Preparation method of a composite extract of gavvia, the composite extract and application thereof
By combining liquid nitrogen freezing and microwave treatment with a high proportion of solvent in the kava composite extraction technology, the problem of easy oxidation of kava extract has been solved, achieving efficient extraction and long-lasting and stable anti-inflammatory and analgesic effects.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- GUANGZHOU JIANENG BIOTECHNOLOGY CO LTD
- Filing Date
- 2022-04-22
- Publication Date
- 2026-06-19
AI Technical Summary
Kava extract is prone to oxidation and discoloration in traditional preparation processes, which leads to a decrease in the content of active ingredients and the generation of new irritants, and the extraction rate is low.
A combined cell wall disruption and extraction technology was adopted, which reduced oxidation through the synergistic effect of liquid nitrogen freezing, microwave treatment and high proportion of solvent, and combined with the extract of Opuntia ficus-indica leaf to prepare a Kava composite extract.
It improved the stability and extraction rate of kava complex extract, extended its shelf life, enhanced its anti-inflammatory and analgesic effects, and reduced the generation of new irritants.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of plant extracts, and in particular to a kava complex extract, its preparation method, and its application. Background Technology
[0002] The roots, stems, and fresh leaves of kava pepper have excellent medicinal value, with anti-inflammatory, antibacterial, insecticidal, antispasmodic, and local anesthetic effects. In addition, it can also treat convulsions, asthma, anxiety, and depression. It also has significant effects on promoting sleep and improving sleep quality, with few toxic side effects.
[0003] In the field of daily chemical products, kava extract is mainly used as a plant-derived active ingredient that soothes nerve conduction. By non-specifically regulating GABA receptors, it causes neurons to hyperpolarize or depolarize, which can quickly relieve itching and pain caused by various skin discomforts. It also has a good soothing and anti-inflammatory effect.
[0004] Kava's main active ingredients are unsaturated lactones, such as capsaicin, methylenedioxycapsaicin, demethoxymethoxycapsaicin, methoxycapsaicin, dihydrocapsaicin, and methylenedioxydihydrocapsaicin.
[0005] However, the aforementioned components are easily oxidized and deactivated, discolored, and can become irritants. Traditional kava preparation processes involve high temperatures or sterilization, which easily leads to oxidation, causing discoloration, reduced content, and the resulting oxidation products becoming new irritants. Therefore, there is still room for improvement. Summary of the Invention
[0006] To reduce the oxidation of calvalactone, this application provides a method for preparing a calva complex extract, the complex extract, and its applications.
[0007] In a first aspect, this application provides a method for preparing a kava complex extract, employing the following technical solution:
[0008] A method for preparing a kava complex extract includes the following steps:
[0009] Step 1), prepare the leaf extract of Opuntia ficus-indica;
[0010] Step 2), preparing kava root extract, specifically including:
[0011] Step 2-1): Crush the kava pepper root, add solvent, and stir for 0.5-1 h to form a first mixture. The mass of the solvent is 3-4 times that of the kava pepper root.
[0012] Step 2-2): Centrifuge the first mixture to separate the centrifuged liquid from the drug residue. Add purified water to the drug residue and stir for 0.5-1 h to form the second mixture. The mass of the purified water is 3-4 times the mass of the drug residue.
[0013] Steps 2-3): Centrifuge the second mixture, collect the residue, and freeze the residue with liquid nitrogen;
[0014] Steps 2-4): Melt the frozen medicinal residue at room temperature, and then microwave the residue for 60-80 seconds.
[0015] Steps 2-5): Cool the residue to 0-20°C with liquid nitrogen, then add the centrifuged liquid obtained in step 2-2) to the residue to form a third mixture, and treat the third mixture with microwave for 60-80 seconds.
[0016] Steps 2-6): Add solvent to the third mixture so that the total mass of solvent and centrifuged liquid is 5-9 times the mass of the residue, stir and extract to obtain the fourth mixture;
[0017] Steps 2-7): Centrifuge, age, centrifuge again, filter, and collect the filtrate to obtain Kava pepper root extract;
[0018] Step 3) Add prickly pear leaf extract to kava pepper root extract and stir to obtain kava complex extract.
[0019] By adopting the above technical solution and using special preparation techniques, the oxidation of kavalactone is reduced, making it less prone to discoloration and content reduction. It is also less likely to generate oxidation products that could form new irritants. Furthermore, by combining it with cactus extract, not only is a synergistic effect on efficacy achieved, but the shelf-life stability of kavalactone is also enhanced, resulting in a longer and more stable shelf life for the kavalactone complex extract.
