A composite anti-allergic soothing extract and its use in cosmetics

Abstract

The application discloses a composite anti-allergic soothing extract and application thereof in cosmetics. The application selects Gentiana macrophylla Pall and Lonicera japonica as raw materials, and provides a composite anti-allergic soothing extract. A low-temperature extraction process is adopted to maximize the stability of active components of Gentiana macrophylla Pall and simultaneously enrich anti-allergic soothing components of iridoid glycosides and alkaloids. The composite anti-allergic soothing extract provided by the embodiment of the application can be added into auxiliary materials or auxiliary components in the field of cosmetics to prepare cosmetics with anti-allergic soothing effects, such as creams, lotions, serums, masks and toners.

Description

Technical Field

[0001] This invention relates to the field of cosmetics, and in particular to a compound anti-allergic and soothing extract and its application in cosmetics. Background Technology

[0002] Gentiana macrophylla Pall., a perennial herb belonging to the Gentianaceae family and the Gentian genus, is a traditional and commonly used Chinese medicinal herb. First recorded in the *Shennong Bencao Jing* (Shennong's Classic of Materia Medica), it is listed as a medium-grade herb. Its root is used medicinally; it is bitter and pungent in taste, neutral in nature, and enters the stomach, liver, and gallbladder meridians. It has the effects of dispelling wind-dampness, clearing damp-heat, and relieving pain. Modern pharmacological studies have shown that Gentiana macrophylla contains various active ingredients such as iridoid glycosides, alkaloids, triterpenoids, and flavonoids, exhibiting multiple biological activities including anti-inflammatory, antioxidant, moisturizing, soothing, repairing, and antibacterial properties. These activities highly align with the core efficacy of cosmetics, making it a promising candidate for application in the field of functional cosmetics.

[0003] Among them, iridoid glycosides (such as gentiopicroside, loganic acid, and swertiamarin) and alkaloids (such as gentianine and gentianine A) are the main active components of Gentiana macrophylla that exert its anti-allergic and soothing effects. Iridoid glycosides have significant anti-inflammatory, antioxidant, and soothing repair effects. They can inhibit the release of inflammatory factors such as TNF-α, IL-6, and prostaglandin E2, scavenge free radicals such as DPPH and ABTS, and reduce skin inflammation and oxidative damage. Studies have also shown that they can promote the synthesis of ceramides in the stratum corneum, repair the skin barrier, and alleviate common problems of sensitive skin such as redness, stinging, and dryness. Alkaloids have anti-inflammatory, antibacterial, and sedative activities. For example, gentianine A can inhibit the release of allergic mediators such as histamine and serotonin, reduce skin allergic reactions, and relieve burning and itching caused by inflammation.

[0004] Currently, the extraction of active ingredients from Gentiana macrophylla mainly employs water decoction, organic solvent reflux, or macroporous resin purification. For example, Chinese patent application CN102372752A discloses a method for extracting gentiopicrin from Gentiana macrophylla, the steps of which include: pulverizing Gentiana macrophylla, adding water and heating for extraction 2-3 times, the extract being adsorbed by macroporous resin, concentrated by nanofiltration membrane, purified by polyamide resin column, and then extracted with ethyl acetate, crystallized, and dried to obtain the gentiopicrin product. However, this method has the following drawbacks: high-temperature extraction easily leads to the degradation and inactivation of heat-sensitive iridoid glycosides and alkaloids; organic solvent (ethyl acetate) extraction poses a risk of solvent residue, which does not meet the green safety requirements for cosmetics; the extraction selectivity is poor, a large number of impurities are co-extracted, and existing methods are mostly targeted at single components (such as gentiopicrin).

[0005] Therefore, there is an urgent need to develop an extraction and processing technology that can maintain the stability of Gentiana macrophylla's active ingredients while enriching iridoid glycosides and alkaloids for anti-allergic and soothing effects, in order to meet the cosmetics industry's pressing demand for functional plant-based raw materials. Summary of the Invention

[0006] The purpose of this invention is to provide a compound anti-allergic and soothing extract, which uses a low-temperature extraction process to maximize the stability of the active ingredients of Gentiana macrophylla, and simultaneously enriches iridoid glycosides and alkaloid anti-allergic and soothing components.

