A stabilized piper longum root extract and method of preparation
By employing supercritical carbon dioxide defatting, ethanol-water mixed solvent reflux extraction, and nanoemulsion technology, combined with low-temperature drying and light-proof packaging, the structural damage and uneven dispersion problems of kava pepper root extract during high-temperature drying were solved, achieving the stabilization and long-term stability of the extract.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- MINGXING KEPAI BIOTECHNOLOGY (SHANGHAI) CO LTD
- Filing Date
- 2026-06-05
- Publication Date
- 2026-07-14
AI Technical Summary
In existing methods for preparing kava root extract, high-temperature drying processes can easily cause kavalactone ring opening, cis-trans isomerization, or polymerization. During freeze-drying, the precursor liquid does not form a structurally stable dispersion system, leading to component segregation, interfacial adsorption deactivation, or physical aggregation, resulting in poor resolubility and batch-to-batch inconsistency.
Supercritical carbon dioxide defatting and reflux extraction with ethanol-water mixed solvent were used to simultaneously add β-cyclodextrin, rosmarinic acid and ascorbate palmitate to form a polyphenol-lipid-cyclodextrin ternary stable system. Subsequently, a nanoemulsion was formed and instantaneously frozen. Finally, it was sublimated and dried under low temperature vacuum and packaged in a light-proof and moisture-proof container.
This improved the structural stability and resolubility of calvalactone, ensuring the long-term stability and efficacy integrity of the extract at room temperature storage, and avoiding degradation problems caused by high-temperature drying.
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Figure CN122376645A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of biomedicine, and in particular to a stabilized kava root extract and its preparation method. Background Technology
[0002] Kava root extract has received widespread attention in recent years in the field of natural sedative, anti-anxiety and sleep-aiding functional foods and dietary supplements due to its rich content of kava lactone compounds with neuromodulatory activity, such as kavain, methysticin and yangonin. Traditional preparation methods mostly use ethanol or acetone reflux extraction, followed by vacuum concentration, spray drying or freeze drying to obtain solid extract.
[0003] Existing conventional drying processes rely on high temperatures, which can easily cause ring opening, cis-trans isomerization, or polymerization of kavalactone lactone, severely damaging the integrity of the drug efficacy. Even if freeze drying is used, if the precursor solution does not form a structurally stable dispersion system, component segregation, interfacial adsorption inactivation, or physical aggregation will still occur during ice crystal growth, resulting in poor reconstitution and batch inconsistency. Summary of the Invention
[0004] In view of the aforementioned existing problems, the present invention is proposed.
[0005] Therefore, this invention provides a stabilized kava pepper root extract and its preparation method to solve the problems of conventional drying processes that rely on high temperatures, which can easily cause kava lactone to open its ring, undergo cis-trans isomerization or polymerization, and seriously damage the integrity of the drug efficacy. Even if freeze drying is used, if the precursor solution does not form a structurally stable dispersion system, component segregation, interfacial adsorption inactivation or physical aggregation will still occur during ice crystal growth, resulting in poor resolubility and batch inconsistency.
[0006] To solve the above-mentioned technical problems, the present invention provides the following technical solution: This invention provides a stabilized kava root extract, comprising the following components in parts by weight: 100 parts of dried kava pepper root extract, 80–150 parts of β-cyclodextrin, 0.5–2.0 parts of rosmarinic acid, and 0.2–1.0 parts of ascorbate palmitate.
[0007] This invention provides a method for preparing stabilized kava root extract, which includes supercritical carbon dioxide defatting of kava roots to obtain defatted material; The defatted material was heated and refluxed with an ethanol-water mixed solvent for extraction. β-cyclodextrin, rosmarinic acid and ascorbate palmitate were added simultaneously during the extraction process to allow the dissolved calvalactone to form a polyphenol-lipid-cyclodextrin ternary stable system in situ, thus obtaining a stable extract. The stabilized extract was mixed with medium-chain triglycerides, Tween 80 and lecithin, and then homogenized under high pressure to form a nanoemulsion. Nanoemulsions are sprayed into liquid nitrogen for instantaneous freezing to form frozen microparticles; The frozen microparticles were transferred to a vacuum drying system and sublimated under low temperature conditions to obtain a low-moisture stable powder. Particle size adjustment and homogenization were performed on low-moisture stable powder to obtain stable kava root extract; The stabilized kava root extract was packaged in a light-proof and moisture-proof container to complete the preparation.
