Cough-relieving composition containing steamed orange active extract and green preparation method of cough-relieving composition

Abstract

The invention belongs to the technical field of medicine and green chemistry, and particularly relates to a cough-relieving composition containing steamed orange active extract and a green preparation method thereof.The method comprises the following steps that S10, steamed orange raw materials are smashed into powder with the particle size of 80-120 meshes, deionized water is added, the powder is mixed according to the mass ratio of 1: 5-1: 10, the mixture is heated to 60-80 DEG C, and the mixture is stirred to be uniform; stirring and extracting for 3-5 hours to obtain a steamed orange crude extract; and S20, cooling the steamed orange crude extract to room temperature, and carrying out primary filtration through a ceramic membrane. By adopting a recyclable natural adsorbent and a high-efficiency membrane filtration technology, the extraction and purification process is optimized, the purity and the recovery rate of active ingredients of the steamed oranges are remarkably improved, meanwhile, waste discharge is reduced, and the method has the characteristics of being green and environmentally friendly; the method is superior to a traditional process in the aspects of purity, recovery rate and environmental protection of active ingredients, and is suitable for being used as an efficient and environment-friendly preparation scheme of the cough-relieving composition.

Description

Technical Field

[0001] The invention belongs to the technical field of medicine and green chemistry, and in particular relates to a cough suppressant composition containing steamed orange active extract and a green preparation method thereof. Background Art

[0002] Steamed orange extract has significant cough-relieving and expectorant properties and is widely used in traditional Chinese medicine preparations. However, existing techniques for preparing cough-relieving compositions containing steamed orange extract primarily rely on traditional extraction and purification methods, such as decoction, ethanol extraction, or macroporous resin adsorption. While these methods can achieve a certain degree of effective ingredient extraction, they still have limitations in terms of green preparation and overall performance optimization.

[0003] Patent WO2017036241A1 discloses an acne-removing traditional Chinese medicine composition and its preparation method. The composition is prepared using mangosteen peel, thyme, and fructus aurantii via ethanol extraction and macroporous resin purification. Its advantage lies in achieving a synergistic effect of the active ingredients through elution with a specific ethanol concentration (60%-80%), while also exhibiting a good anti-inflammatory effect. However, this method requires high equipment requirements, and the use of macroporous resin may lead to difficulties in regeneration, thereby increasing resource consumption and environmental burden.

[0004] Patent WO2019233158A1 discloses a traditional Chinese medicine gel composition and its preparation method. Its core is a decoction of traditional Chinese medicine extracts and a clear paste purified with a macroporous adsorption resin, supplemented with surfactants and polymer hydrogels. This technology has the advantage of effectively combining multiple traditional Chinese medicine ingredients to form a stable gel system, making it suitable for the development of beauty products.

[0005] However, most of the above methods face the environmental problem that the macroporous adsorption resin is difficult to completely degrade, which limits their application scope. Therefore, to address the above problem, a cough suppressant composition containing steamed orange active extract and an environmentally friendly preparation method thereof are proposed. Summary of the Invention

[0006] The present application provides a cough suppressant composition containing steamed orange active extract and a green preparation method thereof, aiming to optimize the extraction and purification process by adopting recyclable natural adsorbents and high-efficiency membrane filtration technology, while reducing waste emissions and improving product purity.

[0007] The technical solution adopted by the present invention to solve the technical problem is as follows: In a first aspect, the present application provides a method for preparing a cough suppressant composition containing an active extract of steamed orange, comprising the following steps: S10: Grinding the steamed orange raw material into a powder with a particle size of 80 mesh to 120 mesh, adding deionized water, mixing at a mass ratio of 1:5 to 1:10, heating to 60° C. to 80° C., and stirring and extracting for 3 to 5 hours to obtain a crude steamed orange extract; S20: After cooling the crude orange extract to room temperature, the crude orange extract is filtered through a ceramic membrane with a pore size of 0.45 μm to 0.8 μm to remove suspended particulate impurities, and the filtrate is collected; S30: Passing the filtrate after the primary filtration through an activated carbon column loaded with chitosan for adsorption purification, controlling the flow rate to be 10 ml / min to 20 ml / min, and the adsorption time to be 30 min to 60 min; S40: eluting the adsorption column with a 40% to 60% volume fraction ethanol solution, collecting the eluate, and concentrating under reduced pressure to 1 / 5 to 1 / 10 of the original volume to obtain a concentrated solution of the steamed orange active extract; S50: Mixing the concentrated active extract of steamed orange with auxiliary materials, wherein the auxiliary materials include honey, licorice extract and peppermint oil, in a mass ratio of 1:0.2 to 1:0.5, and preparing a cough suppressant composition after drying.