[0007] To achieve the above-mentioned objectives, the present invention provides the following technical solution: A compound anti-allergic and soothing extract is obtained by the following preparation method: (A) Weigh the following raw materials in parts by weight: 10-20 parts of Gentiana macrophylla root and 1-10 parts of Lonicera japonica, mix them, crush them, and pass them through a 10-50 mesh sieve to obtain a mixed powder; (B) The mixed powder is packed into a chromatography column and compacted to form a mixed powder packed column; it is then eluted with an aqueous ethanol solution to obtain the eluent. (C) The eluent is concentrated by rotary evaporation to obtain a concentrate; the concentrate is loaded onto a chromatography column packed with AB-8 macroporous resin; after loading, the resin is rinsed with deionized water, then eluted with citric acid aqueous solution to remove impurities, and finally eluted with high-concentration ethanol aqueous solution to collect the eluent. (D) The eluent is rotary evaporated to remove ethanol, thus obtaining the compound anti-allergic and soothing extract.

[0008] In some embodiments, the weight parts of each raw material in step (A) are: 15 parts of Gentiana macrophylla root and 4 parts of Lonicera japonica.

[0009] In some embodiments, the volume fraction of the ethanol-water solution in step (B) is 70-80%; the elution rate of the ethanol-water solution is 1-2 BV / h, and the collected eluent is 1-2 BV.

[0010] This invention employs an on-column dynamic extraction method, where the solvent continuously flows through the powder-filled column, continuously carrying out the dissolved active ingredients. This avoids the problem of insufficient extraction caused by concentration balance in traditional soaking extraction, while room temperature operation is beneficial for the stability of heat-sensitive components.

[0011] In some embodiments, the eluent in step (C) is concentrated by rotary evaporation to less than 1 / 10 of its original volume.

[0012] In some embodiments, the concentration loading rate in step (C) is 1-2 BV / h.

[0013] In some embodiments, the deionized water rinsing rate in step (C) is 1-2 BV / h, and the deionized water elution volume is 2-3 BV.

[0014] In some embodiments, the elution rate of the citric acid aqueous solution in step (C) is 1-2 BV / h, the concentration of the citric acid aqueous solution is 0.05-0.5 wt%, and the elution volume of the citric acid aqueous solution is 1-2 BV. This invention uses a low-concentration citric acid aqueous solution for intermediate elution, utilizing acidic conditions to protonate and elute some weakly acidic impurities, while the target components, iridoid glycosides and alkaloids, remain on the resin, thereby improving the purity of the final product.

[0015] In some embodiments, the elution rate of the high-concentration ethanol aqueous solution in step (C) is 1-2 BV / h; the volume fraction of the high-concentration ethanol aqueous solution is 85-95%; and the elution volume of the high-concentration ethanol aqueous solution is 2-3 BV.

[0016] A cosmetic product, wherein the cosmetic product is prepared by adding the above-mentioned compound anti-allergic and soothing extract, and excipients or auxiliary ingredients in the field of cosmetics.

[0017] The cosmetics mentioned can be in the form of creams, lotions, serums, masks, toners, shampoos, shower gels, etc.

[0018] Compared with the prior art, the present invention has the following advantages: The compound anti-allergic and soothing extract provided in this embodiment of the invention uses Gentiana macrophylla and Lonicera japonica as raw materials to provide a compound anti-allergic and soothing extract. It adopts a low-temperature extraction process to maximize the stability of the active ingredients of Gentiana macrophylla and simultaneously enrich iridoid glycosides and alkaloid anti-allergic and soothing components.

[0019] The compound anti-allergic and soothing extract provided in this invention can be added to excipients or auxiliary ingredients in the cosmetics field to prepare cosmetics with anti-allergic and soothing effects, such as creams, lotions, serums, masks, toners, etc. Detailed Implementation

[0020] This invention discloses a compound anti-allergic and soothing extract. Those skilled in the art can refer to the content of this document and appropriately modify the process parameters to achieve the desired result. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and are considered to be included in this invention. The methods and applications of this invention have been described through preferred embodiments. Those skilled in the art can clearly modify or appropriately change and combine the methods and applications described herein without departing from the content, spirit, and scope of this invention to implement and apply the technology of this invention.

