsifier to 10 parts of water according to the above mass parts, stir and mix, then add acrylic acid, methyl acrylate and trihydroxypropane trimethacrylate, and stir at 50°C for 0.5h to obtain a pre-emulsion;

[0055] S3. Under nitrogen protection, the pre-emulsion and the initiator are mixed, stirred and reacted at 80° C. for 10 hours, and filtered to obtain a film coating material emulsion;

[0056] S4. According to the above-mentioned mass fractions, the components other than the film coating material are evenly blended and pressed into plain tablets with a tablet weight of 1.2 g. The plain tablets are placed in a coating pan and preheated. When the tablet bed temperature reaches 50°C, the film coating material emulsion is used for coating. The tablet bed temperature is controlled to be about 50°C and the flow rate of the film coating material emulsion is 50 g / min. The film coating material is coated on the surface of the plain tablet. After drying, an anti-aging and sleep-aiding multifunctional preparation is obtained, and the coating weight gain is 3%.

[0057] Example 2

[0058] A multifunctional anti-aging and sleep-aiding preparation, comprising the following components in parts by mass:

[0059]

[0060] The modified calcium carbonate is porous calcium carbonate that has been aminated;

[0061] The film coating material is prepared by reacting the following raw materials in parts by mass:

[0062]

[0063] The preparation method of the above multifunctional anti-aging and sleep-aiding preparation is the same as that of Example 1, except that, in step S2, an emulsifier is added to 7 parts of water.

[0064] Example 3

[0065] A multifunctional anti-aging and sleep-aiding preparation, comprising the following components in parts by mass:

[0066]

[0067] The modified calcium carbonate is porous calcium carbonate that has been aminated;

[0068] The film coating material is prepared by reacting the following raw materials in parts by mass:

[0069]

[0070] The preparation method of the above multifunctional anti-aging and sleep-aiding preparation is the same as that of Example 1, except that, in step S2, an emulsifier is added to 12 parts of water.

[0071] Comparative Example 1

[0072] A multifunctional preparation for anti-aging and sleep aid. The difference between this comparative example and Example 1 is that in step S1, the porous calcium carbonate is not modified, and in step S4, the modified calcium carbonate is replaced with porous calcium carbonate. The other steps and amounts are the same as in Example 1.

[0073] Comparative Example 2

[0074] A multifunctional preparation for anti-aging and sleep aid. The difference between this comparative example and Example 1 is that in step S2, the mass of the acrylic acid is replaced by methyl acrylate, and the other steps and amounts are the same as those in Example 1.

[0075] Test Example 1

[0076] Performance tests were performed on Examples 1-3 and Comparative Examples 1-2.

[0077] Test Method: Appearance testing was performed using the Chinese Pharmacopoeia (2010 edition), along with hardness testing using a YD-3 hardness tester and friability testing using a CS-1 friability tester. The samples were then placed under normal temperature and humidity conditions for 12 months and then tested again.

[0078] The test results are shown in Table 1.

[0079] Table 1 Performance test results

[0080]

[0081] The above test results show that the anti-aging and sleep-aiding multifunctional preparation of the present invention has no obvious change in appearance after 12 months of storage at room temperature and humidity, a small decrease in hardness, and meets the requirements for friability. It has the characteristics of good sealing, good coating, and good stability, and will not leak.

[0082] Test Example 2

[0083] The anti-aging and sleep-aiding multifunctional preparation of Example 1 was tested to verify the improvement effects of the main active ingredients of the product on volunteers.

[0084] Test method:

[0085] (1) Recruit volunteers through questionnaires.

[0086] (2) Preliminary testing: 16 volunteers were recruited to pick up the products on site and conduct a one-week test.

[0087] (3) Expand the population test: After initially confirming the effectiveness of the product, expand the population and recruit volunteers to conduct four batches of 26 people for a week to analyze the differences between the populations.

[0088] (4) Repeat verification: The second week test is conducted on the 26 people in the four groups mentioned above who do not have obvious physical sensations every time, to see if the results are improved and to verify the repeatability of the efficacy.

[0089] (5) Long-term testing: Repeat the experiment to conduct long-term testing (total time is 28 days) on products with unstable sensory feedback results to verify the long-term effectiveness and safety of the product, to see whether the efficacy is stable and whether there will be any adverse reactions.

[0090] Data collection methods: questionnaire (screening, follow-up, information collection, etc.), WeChat chat, and telephone follow-up.

[0091] The test results are shown in Table 1-5. Figure 1-5 shown.

[0092] Table 1 Preliminary test results (unit: person)

[0093]

[0094] Figure 1 A histogram showing the percentages of preliminary test results is shown. These test results indicate that after seven days of intervention, all 16 subjects showed positive improvements in both physiological (sleep, gastrointestinal) and psychological (state, appetite) aspects, with an overall upward trend in improvement rates. This validates the short-term effectiveness of the present invention, and further consideration is given to expanding the scope of testing and extending the testing period.