[0020] Kava root cells have strong fibers, high starch content, and contain some plant oil, making them prone to aggregation. Traditional cell disruption pretreatment methods can lead to clumping, heat generation, and oxidation of active ingredients. However, without cell disruption, solvents do not easily penetrate at room temperature, resulting in low extraction rates. The above-mentioned technical solution employs a combined cell disruption and simultaneous extraction method to achieve efficient extraction while preventing oxidation of active ingredients. Solvents are added sequentially for dehydration and displacement, creating a high intracellular osmotic pressure. Water is then added to rapidly swell the cells to a taut state. Rapid freezing with liquid nitrogen turns the intracellular water into ice, partially breaking down the cell walls. Microwave treatment further expands the existing cell fragmentation area due to the increased intracellular pressure. The solvent also has a certain desorption effect on active ingredients during internal microwave treatment, allowing for efficient subsequent room-temperature extraction. Since the entire process takes less than 3 minutes to heat, and the rapid heating and cooling effectively protect the active ingredients, the resulting kava complex extract is of high quality.
[0021] Through the synergistic effect of cell wall disruption and high proportion of solvents, sterilization is achieved at room temperature, making the active ingredients less prone to oxidation, inactivation, discoloration, and the generation of new irritants.
[0022] Preferably, in steps 2-1) and 2-6), the solvent is polyethylene glycol-8 or a mixture of 1,2-pentanediol and 1,3-butanediol, and the mass ratio of 1,2-pentanediol to 1,3-butanediol is (1-2):(1-2).
[0023] By adopting the above technical solution and specifically selecting the solvent, the sterilization effect is better, the desorption effect on active substances is better, and the extraction effect is better.
[0024] Preferably, in steps 2-3), the dregs are frozen with liquid nitrogen for 30-35 minutes.
[0025] By adopting the above technical solution and specifically selecting the freezing time, the water in the cells is fully frozen, which has a better effect on destroying the cell wall and ensures better extraction efficiency.
[0026] Preferably, in steps 2-4), the microwave frequency during microwave processing is 2400-2500MHz.
[0027] By adopting the above technical solution and using a specific microwave frequency, the cell wall is better destroyed, the active substances are better extracted, and the active substances are not easily damaged, resulting in better quality extracts.
[0028] Preferably, in steps 2-5), the microwave frequency during microwave processing is 2400-2500MHz.
[0029] By adopting the above technical solution, and through two microwave treatments with specific microwave frequencies selected for homopolymer polyurethane, the cell wall breaking effect is better and more thorough, making it easier to extract the active ingredients completely, increasing the content of active ingredients in the extract, and thus improving the quality of the extract.
[0030] Preferably, step 1) specifically includes:
[0031] Step 1-1): Mix the leaves of the prickly pear cactus with water and extract at 85-90℃ to obtain an extract. The mass of the water is 10-12 times the mass of the prickly pear cactus leaves.
[0032] Steps 1-2): Add chitosan to the extract for flocculation, stir, let stand, centrifuge, and collect the centrifuged liquid;
[0033] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1-1.5 g / ml to obtain a concentrated solution;
[0034] Steps 1-4): The concentrated solution is adsorbed through an adsorption column and then eluted with a solution to obtain the eluent.
[0035] Steps 1-5): Add alumina powder to the eluent, stir, filter, take the filtrate, concentrate the filtrate to a crude drug ratio of 1.5-2 g / ml, and obtain the prickly pear cactus leaf extract. The mass of alumina powder added is consistent with the mass of prickly pear cactus leaves in step 1-1).
[0036] By adopting the above technical solution, the active ingredient content of the prickly pear leaf extract was high and the quality was good. The synergistic effect of the extract combined with the kava root extract was better, and the quality of the resulting compound extract was even better.
[0037] Preferably, in steps 1-4), the elution solution is an ethanol solution with a concentration of 50% and a volume of ethanol solution that is 3-4 times the column volume.
[0038] By adopting the above technical solution and specifically selecting the elution solution, the elution effect is more thorough, reducing the waste of active substances and having higher economic value.
[0039] Preferably, the adsorption column is a macroporous resin column.
[0040] By adopting the above technical solution and specifically selecting macroporous resin columns, the adsorption effect is better, impurities are effectively reduced, and the subsequent eluent is purer and of better quality.
[0041] Secondly, this application provides a kava complex extract, which adopts the following technical solution:
[0042] A kava compound extract, comprising kava root extract and prickly pear leaf extract, wherein the mass ratio of kava root extract to prickly pear leaf extract is (3-4):1.
[0043] By adopting the above technical solution, the anti-inflammatory and analgesic effects are better when kava pepper root extract and prickly pear leaf extract are combined in a specific ratio, and the kava compound extract has a longer shelf life and is more stable.