[0021] The raw materials and reagents used in the compound anti-allergy and soothing extract provided by this invention are commercially available.

[0022] The present invention will be further illustrated below with reference to the embodiments: Example 1 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials in parts by weight: 10 parts of Gentiana macrophylla root and 10 parts of Lonicera japonica, mix them, crush them, and pass them through a 10-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with an 80% ethanol aqueous solution at a rate of 1 BV / h to obtain 2 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 1 BV / h. After loading, the resin was washed with deionized water at a flow rate of 2 BV / h, with a elution volume of 2 BV. Subsequently, impurities were removed by elution with a 0.5 wt% citric acid aqueous solution at a flow rate of 1 BV / h, with a elution volume of 2 BV. Finally, the eluent was collected with a high-concentration ethanol aqueous solution of 85% (v / v) at a flow rate of 2 BV / h. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0023] Example 2 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials by weight: 20 parts of Gentiana macrophylla root and 1 part of Lonicera japonica, mix them, crush them, and pass them through a 50-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with a 70% (v / v) ethanol aqueous solution at a rate of 2 BV / h to obtain 1 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 2 BV / h. After loading, the resin was washed with deionized water at a flow rate of 1 BV / h, with a elution volume of 3 BV. Subsequently, impurities were removed by elution with a 0.05 wt% citric acid aqueous solution at a flow rate of 2 BV / h, with a elution volume of 1 BV. Finally, the eluent was eluted with a 95% (v / v) high-concentration ethanol aqueous solution at a flow rate of 1 BV / h, and 3 BV of eluent was collected. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0024] Comparative Example 1 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials in parts by weight: 10 parts of Gentiana macrophylla root and 10 parts of Lonicera japonica, mix them, crush them, and pass them through a 30-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with a 75% (v / v) ethanol aqueous solution at a rate of 1.5 BV / h to obtain 1.5 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 1.5 BV / h. After loading, the resin was washed with deionized water at a flow rate of 1.5 BV / h, and the eluent volume was 2.5 BV. Finally, the column was eluted with a high-concentration ethanol aqueous solution with a volume fraction of 90% at a flow rate of 1.5 BV / h, and the eluent volume was collected to 2.5 BV. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0025] Comparative Example 2 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials in parts by weight: 10 parts of Gentiana macrophylla root and 10 parts of Lonicera japonica, mix them, crush them, and pass them through a 30-mesh sieve to obtain a mixed powder; The mixed powder was put into an extraction vessel, 190 parts by weight of water was added, the mixture was heated to 50°C, stirred and extracted for 3 hours, the supernatant was extracted, and the same conditions were applied twice more. The extracts were combined and filtered, and then added to an S-8 macroporous resin column at room temperature for adsorption at a flow rate of 15 L / H. After adsorption, the resin column was washed with water until no sugar color was found, and then eluted with 60% volume fraction of ethanol to obtain 2.5 BV of eluent. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0026] Test 1 The contents of iridoid glycosides (with gentiopicroside as the main component) and alkaloids in the compound anti-allergic and soothing extracts prepared in Examples 1-2 and Comparative Examples 1-2 were determined according to the method described in the reference "Wei Xin, He Hongsheng, Wang Shu. Determination of alkaloids and gentiopicroside in Gentiana macrophylla by HPLC [J]. West China Journal of Pharmaceutical Sciences, 2006, 21(1):3.". The specific test results are shown in Table 1.

[0027] Table 1. Gentianin and alkaloid content in each test group

[0028] As shown in Table 1, the contents of iridoid glycosides and alkaloids in the composite anti-allergic and soothing extracts prepared in Examples 1-2 were higher than those in Comparative Example 1. This indicates that the present invention uses a low-concentration citric acid aqueous solution for intermediate elution, utilizing acidic conditions to protonate and elute some weakly acidic impurities, while the target components of iridoid glycosides and alkaloids remain on the resin, thereby improving the purity of the final product.