[0008] According to the present application, the above-mentioned method can significantly reduce the amount of non-renewable adsorbent used in traditional processes, while also avoiding the problem of difficult degradation of macroporous resins. Chitosan, as a natural polymer material, has excellent adsorption properties and is easily biodegradable. Combined with the synergistic effect of the activated carbon column, it improves the recovery rate and purity of the active ingredients of the steamed orange. In addition, the primary filtration step of the ceramic membrane effectively reduces the risk of suspended particulate contamination of subsequent adsorption columns, extending the service life of the adsorption columns.

[0009] Preferably, in some embodiments, in step S20, the pore size of the ceramic membrane is preferably 0.5 μm to 0.7 μm. This pore size range can maximize the retention of the active ingredients of the distilled orange while ensuring filtration efficiency, and avoid impurity residues caused by excessively large pores or membrane clogging caused by excessively small pores.

[0010] Preferably, in some embodiments, in step S30, the chitosan loading accounts for 5% to 15% of the total weight of the activated carbon. The appropriate loading of chitosan not only improves the adsorption capacity of the activated carbon, but also enhances its selective adsorption effect on the active ingredients of the steamed orange, thereby further improving the purity of the target product.

[0011] Preferably, in some embodiments, in step S40, the flow rate of the ethanol solution during the elution process is controlled within a range of 15 ml / min to 25 ml / min. By adjusting the flow rate, the eluent is ensured to fully contact the active sites within the adsorption column, thereby achieving efficient desorption of the active ingredient in the distilled orange.

[0012] Preferably, in some embodiments, in step S50, the mass ratio of honey, licorice extract, and peppermint oil is preferably 1:0.3:0.1. The combination of excipients at this ratio not only improves the taste of the cough suppressant composition, but also enhances its throat-soothing effect, making it more suitable for use as an oral preparation.

[0013] Preferably, in some embodiments, in step S10, the steamed orange raw material is pulverized into a particle size of 100 mesh.

[0014] Preferably, in some embodiments, in step S10, the mass ratio of the steamed orange raw material to the deionized water is 1:8.

[0015] Preferably, in some embodiments, in step S40, the volume fraction of the ethanol solution is 50%.

[0016] Preferably, in some embodiments, in step S30, the adsorption time is 45 minutes.

[0017] In a second aspect, the present application provides a cough suppressant composition containing an active extract of steamed orange, prepared according to the method described in any embodiment of the first aspect. Because the cough suppressant composition is prepared according to the method described in any embodiment of the first aspect, it has high active ingredient purity and environmentally friendly properties.

[0018] Beneficial effects of the present invention: By utilizing recyclable natural adsorbents and high-efficiency membrane filtration technology, this method optimizes the extraction and purification process, significantly improving the purity and recovery rate of the active ingredient in steamed orange, while also reducing waste emissions and demonstrating environmental friendliness. Experimental data demonstrates that this method outperforms traditional processes in terms of active ingredient purity, recovery rate, and environmental friendliness, making it suitable for the preparation of an efficient and environmentally friendly cough suppressant composition. The present invention can significantly reduce the amount of non-renewable adsorbents used in traditional processes, while avoiding the problem of difficult degradation of macroporous resins. Chitosan, as a natural polymer material, has good adsorption properties and is easy to biodegrade. Combined with the synergistic effect of the activated carbon column, the recovery rate and purity of the active ingredients of steamed orange are improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The drawings described herein are used to provide further understanding of the present invention and constitute a part of this application. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations on the present invention.

[0020] In the attached figure: Figure 1 It is the overall process flow chart of the present invention; Figure 2 It is a detailed step flow chart of the present invention. DETAILED DESCRIPTION

[0021] The following embodiments or implementation schemes in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. In the description of this specification, the reference terms "one embodiment", "some embodiments", "illustrative embodiments", "example", "specific example", or "some examples" are intended to refer to specific features, structures, materials or characteristics described in conjunction with the implementation or example and included in at least one embodiment or example of the present application. In this specification, the schematic representation of the above terms does not necessarily refer to the same implementation or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more implementations or examples in a suitable scheme.