[0008] In a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the specific steps of defatting the kava root with supercritical carbon dioxide to obtain the defatted material are as follows: The dried kava roots were crushed to a particle size of 2 mm to 4 mm and then loaded into a supercritical extraction vessel. Carbon dioxide fluid was introduced, and dynamic extraction was carried out for 60 to 120 minutes under conditions of pressure of 30 MPa to 40 MPa and temperature of 45°C to 55°C, followed by 10 to 20 minutes of static soaking. After extraction, the pressure is released to recover carbon dioxide, and the solid material is removed to obtain a defatted material with a lipid content of less than 1%.
[0009] As a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the defatted material is heated and refluxed with an ethanol-water mixed solvent for extraction, and β-cyclodextrin, rosmarinic acid and ascorbate palmitate are added simultaneously during the extraction process, so that the dissolved kava lactone forms a polyphenol-lipid-cyclodextrin ternary stable system in situ, thereby obtaining a stabilized extract. The specific steps are as follows: The defatted material was mixed with an ethanol-water mixed solvent with a volume ratio of 7:3 at a material-to-liquid ratio of 1:10 and placed in a reflux extraction device; While heating to 75°C, β-cyclodextrin, rosmarinic acid, and ascorbyl palmitate were added to the extraction system. The amount of β-cyclodextrin added was calculated based on its molar ratio with kavalactone of 1.2:1. The amount of rosmarinic acid added was 1.0% of the total mass of the extract, and the amount of ascorbyl palmitate added was 0.5% of the total mass of the extract. Maintain reflux for 90 minutes to allow calvalactone to be encapsulated and protected against oxidation during dissolution, resulting in a clear or microemulsion-like stabilized extract.
[0010] In a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the steps of mixing the stabilized extract with medium-chain triglycerides, Tween 80 and lecithin, and then homogenizing under high pressure to form a nanoemulsion are as follows: Take the stabilized extract, add 15% by volume of medium-chain triglycerides as the oil phase, and then add 2.0% by mass of Tween 80 and 1.0% by mass of soybean lecithin. First, the pre-emulsion is formed by high-speed shearing at 10,000 rpm for 5 minutes. Then, the pre-emulsion is homogenized three times by high-pressure homogenizer at 80 MPa pressure to obtain O / W type nanoemulsion with uniform particle size and semi-transparent milky white appearance.
[0011] In a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the step of spraying the nanoemulsion into liquid nitrogen for instantaneous freezing to form frozen microparticles includes: The nanoemulsion was continuously sprayed into a stainless steel freezing tank containing liquid nitrogen at a flow rate of 0.5 mL / s using a pneumatic spray device. The droplets freeze instantly into spherical particles upon contact with liquid nitrogen, with particle sizes ranging from 50 μm to 200 μm. The entire spraying process is completed in a closed, low-temperature environment to prevent moisture condensation or oxidation interference.
[0012] As a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the specific steps of transferring the frozen microparticles to a vacuum drying system and sublimating and drying them at low temperature to obtain a low-moisture stable powder are as follows: The frozen microparticles are transferred to the freeze-drying chamber tray within 5 minutes to avoid temperature rise; Set the initial shelf temperature to -45°C, control the system vacuum degree to below 10Pa, and perform primary drying for 12 hours; The shelf temperature was then raised to 25°C, and the drying process continued for 6 hours until the product moisture content was below 2%, resulting in a loose, porous, light yellow, low-moisture stable powder.
[0013] In a preferred embodiment of the method for preparing the stabilized kava root extract of the present invention, the specific steps of performing particle size adjustment and homogenization treatment on the low-moisture stable powder to obtain the stabilized kava root extract are as follows: The low-moisture stable powder is passed through a 300-mesh sieve to remove agglomerated particles; The sieved material was then fed into a three-dimensional motion mixer and mixed at 20 rpm for 15 minutes to ensure uniform particle size distribution and consistent component content, thus obtaining stabilized kava pepper root extract.
[0014] In a preferred embodiment of the preparation method of the stabilized kava root extract of the present invention, the step of encapsulating the stabilized kava root extract in a light-proof and moisture-proof container to complete the preparation includes the following steps: The stabilized pepper root extract was packaged in single doses using aluminum-plastic composite film bags, with the amount per bag set according to the formulation requirements. Before sealing, high-purity nitrogen is introduced into the bag to replace the internal air, and then heat-sealed. The packaging materials used have a water vapor permeability of less than 0.5 g / (m²). 2 With performance including 24h) and visible light transmittance of less than 1%, the product is guaranteed to be stable for a long time under normal temperature storage conditions.