[0029] The composite anti-allergic and soothing extracts prepared in Examples 1-2 contained higher levels of iridoid glycosides and alkaloids than those in Comparative Example 2. This indicates that the present invention employs a low-temperature extraction process, which maximizes the stability of the active ingredients of Gentiana macrophylla and simultaneously enriches the anti-allergic and soothing components of iridoid glycosides and alkaloids.

[0030] Example 3 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials by weight: 15 parts of Gentiana macrophylla root and 4 parts of Lonicera japonica, mix them, crush them, and pass them through a 30-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with a 75% (v / v) ethanol aqueous solution at a rate of 1.5 BV / h to obtain 1.5 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 1.5 BV / h. After loading, the resin was washed with deionized water at a flow rate of 1.5 BV / h, with a elution volume of 2.5 BV. Subsequently, impurities were removed by elution with 0.2 wt% citric acid aqueous solution at a flow rate of 1.5 BV / h, with a elution volume of 1.5 BV. Finally, elution was carried out with a 90% (v / v) high-concentration ethanol aqueous solution at a flow rate of 1.5 BV / h, and 2.5 BV of eluent was collected. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0031] Comparative Example 3 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials by weight: 19 parts of Gentiana macrophylla root, mix, crush, and pass through a 30-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with a 75% (v / v) ethanol aqueous solution at a rate of 1.5 BV / h to obtain 1.5 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 1.5 BV / h. After loading, the resin was washed with deionized water at a flow rate of 1.5 BV / h, with a elution volume of 2.5 BV. Subsequently, impurities were removed by elution with 0.2 wt% citric acid aqueous solution at a flow rate of 1.5 BV / h, with a elution volume of 1.5 BV. Finally, elution was carried out with a 90% (v / v) high-concentration ethanol aqueous solution at a flow rate of 1.5 BV / h, and 2.5 BV of eluent was collected. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0032] Comparative Example 4 A compound anti-allergic and soothing extract is obtained by the following preparation method: Weigh the following raw materials by weight: 19 parts of honeysuckle, mix, crush, and pass through a 30-mesh sieve to obtain a mixed powder; The mixed powder was packed into a chromatography column and compacted to form a mixed powder packed column; it was eluted with a 75% (v / v) ethanol aqueous solution at a rate of 1.5 BV / h to obtain 1.5 BV of eluent. The eluent was concentrated by rotary evaporation to less than 1 / 10 of its original volume to obtain a concentrated solution. The concentrated solution was loaded onto a chromatography column packed with AB-8 macroporous resin at a flow rate of 1.5 BV / h. After loading, the resin was washed with deionized water at a flow rate of 1.5 BV / h, with a elution volume of 2.5 BV. Subsequently, impurities were removed by elution with 0.2 wt% citric acid aqueous solution at a flow rate of 1.5 BV / h, with a elution volume of 1.5 BV. Finally, elution was carried out with a 90% (v / v) high-concentration ethanol aqueous solution at a flow rate of 1.5 BV / h, and 2.5 BV of eluent was collected. The ethanol was removed by rotary evaporation of the eluent to obtain the compound anti-allergic and soothing extract.

[0033] Test 2 The composite anti-inflammatory and soothing extracts prepared in Example 3 and Comparative Examples 3-4 were tested according to the in vitro anti-inflammatory evaluation method described in Chinese Patent CN 113855599 B. IL-6 was used as the target inflammatory factor, and the detection method was ELISA kit. The results are shown in Table 2.

[0034] Table 2 Comparison of IL-6 differences among test groups The # symbol indicates that the difference was statistically significant compared with the negative control group (NT) (p<0.05). The asterisk (*) indicates that the difference is statistically significant compared with the model control group (M) (p<0.05). As shown in Table 2, the relative content of IL-6 in Example 3 was significantly lower than that in the model control group, indicating that the prepared compound anti-allergic and soothing extract has significant anti-inflammatory and soothing abilities. The relative content of IL-6 in Example 3 was significantly lower than that in Comparative Examples 3-4, showing better anti-inflammatory and soothing abilities. This suggests that the combined use of Gentiana macrophylla and Lonicera japonica has a better effect.