[0022] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of such features. Throughout the description of this application, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0023] In a first aspect, the present application provides a method for preparing an antitussive composition containing an active extract of steamed orange, comprising the following steps: S10: Grinding the steamed orange raw material into a powder with a particle size of 80 mesh to 120 mesh, adding deionized water, mixing at a mass ratio of 1:5 to 1:10, heating to 60° C. to 80° C., and stirring and extracting for 3 to 5 hours to obtain a crude steamed orange extract; S20: After cooling the crude orange extract to room temperature, the crude orange extract is filtered through a ceramic membrane with a pore size of 0.45 μm to 0.8 μm to remove suspended particulate impurities, and the filtrate is collected; S30: Passing the filtrate after the primary filtration through an activated carbon column loaded with chitosan for adsorption purification, controlling the flow rate to be 10 ml / min to 20 ml / min, and the adsorption time to be 30 min to 60 min; S40: eluting the adsorption column with a 40% to 60% volume fraction ethanol solution, collecting the eluate, and concentrating under reduced pressure to 1 / 5 to 1 / 10 of the original volume to obtain a concentrated solution of the steamed orange active extract; S50: Mixing the concentrated active extract of steamed orange with auxiliary materials, wherein the auxiliary materials include honey, licorice extract and peppermint oil, in a mass ratio of 1:0.2 to 1:0.5, and preparing a cough suppressant composition after drying.

[0024] According to the present application, in step S10, the steamed orange raw material is preferably fresh steamed orange peel, which is crushed to a particle size range of 80 to 120 mesh, which can effectively increase the raw material surface area and improve extraction efficiency. The mass ratio of deionized water added to the steamed orange raw material is 1:5 to 1:10, which can ensure sufficient contact during the extraction process. The heating temperature is 60°C to 80°C, and the stirring time is set to 3 to 5 hours, which can ensure extraction efficiency while avoiding the destruction of active ingredients caused by high temperature.

[0025] In step S20, the ceramic membrane has a pore size range of 0.45 to 0.8 microns, preferably 0.5 to 0.7 microns. This pore size range effectively removes suspended particulate impurities while maximizing the retention of the active ingredients in the distilled orange. Ceramic membranes are selected for their high-temperature resistance, corrosion resistance, and ease of cleaning, making them suitable for the separation and purification of natural products.

[0026] In step S30, the activated carbon column is loaded with chitosan, with the chitosan loading accounting for 5% to 15% of the total mass of the activated carbon. Chitosan, a natural polymer material, has excellent adsorption properties and is easily biodegradable. Its appropriate loading can improve the adsorption capacity of the activated carbon and enhance the selective adsorption of the active ingredient in the steamed orange. During the adsorption process, the flow rate is controlled within the range of 10 ml / min to 20 ml / min, and the adsorption time is 30 to 60 minutes, which can ensure sufficient adsorption of the target ingredient.

[0027] In step S40, elution is performed using a 40% to 60% ethanol solution by volume, with a flow rate controlled within the range of 15 to 25 ml / min. This ensures that the eluent fully contacts the active sites within the adsorption column, achieving efficient desorption of the active ingredients from the steamed orange. The eluent is then concentrated under reduced pressure to 1 / 5 to 1 / 10 of its original volume, significantly increasing the concentration of the active extract from the steamed orange.

[0028] In step S50, the concentrated active extract of steamed orange is mixed with auxiliary materials, including honey, licorice extract, and peppermint oil, which are uniformly mixed in a mass ratio of 1:0.2 to 1:0.5. The addition of honey improves the taste and soothes the throat, the licorice extract has a certain auxiliary cough-relieving effect, and the peppermint oil provides a cooling sensation and relieves throat discomfort. The mixed materials are then dried to produce a cough-relieving composition.

[0029] In some embodiments, in step S10, the particle size of the steamed orange raw material is preferably 100 mesh, the mass ratio of the added deionized water to the steamed orange raw material is preferably 1:8, the heating temperature is preferably 70°C, and the stirring time is preferably 4 hours. Optimizing these parameters can further improve extraction efficiency.

[0030] In some embodiments, in step S20, the pore size of the ceramic membrane is preferably 0.6 microns. This pore size can maximize the retention of the active ingredients of the distilled orange while ensuring filtration efficiency, and avoid impurity residues caused by too large a pore size or membrane clogging caused by too small a pore size.

[0031] In some embodiments, in step S30, the chitosan loading is preferably 10% of the total mass of the activated carbon, the adsorption flow rate is preferably 15 ml / min, and the adsorption time is preferably 45 minutes. Optimization of these parameters can improve adsorption efficiency and extend the service life of the adsorption column.