[0095] Table 2 Expanded population test results (unit: person)

[0096]

[0097] Figure 2 A histogram showing the percentage of test results for the expanded population is shown. The above test results show that over the 7-day test, the somatosensory feedback data of the 26 subjects showed large fluctuations in improvement. However, this group of people did not completely lose any somatosensory perception. It is speculated that this may be due to insufficient duration of use, insufficient improvement, or individual differences. Long-term trials are being conducted to screen those with less obvious somatosensory perceptions to observe changes and monitor the possibility of adverse reactions.

[0098] Table 3 Repeated verification test results

[0099] stage Easy to fall asleep Overall sleep quality Next day status Bowel movement / gastrointestinal conditioning skin appetite Day 9 17％ 26％ 35％ 4％ 4％ 0％ Day 11 70％ 35％ 65％ 48％ 61％ 43％ Day 13 57％ 43％ 70％ 61％ 52％ 57％ Day 15 65％ 39％ 74％ 57％ 61％ 57％

[0100] Figure 3 The following histogram shows the results of repeated validation tests. As can be seen from the above test results, the overall improvement was significant in the second week, indicating that extending the duration of use significantly improved the improvement. However, after stopping for one day in the middle of the two-week period, the physical sensation was not immediately noticeable, indicating that the product's effectiveness is best achieved with continuous use.

[0101] Table 4 Long-term test results (unit: person)

[0102]

[0103] Table 5 Percentage of long-term test results

[0104]

[0105] Figure 4 A histogram showing the percentages of test results for the long-term test; Figure 5 A line chart showing the percentage of long-term test results shows that the long-term efficacy of the present invention is relatively stable, but if you take it again after a 2-3 day interval, the effect will not be immediate on the first day of use. It takes two days for the effect to gradually recover. No serious adverse reactions occurred during this period.

[0106] Preliminary testing, expanded population testing, repeatable experiments, and long-term validation have shown that the primary benefits of this invention are promoting sleep onset, improving overall sleep quality, enhancing next-day mental well-being, and supporting gastrointestinal conditioning, with associated benefits such as enhancing appetite and brightening skin tone. Those with a high sensitivity to the product will experience noticeable and sustained effects within the first week of use. Those with less noticeable effects will also experience significant improvements with long-term use, but prolonged interruptions are not recommended to prevent diminished effects.

[0107] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0108] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A multifunctional anti-aging and sleep-aiding preparation, characterized in that: The anti-aging and sleep-aiding multifunctional preparation comprises the following components in parts by mass: The modified calcium carbonate is porous calcium carbonate that has been aminated; The film coating material is prepared by reacting the following raw materials in parts by mass:

2. The anti-aging and sleep-aiding multifunctional preparation according to claim 1, characterized in that: The acrylic acid ester is selected from one or more of methyl methacrylate, ethyl methacrylate or n-butyl acrylate.

3. The anti-aging and sleep-aiding multifunctional preparation according to claim 1, characterized in that: The emulsifier is selected from one or more of sodium lauryl sulfate, octylphenol polyoxyethylene ether-10, sorbitan monolaurate, and polyoxyethylene sorbitan monooleate.

4. The anti-aging and sleep-aiding multifunctional preparation according to claim 1, characterized in that: The initiator is potassium persulfate.

5. The method for preparing the anti-aging and sleep-aiding multifunctional preparation according to any one of claims 1 to 4, characterized in that: The steps include: S1. Blending calcium acetate and ammonium carbonate, stirring and reacting to obtain porous calcium carbonate; blending the porous calcium carbonate with triethanolamine, heating and reacting to obtain modified calcium carbonate; S2, blending the emulsifier and water, stirring and mixing, then adding acrylic acid, acrylate and trihydroxypropane trimethacrylate, heating and stirring to obtain a pre-emulsion; S3. Under the protection of inert gas, the pre-emulsion and the initiator are mixed, heated and stirred to react, to obtain a film coating material emulsion; S4. Evenly blend the components other than the film coating material, press into plain tablets, and then coat with the film coating material emulsion to coat the surface of the plain tablets with the film coating material. After drying, obtain the anti-aging and sleep-aiding multifunctional preparation.

6. The method for preparing the anti-aging and sleep-aiding multifunctional preparation according to claim 5, characterized in that: In step S1, the molar ratio of calcium acetate to ammonium carbonate is 1:(0.5-1.5).

7. The method for preparing the anti-aging and sleep-aiding multifunctional preparation according to claim 5, characterized in that: In step S1, the mass ratio of the porous calcium carbonate to triethanolamine is 1:(10-15).

8. The method for preparing the anti-aging and sleep-aiding multifunctional preparation according to claim 5, characterized in that: In step S1, the heating temperature is 70-90°C.

9. The method for preparing the multifunctional anti-aging and sleep-aiding preparation according to claim 5, characterized in that: In step S2, the heating temperature is 40-60°C.

10. The method for preparing the anti-aging and sleep-aiding multifunctional preparation according to claim 5, characterized in that: In step S3, the heating temperature is 70-90°C.

Images