[0044] Thirdly, this application provides an application of a kava complex extract, employing the following technical solution:
[0045] An application of a kava complex extract, added to skincare products at a concentration of 0.5%-5%.
[0046] By adopting the above technical solution and adding kava compound extract to skin care products, the skin care products have better analgesic and anti-inflammatory effects and better skin repair effects.
[0047] Skincare products can be conventional skincare products in this field, such as toners, lotions, serums, etc.
[0048] In summary, this application has the following beneficial effects:
[0049] 1. Because this application uses a special preparation technology, it reduces the oxidation of kavalactone, making it less prone to discoloration and content reduction. It is also less likely to generate oxidation products that could form new irritants. Furthermore, by combining it with cactus extract, it not only produces a synergistic effect in efficacy but also enhances the shelf-life stability of the active ingredients in kavalactone, resulting in a longer and more stable shelf life for the kavalactone complex extract.
[0050] 2. In this application, kava root extract and prickly pear leaf extract are preferably combined in a specific ratio, which has a better anti-inflammatory and analgesic effect, and the kava compound extract has a longer shelf life and is more stable. Detailed Implementation
[0051] The present application will be further described in detail below with reference to the embodiments.
[0052] Example 1
[0053] A method for preparing a kava complex extract includes the following steps:
[0054] Step 1), preparing the leaf extract of Opuntia ficus-indica, specifically including:
[0055] Step 1-1): Mix 150g of prickly pear leaf slices with water and extract at 90℃ using external circulation for 2 hours to obtain the extract. The mass of water should be 10 times the mass of the prickly pear leaf.
[0056] Steps 1-2): Add chitosan to the extract for flocculation, stir at room temperature for 0.5 h, let stand for 2 h, centrifuge until clear, and take the centrifuged liquid. The mass of chitosan added is 0.05% of the mass of the extract.
[0057] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1g / ml, thus obtaining 150ml of concentrated liquid.
[0058] Steps 1-4) The concentrate is adsorbed through a D101 macroporous resin column and then eluted with 3 column volumes of 50% ethanol to obtain the eluent.
[0059] Steps 1-5): Add 100g of alumina powder to the eluent, stir at room temperature for 1 hour, filter through a filter screen, collect the filtrate, and concentrate the filtrate under reduced pressure at a vacuum degree of 0.08MPa to a crude drug ratio of 1.5g / ml, thus obtaining 100ml of Opuntia ficus-indica leaf extract filtrate.
[0060] Step 2), preparing kava root extract, specifically including:
[0061] Step 2-1): Crush 100g of kava pepper root to 40 mesh, add 4 times the weight of kava pepper root in solvent (polyethylene glycol-8), stir for 1 hour to form the first mixture.
[0062] Step 2-2): Centrifuge the first mixture at 2000 rpm for 15 min to separate the centrifuged liquid from the drug residue. Add purified water at 4 times the mass of the drug residue to the drug residue and stir for 1 h to form the second mixture.
[0063] Steps 2-3): Centrifuge the second mixture at 2000 rpm for 15 minutes, collect the residue, and freeze the residue with liquid nitrogen for 30 minutes.
[0064] Steps 2-4): Melt the frozen medicinal residue at room temperature. After melting, microwave the residue for 80 seconds at a frequency of 2450MHz.
[0065] Steps 2-5): Cool the residue to 20°C using liquid nitrogen, then add the centrifuged liquid obtained in step 2-2) to the residue to form a third mixture. Treat the third mixture with microwave for 60 seconds at a frequency of 2450MHz.
[0066] Steps 2-6): Add solvent, polyethylene glycol-8, to the third mixture, so that the total mass of the solvent and the centrifuged liquid is 9 times the mass of the residue. Stir and extract at room temperature for 2 hours to obtain the fourth mixture.
[0067] Steps 2-7): Centrifuge the fourth mixture at 2000 rpm for 15 min, then age it at 4°C for 48 h, then centrifuge it at 18000 rpm for 20 min, and then ultrafilter it through a 100 nm ceramic membrane at 3 bar. Collect the filtrate to obtain the Kava pepper root extract filtrate.
[0068] Step 3): Take 75g of Kava root extract filtrate and 25g of Opuntia ficus-indica leaf extract filtrate, add polyethylene glycol-8 until the total content of Kava root extract and Opuntia ficus-indica leaf extract in the solution is 4%, stir until clear, and obtain Kava complex extract.