[0035] Example 4 A soothing serum comprising the following components in percentage by weight: 5% glycerin, 3% butylene glycol, 0.5% p-hydroxyacetophenone, 0.15% xanthan gum, 0.5% betaine, 0.2% inositol, 0.05% sodium hyaluronate, 0.05% hydrolyzed hyaluronic acid, 5% of the compound anti-allergic and soothing extract prepared in Example 3, and the balance being water.

[0036] Example 5 A soothing serum comprising the following components in percentage by weight: Glycerin 5%, Butylene Glycol 5%, Xanthan Gum 0.1%, Carbomer 0.2%, Methylparaben 0.2%, p-hydroxyacetophenone 0.5%, Phytosterol Oleate 0.5%, Diethylhexyl Carbonate 3%, Polydimethylsiloxane 2%, Beeswax 0.5%, Cetearyl Alcohol 1.5%, Cetearyl Glucoside 1%, Glyceryl Stearate 0.5%, Hydrogenated Lecithin 0.1%, Arginine 0.2%, The Compound Anti-allergic and Soothing Extract Prepared in Example 2 5%, Water balance.

[0037] Test 3 Twenty female volunteers who self-reported as having sensitive skin were recruited and used the soothing essence from Example 4 and the soothing serum from Example 5 in combination. After cleansing, an appropriate amount of the soothing essence was applied to the face and gently patted until absorbed. Then, an appropriate amount of the soothing serum was applied to the face and gently massaged in circular motions until fully absorbed. This was done twice a day, morning and evening. A follow-up four weeks later revealed that all volunteers reported relief from their sensitive skin condition. Seventeen volunteers reported significant relief from facial itching and redness, resulting in a significant efficacy rate exceeding 85%.

[0038] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A compound anti-allergic and soothing extract, characterized in that, It is obtained through the following preparation method: (A) Weigh the following raw materials in parts by weight: 10-20 parts of Gentiana macrophylla root and 1-10 parts of Lonicera japonica, mix them, crush them, and pass them through a 10-50 mesh sieve to obtain a mixed powder; (B) The mixed powder is packed into a chromatography column and compacted to form a mixed powder packed column; it is then eluted with an aqueous ethanol solution to obtain the eluent. (C) The eluent is concentrated by rotary evaporation to obtain a concentrate; the concentrate is loaded onto a chromatography column packed with AB-8 macroporous resin. After the sample loading is completed, the resin is rinsed with deionized water, then eluted with citric acid aqueous solution to remove impurities, and finally eluted with high concentration ethanol aqueous solution and the eluent is collected. (D) The eluent is rotary evaporated to remove ethanol, thus obtaining the compound anti-allergic and soothing extract.

2. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The weight parts of each raw material in step (A) are: 15 parts of Gentiana macrophylla root and 4 parts of Lonicera japonica.

3. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The volume fraction of the ethanol-water solution in step (B) is 70-80%; the elution rate of the ethanol-water solution is 1-2 BV / h, and the collected eluent is 1-2 BV.

4. The compound anti-allergic and soothing extract according to claim 1, characterized in that, In step (C), the eluent is concentrated by rotary evaporation to less than 1 / 10 of its original volume.

5. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The loading rate of the concentrate in step (C) is 1-2 BV / h.

6. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The deionized water rinsing rate in step (C) is 1-2 BV / h, and the deionized water elution volume is 2-3 BV.

7. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The elution rate of the citric acid aqueous solution in step (C) is 1-2 BV / h, the concentration of the citric acid aqueous solution is 0.05-0.5 wt%, and the elution volume of the citric acid aqueous solution is 1-2 BV.

8. The compound anti-allergic and soothing extract according to claim 1, characterized in that, The elution rate of the high-concentration ethanol aqueous solution in step (C) is 1-2 BV / h; the volume fraction of the high-concentration ethanol aqueous solution is 85-95%; and the elution volume of the high-concentration ethanol aqueous solution is 2-3 BV.

9. The use of the compound anti-allergic and soothing extract according to any one of claims 1-8 in the preparation of cosmetics with anti-allergic and soothing effects.

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