[0032] In some embodiments, in step S40, the volume fraction of the ethanol solution is preferably 50%, and the elution flow rate is preferably 20 ml / min. Optimization of these parameters can achieve efficient elution of the active ingredient of the distilled orange.

[0033] In some embodiments, in step S50, the mass ratio of honey, licorice extract and peppermint oil is preferably 1:0.3:0.1. The combination of excipients in this ratio can improve the taste of the cough suppressant composition and enhance its throat-soothing effect.

[0034] In a second aspect, the present application provides an antitussive composition containing an active extract of steamed orange, which is prepared according to the method of any embodiment of the first aspect.

[0035] Specific examples are given below.

[0036] Example 1 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 100 mesh, add 8 liters of deionized water, heat it to 70°C, and stir and extract for 4 hours to obtain a crude steamed orange extract. After the crude extract is cooled to room temperature, it is filtered through a ceramic membrane with a pore size of 0.6 microns, and the filtrate is collected; Subsequently, the filtrate was purified by adsorption on an activated carbon column loaded with 10% chitosan, with a controlled flow rate of 15 ml / min and an adsorption time of 45 min; The mixture was eluted with 50% ethanol solution, the eluate was collected, and concentrated under reduced pressure to 1 / 8 of the original volume to obtain a concentrated solution of the active extract of distilled orange; Finally, the concentrate was evenly mixed with honey, licorice extract and peppermint oil in a mass ratio of 1:0.3:0.1, and dried to prepare a cough suppressant composition.

[0037] Example 2 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 80 mesh, add 10 liters of deionized water, heat it to 65°C, and stir and extract for 5 hours to obtain a crude steamed orange extract. After the crude extract is cooled to room temperature, it is filtered through a ceramic membrane with a pore size of 0.7 microns, and the filtrate is collected; Subsequently, the filtrate was purified by adsorption on an activated carbon column loaded with 15% chitosan, with a controlled flow rate of 20 ml / min and an adsorption time of 30 min; The mixture was eluted with 60% ethanol solution, the eluate was collected, and concentrated under reduced pressure to 1 / 10 of the original volume to obtain a concentrated solution of the active extract of distilled orange; Finally, the concentrate was evenly mixed with honey, licorice extract and peppermint oil in a mass ratio of 1:0.2:0.1, and dried to prepare a cough suppressant composition.

[0038] Example 3 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 120 mesh, add 5 liters of deionized water, heat it to 75°C, and stir and extract for 3 hours to obtain a crude steamed orange extract. After the crude extract is cooled to room temperature, it is filtered through a ceramic membrane with a pore size of 0.5 microns and the filtrate is collected; Subsequently, the filtrate was purified by adsorption on an activated carbon column loaded with 5% chitosan, with a controlled flow rate of 10 ml / min and an adsorption time of 60 min; The mixture was eluted with 40% ethanol solution, the eluate was collected, and concentrated under reduced pressure to 1 / 5 of the original volume to obtain a concentrated solution of the active extract of distilled orange; Finally, the concentrate was evenly mixed with honey, licorice extract and peppermint oil in a mass ratio of 1:0.5:0.2, and dried to prepare a cough suppressant composition.

[0039] Comparative Example 1 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 100 mesh, add 8 liters of deionized water, heat to 70°C, and stir and extract for 4 hours to obtain a crude steamed orange extract; After the crude extract was cooled to room temperature, it was directly passed through an activated carbon column without chitosan loading for adsorption purification, with a flow rate of 15 ml / min and an adsorption time of 45 min. The mixture was eluted with 50% ethanol solution, the eluate was collected, and concentrated under reduced pressure to 1 / 8 of the original volume to obtain a concentrated solution of the active extract of distilled orange; Finally, the concentrate was evenly mixed with honey, licorice extract and peppermint oil in a mass ratio of 1:0.3:0.1, and dried to prepare a cough suppressant composition.

[0040] Comparative Example 2 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 100 mesh, add 8 liters of deionized water, heat it to 70°C, and stir and extract for 4 hours to obtain a crude steamed orange extract. After the crude extract is cooled to room temperature, it is filtered through a ceramic membrane with a pore size of 0.6 microns, and the filtrate is collected; Subsequently, the filtrate was passed through a macroporous resin column for adsorption purification, with a controlled flow rate of 15 ml per minute and an adsorption time of 45 minutes; The mixture was eluted with 50% ethanol solution, the eluate was collected, and concentrated under reduced pressure to 1 / 8 of the original volume to obtain a concentrated solution of the active extract of distilled orange; Finally, the concentrate was evenly mixed with honey, licorice extract and peppermint oil in a mass ratio of 1:0.3:0.1, and dried to prepare a cough suppressant composition.