[0069] Example 2
[0070] A method for preparing a kava complex extract includes the following steps:
[0071] Step 1), preparing the leaf extract of Opuntia ficus-indica, specifically including:
[0072] Step 1-1): Mix 150g of prickly pear leaf slices with water and extract at 85℃ using external circulation for 2.5h to obtain the extract. The mass of water is 12 times the mass of the prickly pear leaf.
[0073] Steps 1-2): Add chitosan to the extract for flocculation, stir at room temperature for 1 hour, let stand for 2.5 hours, centrifuge until clear, and take the centrifuged liquid. The mass of chitosan added is 0.05% of the mass of the extract.
[0074] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1.5 g / ml to obtain 100 ml of concentrate.
[0075] Steps 1-4) The concentrate is adsorbed through a D101 macroporous resin column and then eluted with 4 column volumes of 50% ethanol to obtain the eluent.
[0076] Steps 1-5): Add 150g of alumina powder to the eluent, stir at room temperature for 1.5h, filter through a filter screen, collect the filtrate, and concentrate the filtrate under reduced pressure at a vacuum degree of 0.09MPa to a crude drug ratio of 2g / ml, thus obtaining 75ml of Opuntia ficus-indica leaf extract filtrate.
[0077] Step 2), preparing kava root extract, specifically including:
[0078] Step 2-1): Crush 100g of kava pepper root to 100 mesh, add solvent of 3 times the mass of kava pepper root, the solvent is composed of 1,2-pentanediol and 1,3-butanediol in a mass ratio of 2:1, stir for 0.5h to form the first mixture.
[0079] Step 2-2): Centrifuge the first mixture at 2000 rpm for 15 min to separate the centrifuged liquid from the drug residue. Add purified water at 3 times the mass of the drug residue to the drug residue and stir for 0.5 h to form the second mixture.
[0080] Steps 2-3): Centrifuge the second mixture at 2000 rpm for 15 minutes, collect the residue, and freeze the residue with liquid nitrogen for 35 minutes.
[0081] Steps 2-4): Melt the frozen medicinal residue at room temperature. After melting, microwave the residue for 60 seconds at a frequency of 2400MHz.
[0082] Steps 2-5): Cool the residue to 10°C using liquid nitrogen, then add the centrifuged liquid obtained in step 2-2) to the residue to form a third mixture. Treat the third mixture with microwave for 80 seconds at a frequency of 2400MHz.
[0083] Steps 2-6): Add solvent to the third mixture. The solvent consists of 1,2-pentanediol and 1,3-butanediol in a mass ratio of 2:1, so that the total mass of the solvent and the centrifuged liquid is 5 times the mass of the residue. Stir and extract at room temperature for 2.5 hours to obtain the fourth mixture.
[0084] Steps 2-7): Centrifuge the fourth mixture at 2000 rpm for 15 min, then age it at 2°C for 48 h, then centrifuge it at 18000 rpm for 20 min, and then ultrafilter it through a 100 nm ceramic membrane at 4 bar. Collect the filtrate to obtain the Kava pepper root extract filtrate.
[0085] Step 3): Take 80g of Kava root extract filtrate and 20g of Opuntia ficus-indica leaf extract filtrate, add 1,2-pentanediol and 1,3-butanediol mixed solvent until the total content of Kava root extract and Opuntia ficus-indica leaf extract in the solution is 2.5%, stir until clear, and obtain Kava complex extract.
[0086] Example 3
[0087] A method for preparing a kava complex extract includes the following steps:
[0088] Step 1), preparing the leaf extract of Opuntia ficus-indica, specifically including:
[0089] Step 1-1): Mix 180g of prickly pear leaf slices with water and extract at 88℃ using external circulation for 2 hours to obtain the extract. The mass of water is 11 times the mass of the prickly pear leaf.
[0090] Steps 1-2): Add chitosan to the extract for flocculation, stir at room temperature for 0.5 h, let stand for 2 h, centrifuge until clear, and take the centrifuged liquid. The mass of chitosan added is 0.05% of the mass of the extract.
[0091] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1.2 g / ml, thus obtaining 150 ml of concentrate.
[0092] Steps 1-4) The concentrate is adsorbed through a D101 macroporous resin column and then eluted with 3.5 column volumes of 50% ethanol to obtain the eluent.
[0093] Steps 1-5): Add 180g of alumina powder to the eluent, stir at room temperature for 1 hour, filter through a filter screen, collect the filtrate, and concentrate the filtrate under reduced pressure at a vacuum degree of 0.08MPa to a crude drug ratio of 1.8g / ml, thus obtaining 100ml of Opuntia ficus-indica leaf extract filtrate.
[0094] Step 2), preparing kava root extract, specifically including:
[0095] Step 2-1): Crush 100g of kava pepper root to 80 mesh, add 3.5 times the mass of kava pepper root in solvent, the solvent being composed of 1,2-pentanediol and 1,3-butanediol in a mass ratio of 1:2, stir for 0.75h to form the first mixture.
[0096] Step 2-2): Centrifuge the first mixture at 2000 rpm for 15 min to separate the centrifuged liquid from the residue. Add 3.5 times the mass of purified water to the residue and stir for 0.75 h to form the second mixture.
[0097] Steps 2-3): Centrifuge the second mixture at 2000 rpm for 15 minutes, collect the residue, and freeze the residue with liquid nitrogen for 30 minutes.
[0098] Steps 2-4): Melt the frozen medicinal residue at room temperature. After melting, microwave the residue for 70 seconds at a frequency of 2500MHz.
[0099] Steps 2-5): Cool the residue to 0°C using liquid nitrogen, then add the centrifuged liquid obtained in step 2-2) to the residue to form a third mixture. Treat the third mixture with microwave for 70 seconds at a microwave frequency of 2500MHz.
[0100] Steps 2-6): Add solvent to the third mixture. The solvent consists of 1,2-pentanediol and 1,3-butanediol in a mass ratio of 1:2, so that the total mass of the solvent and the centrifuged liquid is 7 times the mass of the residue. Stir and extract at room temperature for 2 hours to obtain the fourth mixture.
[0101] Steps 2-7): Centrifuge the fourth mixture at 2000 rpm for 15 min, then age it at 0°C for 48 h, then centrifuge it at 18000 rpm for 20 min, and then ultrafilter it through a 100 nm ceramic membrane at 4 bar. Collect the filtrate to obtain the Kava pepper root extract filtrate.
[0102] Step 3): Take 77.5g of Kava root extract filtrate and 22.5g of Opuntia ficus-indica leaf extract filtrate, add 1,2-pentanediol and 1,3-butanediol mixed solvent until the total content of Kava root extract and Opuntia ficus-indica leaf extract in the solution is 3.2%, stir until clear, and obtain Kava complex extract.
[0103] Comparative Example 1
[0104] A method for preparing a kava complex extract, which differs from Example 1 only in that:
[0105] In step 3), 70g of pepper root extract filtrate and 30g of prickly pear leaf extract filtrate are mixed.
[0106] Comparative Example 2
[0107] A method for preparing a kava complex extract, which differs from Example 1 only in that:
[0108] In step 3), 85g of pepper root extract filtrate and 15g of prickly pear leaf extract filtrate are mixed.
[0109] Comparative Example 3
[0110] A method for preparing a kava complex extract includes the following steps:
[0111] Step 1), preparing the leaf extract of Opuntia ficus-indica, specifically including:
[0112] Step 1-1): Mix 150g of prickly pear leaf slices with water and extract at 90℃ using external circulation for 2 hours to obtain the extract. The mass of water should be 10 times the mass of the prickly pear leaf.
[0113] Steps 1-2): Add chitosan to the extract for flocculation, stir at room temperature for 0.5 h, let stand for 2 h, centrifuge until clear, and take the centrifuged liquid. The mass of chitosan added is 0.05% of the mass of the extract.
[0114] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1g / ml, thus obtaining 150ml of concentrated liquid.
[0115] Steps 1-4) The concentrate is adsorbed through a D101 macroporous resin column and then eluted with 3 column volumes of 50% ethanol to obtain the eluent.
[0116] Steps 1-5): Add 100g of alumina powder to the eluent, stir at room temperature for 1 hour, filter through a filter screen, collect the filtrate, and concentrate the filtrate under reduced pressure at a vacuum degree of 0.08MPa to a crude drug ratio of 1.5g / ml, thus obtaining 100ml of Opuntia ficus-indica leaf extract filtrate.
[0117] Step 2), preparing kava root extract, specifically including:
[0118] Step 2-1): Crush 100g of kava root to 40 mesh, add solvent equal to 9 times the weight of kava root, and stir at 85°C for 1 hour to form the first mixture.
[0119] Step 2-2): Centrifuge the first mixture at 2000 rpm for 15 min, collect the centrifuged liquid, age the centrifuged liquid at 4°C for 48 h, then centrifuge at 18000 rpm for 20 min, and ultrafilter it through a 100 nm ceramic membrane at 3 bar. Collect the filtrate to obtain the Kava pepper root extract filtrate.
[0120] Step 3): Take 75g of Kava root extract filtrate and 25g of Opuntia ficus-indica leaf extract filtrate, add polyethylene glycol-8 until the total content of Kava root extract and Opuntia ficus-indica leaf extract in the solution is 4%, stir until clear, and obtain Kava complex extract.