[0041] Comparative Example 3 Take 1 kg of fresh steamed orange peel, crush it to a particle size of 100 mesh, add 8 liters of deionized water, heat to 70°C, and stir and extract for 4 hours to obtain a crude steamed orange extract; After the crude extract was cooled to room temperature, it was filtered through a ceramic membrane with a pore size of 0.6 μm and the filtrate was collected; Subsequently, the filtrate was directly concentrated under reduced pressure to 1 / 8 of its original volume to obtain a concentrated solution of steamed orange active extract. Finally, the concentrated solution was evenly mixed with honey, licorice extract, and peppermint oil in a mass ratio of 1:0.3:0.1, and dried to obtain a cough suppressant composition.

[0042] In the examples, recyclable natural adsorbents and high-efficiency membrane filtration technology were used, while in the comparative examples, traditional processes were used. The purity of the active ingredient was determined by precise analytical testing methods, such as high-performance liquid chromatography (HPLC), and the recovery rate was determined by gravimetric analysis. The waste generated during the production process was weighed to calculate the waste discharge volume. The comparison of Examples 1-3 and Comparative Examples 1-3 in terms of active ingredient purity, recovery rate, and waste discharge is shown in the following table.

[0043]

[0044] By utilizing recyclable natural adsorbents and high-efficiency membrane filtration technology, the extraction and purification process has been optimized, significantly improving the purity and recovery rate of the active ingredient in steamed orange, while also reducing waste emissions and demonstrating environmentally friendly properties. Experimental data demonstrates that this method outperforms traditional processes in terms of active ingredient purity, recovery rate, and environmental friendliness, making it suitable for the preparation of an efficient and environmentally friendly cough suppressant composition. The above data demonstrate that the method provided by this application outperforms the comparative example in terms of active ingredient purity, recovery rate, and environmental friendliness. In particular, the synergistic effect of the chitosan-loaded activated carbon column and ceramic membrane filtration significantly improves overall process performance.

[0045] In the description of the present invention, the preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0046] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A cough suppressant composition containing steamed orange active extract and a green preparation method thereof, characterized in that: The following steps are involved: S10: Grinding the steamed orange raw material into a powder with a particle size of 80 mesh to 120 mesh, adding deionized water, mixing at a mass ratio of 1:5 to 1:10, heating to 60° C. to 80° C., and stirring and extracting for 3 to 5 hours to obtain a crude steamed orange extract; S20: After cooling the crude orange extract to room temperature, the crude orange extract is filtered through a ceramic membrane with a pore size of 0.45 μm to 0.8 μm to remove suspended particulate impurities, and the filtrate is collected; S30: Passing the filtrate after the primary filtration through an activated carbon column loaded with chitosan for adsorption purification, controlling the flow rate to be 10 ml / min to 20 ml / min, and the adsorption time to be 30 min to 60 min; S40: eluting the adsorption column with an ethanol solution having a volume fraction of 40% to 60%, collecting the eluate, and concentrating under reduced pressure to 1 / 5 to 1 / 10 of the original volume to obtain a concentrated solution of the active extract of steamed orange; S50: mixing the concentrated solution of the active extract of steamed orange with excipients, wherein the excipients include honey, licorice extract, and peppermint oil, and uniformly mixing them in a mass ratio of 1:0.2 to 1:0.5, and drying to obtain a cough suppressant composition.

2. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S20, the pore size of the ceramic membrane is 0.5 micrometer to 0.7 micrometer.

3. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S30, the chitosan loading accounts for 5% to 15% of the total mass of the activated carbon.

4. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S40, the flow rate of the ethanol solution during the elution process is 15 ml / min to 25 ml / min.

5. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S50, the mass ratio of honey, licorice extract and peppermint oil is 1:0.3:0.

1.

6. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In the step S10, the steamed orange raw material is pulverized into a particle size of 100 mesh.

7. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S10, the mass ratio of the steamed orange raw material to the deionized water is 1:

8.

8. The cough suppressant composition containing the steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S40, the volume fraction of the ethanol solution is 50%.

9. The cough suppressant composition containing steamed orange active extract and the green preparation method thereof according to claim 1, characterized in that: In step S30, the adsorption time is 45 minutes.

10. A cough suppressant composition containing steamed orange active extract, characterized in that: Prepared according to the method according to any one of claims 1 to 9.

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