[0121] Comparative Example 4
[0122] A method for preparing a kava complex extract includes the following steps:
[0123] Step 1), preparing the leaf extract of Opuntia ficus-indica, specifically including:
[0124] Step 1-1): Mix 150g of prickly pear leaf slices with water and extract at 90℃ using external circulation for 2 hours to obtain the extract. The mass of water should be 10 times the mass of the prickly pear leaf.
[0125] Steps 1-2): Add chitosan to the extract for flocculation, stir at room temperature for 0.5 h, let stand for 2 h, centrifuge until clear, and take the centrifuged liquid. The mass of chitosan added is 0.05% of the mass of the extract.
[0126] Steps 1-3) Concentrate the centrifuged liquid to a crude drug ratio of 1g / ml, thus obtaining 150ml of concentrated liquid.
[0127] Steps 1-4) The concentrate is adsorbed through a D101 macroporous resin column and then eluted with 3 column volumes of 50% ethanol to obtain the eluent.
[0128] Steps 1-5): Add 100g of alumina powder to the eluent, stir at room temperature for 1 hour, filter through a filter screen, collect the filtrate, and concentrate the filtrate under reduced pressure at a vacuum degree of 0.08MPa to a crude drug ratio of 1.5g / ml, thus obtaining 100ml of Opuntia ficus-indica leaf extract filtrate.
[0129] Step 2), preparing kava root extract, specifically including:
[0130] Step 2-1): Crush 100g of kava root to 40 mesh, add solvent equal to 9 times the weight of kava root, stir and extract at room temperature for 1 hour to form the first mixture.
[0131] Step 2-2): Centrifuge the first mixture at 2000 rpm for 15 min, collect the centrifuged liquid, age the centrifuged liquid at 4°C for 48 h, then centrifuge at 18000 rpm for 20 min, and ultrafilter it through a 100 nm ceramic membrane at 3 bar. Collect the filtrate to obtain the Kava pepper root extract filtrate.
[0132] Step 3): Take 75g of Kava root extract filtrate and 25g of Opuntia ficus-indica leaf extract filtrate, add polyethylene glycol-8 until the total content of Kava root extract and Opuntia ficus-indica leaf extract in the solution is 4%, stir until clear, and obtain Kava complex extract.
[0133] Experiment 1
[0134] Stability test (d): The longest time under various conditions of 4℃, 48℃, room temperature and light irradiation for the test sample to show no serious discoloration, no visible precipitation, and a decrease of ≤10% in capsaicin content.
[0135] Experiment 2
[0136] Detection method for capsaicin: Column: WONDASIL C18 SUPERB 5UM 4.6MM×150MM; Mobile phase: 0.1% phosphoric acid water-acetonitrile-isopropanol (60:22:18, V / V / V); Flow rate: 1mL / min; Detection wavelength: 220nm; Column temperature: 25℃; Time: 30min.
[0137] Capsaicin extraction rate = Capsaicin extraction mass ÷ Theoretical mass of capsaicin in medicinal material × 100%.
[0138] Capsaicin residue rate in medicinal residue = mass of capsaicin residue in medicinal residue ÷ theoretical mass of capsaicin in medicinal material × 100%.
[0139] Theoretical mass of capsaicin in medicinal materials: The medicinal materials were pulverized into 80-mesh powder, 30 times the amount of 50% ethanol solution was added, and ultrasonic extraction was performed for 30 minutes. The residue was filtered. The above extraction was repeated 3 times, and the extracts from the 4 extractions were combined to test the capsaicin content.
[0140] Capsaicin residue in medicinal residue: The medicinal material was filtered until no water dripped, 30 times the amount of 50% ethanol solution was added, and ultrasonic extraction was performed for 30 minutes. The residue was then filtered. The above extraction was repeated 3 times, and the 4 extracts were combined to test the capsaicin content.
[0141] Oxidation rate of capsaicin = (Theoretical mass of capsaicin in medicinal materials - Extracted mass of capsaicin - Residual mass of capsaicin in medicinal residue - Residual mass of capsaicin in ultrafiltration retentate) × 100%.
[0142] Experiment 3
[0143] Chicken embryo test: SNT2329-2009-Cosmetic eye irritation-corrosive chicken embryo chorioallantoic membrane test, IS<1 is non-irritating; 1≤IS<5 is mild irritation; 5≤IS<9 is moderate irritation.
[0144] Experiment 4
[0145] Antipruritic experiment: KM mice were randomly divided into three groups of 10 each, half male and half female. The groups included a model group, a compound dexamethasone acetate cream group, and a 0.2% sample group. The administration method was 0.2g / mouse. Hair was removed from the backs of the mice. The mice were administered the medication continuously for 5 days. One hour after the last administration, 0.02% dextran was injected via the tail vein. Various pruritus indicators were recorded.
[0146] Itching inhibition rate (%) = (number of scratches in the model group - number of scratches in the sample group) ÷ number of scratches in the model group × 100%.
[0147] Experiment 5
[0148] Pain relief experiment: KM mice were randomly divided into three groups of 10 each, half male and half female. The groups included a model group, a 1% naproxen injection group, and a 5% sample group. The administration method was 0.2g / mouse. Hair was removed from the backs of the mice. After 7 consecutive days of administration, 160ppm capsaicin was injected into the sole of the right paw to induce pain 1 hour after the last administration. Pain indicators were then statistically analyzed.
[0149] Pain suppression rate (%) = (Number of times the model group rubbed claws - Number of times the sample group rubbed claws) ÷ Number of times the model group rubbed claws × 100%.
[0150] Experiment 6
[0151] Anti-inflammatory experiment: KM mice were randomly divided into groups of 10 each, half male and half female. The groups included a control group, a model group, a dexamethasone sodium phosphate injection group, and a 2% sample group. The administration method was 0.2 g / mouse. After 15 consecutive days of administration, delayed-type anaphylaxis was induced in mice using 1-chloro-2,4-dinitrotoluene (DNCB). Sensitization was achieved on the back of the mice once each on days 1 and 2 with 7% DNCB / 50 μl. Provocation was performed on days 6 and 8 with 0.5% DNCB / 25 μl, and on days 10, 12, and 14 with 1% DNCB / 50 μl. At the end of the experiment, the mice were anesthetized (with 5% chloral hydrate) and injected with luminol sodium salt for 10 minutes before in vivo imaging to assess the intensity of inflammation. The intensity of inflammation in the model group was recorded as 100%.
[0152] The specific test data for Experiments 1-6 are detailed in Tables 1 and 2.
[0153] Table 1
[0154]
[0155]
[0156] Table 2
[0157]
[0158] The extraction rate data of capsaicin can be compared to show that the extraction rate of the technical solution of the present invention (Examples 1-3) is much higher than that of the traditional method (Comparative Examples 3 and 4).
[0159] Based on the oxidation rate, extract color, and safety data (chicken embryo experiment) of capsaicin, it can be seen that the traditional high-temperature extraction process (Comparative Example 3) results in significant loss of capsaicin and produces additional irritation.
[0160] As can be seen from the stability test time and the data in Table 2, the specific formulation of the present invention (Examples 1-3) effectively increased the stability of kava extract, enhanced its antipruritic, analgesic, and anti-inflammatory effects, and was significantly superior to the non-specific formulation (Comparative Examples 1 and 2).
[0161] Application Example 1
[0162] A Kava analgesic spray comprises: 0.02g sodium hyaluronate, 3g glycerin, 0.1g allantoin, 0.15g methylparaben, 0.8g polysorbate-20, 1.5g polyethylene glycol-8, 0.5g Kava complex extract, 0.2g panthenol, 0.5g 1,2-hexanediol, and 93.23g deionized water.
[0163] The kava complex extract used was the kava complex extract from Example 1.
[0164] Preparation method of Kava analgesic spray: Add deionized water to the main pot, then add sodium hyaluronate, glycerin, allantoin and methylparaben in sequence, stir and heat to 85℃, keep warm for 20 minutes, cool down to 45℃, add polysorbate-20, polyethylene glycol-8, Kava complex extract, panthenol and 1,2-hexanediol, stir until dissolved and uniform, and obtain Kava analgesic spray.
[0165] Apply Kava pain relief spray to the affected area, and the pain will be significantly reduced in about 5 minutes.
[0166] Application Example 2
[0167] A kava analgesic essence comprises: 0.02g acrylate / C10-30 alkanol acrylate crosspolymer, 5g glycerin, 0.06g xanthan gum, 0.1g sodium hyaluronate, 0.25g allantoin, 0.15g methylparaben, 0.4g 10% NaOH aqueous solution, 1.6g polysorbate-20, 3g polyethylene glycol-8, 1g kava complex extract, 0.5g PE9010 (phenoxyethanol, ethylhexylglycerin), 0.2g panthenol, 0.25g HRE40 (PEG-40 hydrogenated castor oil), 0.01g (daily use) fragrance, and 87.2g deionized water.
[0168] The kava complex extract used was the kava complex extract from Example 1.
[0169] Apply Kava Pain Relief Essence to the affected area. After about 5 minutes, the pain will be significantly reduced.
[0170] Application Example 3
[0171] A Kava analgesic and repairing lotion comprises: 0.1g sodium hyaluronate, 7g glycerin, 0.2g allantoin, 0.15g methylparaben, 7g caprylic / capric triglyceride, 2g A165 (glyceryl stearate, PEG-100 glyceryl stearate), 1g cetearyl alcohol, 3g squalane, 0.9g hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 2g 1503 (cyclopentamethoxysiloxane, polydimethylsiloxane crosspolymer), 5g Kava complex extract, 0.5g panthenol, 0.1g (daily use) fragrance, 0.6g PE9010 (phenoxyethanol, ethylhexylglycerin), and 70.45g deionized water.
[0172] The kava complex extract used was the kava complex extract from Example 1.
[0173] Apply Kava Pain Relief Lotion to the affected area. After about 5 minutes, the pain will be significantly reduced.
[0174] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.
Claims
1. A method for preparing a kava complex extract with antipruritic, analgesic, and anti-inflammatory properties, characterized in that: Includes the following steps: Step 1), prepare the leaf extract of Opuntia ficus-indica; Step 2), preparing kava root extract, specifically includes: Step 2-1): Crush the kava pepper root, add solvent, and stir for 0.5-1 h to form a first mixture. The mass of the solvent is 3-4 times that of the kava pepper root. Step 2-2): Centrifuge the first mixture to separate the centrifuged liquid from the drug residue. Add purified water to the drug residue and stir for 0.5-1 h to form the second mixture. The mass of the purified water is 3-4 times the mass of the drug residue. Steps 2-3): Centrifuge the second mixture, collect the residue, and freeze the residue with liquid nitrogen; Steps 2-4): Melt the frozen medicinal residue at room temperature. After melting, microwave the residue for 60-80 seconds. Steps 2-5): Cool the residue to 0-20°C with liquid nitrogen, then add the centrifuged liquid obtained in step 2-2) to the residue to form a third mixture, and treat the third mixture with microwave for 60-80 seconds. Steps 2-6): Add solvent to the third mixture so that the total mass of solvent and centrifuged liquid is 5-9 times the mass of the residue, stir and extract to obtain the fourth mixture; Steps 2-7): Centrifuge, age, centrifuge again, filter, and collect the filtrate to obtain Kava pepper root extract; Step 3) Add prickly pear leaf extract to kava root extract, wherein the mass ratio of kava root extract to prickly pear leaf extract is (3-4):
1. Stir to obtain kava compound extract. In steps 2-1) and 2-6), the solvent is polyethylene glycol-8, or a mixture of 1,2-pentanediol and 1,3-butanediol, wherein the mass ratio of 1,2-pentanediol to 1,3-butanediol is (1-2):(1-2). Step 1) specifically includes: Step 1-1): Mix the leaves of the prickly pear cactus with water and extract at 85-90℃ to obtain an extract. The mass of the water is 10-12 times the mass of the prickly pear cactus leaves. Steps 1-2): Add chitosan to the extract for flocculation, stir, let stand, centrifuge, and collect the centrifuged liquid; Steps 1-3) concentrate the centrifuged liquid to a crude drug ratio of 1-1.5 g / ml to obtain a concentrated solution; Steps 1-4): The concentrated solution is adsorbed through an adsorption column and then eluted with a solution to obtain the eluent. Steps 1-5): Add alumina powder to the eluent, stir, filter, take the filtrate, concentrate the filtrate to a crude drug ratio of 1.5-2 g / ml, and obtain the prickly pear cactus leaf extract. The mass of alumina powder added is consistent with the mass of prickly pear cactus leaves in step 1-1). In steps 1-4), the elution solution is an ethanol solution with a concentration of 50% and a volume of 3-4 times the column volume. The adsorption column is a macroporous resin column.
2. The method for preparing a kava complex extract according to claim 1, characterized in that: In steps 2-3), the dregs are frozen with liquid nitrogen for 30-35 minutes.
3. The method for preparing a kava complex extract according to claim 1, characterized in that: In steps 2-4), the microwave frequency during microwave processing is 2400-2500MHz.
4. The method for preparing a kava complex extract according to claim 3, characterized in that: In steps 2-5), the microwave frequency during microwave processing is 2400-2500MHz.
5. A kava complex extract for relieving itching, pain, and inflammation, characterized in that: It is prepared by the method described in any one of claims 1-4 for the preparation of the kava complex extract.
6. The application of the kava complex extract according to claim 5 in the preparation of antipruritic, analgesic, and anti-inflammatory skin care products, characterized in that: Add to water, lotion, or serum at a rate of 0.5%-5%.