[0015] As a preferred embodiment of the preparation method of the stabilized kava root extract of the present invention, the total content of the six major kava lactones in the stabilized kava root extract is not less than 60%, and the dispersion system formed after the extract is redissolved in water shows no visible precipitation or phase separation after standing at 25°C for 24 hours, indicating that it has good physical redispersibility and formulation suitability.
[0016] The beneficial effects of this invention are as follows: When defatted materials are refluxed with an ethanol-water mixed solvent for extraction, β-cyclodextrin, rosmarinic acid, and ascorbyl palmitate are introduced simultaneously, so that the dissolved calvalactone forms a ternary stable system of "polyphenol-lipid-cyclodextrin" in situ at the molecular level, achieving synergistic protection of inclusion isolation, free radical scavenging, and interfacial antioxidation, fundamentally blocking degradation pathways such as oxidation, photolysis, and hydrolysis. Subsequently, the stabilized extract is homogenized with medium-chain triglycerides, Tween 80, and lecithin under high pressure to construct an O / W type nanoemulsion, further forming a multi-layered physical barrier of "inclusion core-phospholipid interface-oil phase microregion" at the nanoscale, improving the dispersion stability and environmental tolerance of the liquid intermediate. Attached Figure Description
[0017] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0018] Figure 1 A flowchart of the preparation method for stabilizing kava root extract. Detailed Implementation
[0019] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
[0020] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of the invention. Therefore, the invention is not limited to the specific embodiments disclosed below.
[0021] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it a single or selective embodiment that is mutually exclusive with other embodiments.
[0022] Example 1, referring to Figure 1 This is the first embodiment of the present invention, which provides a stabilized kava root extract and its preparation method, including the following steps: S1. Supercritical carbon dioxide degreasing of kava pepper roots yields degreased material.
[0023] Furthermore, the dried kava pepper roots are pulverized to a particle size of 2 mm to 4 mm and then loaded into a supercritical extraction vessel; Carbon dioxide fluid was introduced, and dynamic extraction was carried out for 60 to 120 minutes under conditions of pressure of 30 MPa to 40 MPa and temperature of 45°C to 55°C, followed by 10 to 20 minutes of static soaking. After extraction, the pressure is released to recover carbon dioxide, and the solid material is removed to obtain a defatted material with a lipid content of less than 1%.
[0024] It should be noted that by selectively removing fat-soluble impurities using supercritical carbon dioxide, the difficulties in phase separation and loss of calvalactone encapsulation caused by oil emulsification during subsequent water-alcohol extraction are effectively avoided. At the same time, the use of residual organic solvents is avoided, improving the purity of raw materials and extraction efficiency, and providing a clean matrix for subsequent in-situ stabilization.
[0025] S2. The defatted material is heated and refluxed together with an ethanol-water mixed solvent for extraction. During the extraction process, β-cyclodextrin, rosmarinic acid and ascorbate palmitate are added simultaneously to allow the dissolved calvalactone to form a polyphenol-lipid-cyclodextrin ternary stable system in situ, thus obtaining a stable extract.
[0026] Furthermore, the defatted material is mixed with an ethanol-water mixed solvent at a volume ratio of 7:3 and a material-to-liquid ratio of 1:10, and then placed in a reflux extraction device. While heating to 75°C, β-cyclodextrin, rosmarinic acid, and ascorbyl palmitate were added to the extraction system. The amount of β-cyclodextrin added was calculated based on its molar ratio with kavalactone of 1.2:1. The amount of rosmarinic acid added was 1.0% of the total mass of the extract, and the amount of ascorbyl palmitate added was 0.5% of the total mass of the extract. Maintain reflux for 90 minutes to allow calvalactone to be encapsulated and protected against oxidation during dissolution, resulting in a clear or microemulsion-like stabilized extract.
[0027] It should be noted that the simultaneous introduction of ternary stable components during the extraction stage achieves the in-situ stabilization mechanism of kavalactone, which is protected upon dissolution. This avoids the irreversible degradation caused by exposure of the extract to oxygen, heat, and light in traditional processes, improves the retention rate of active ingredients, and forms a molecular-level composite structure, providing a uniform and stable precursor system for subsequent nanoemulsification.
[0028] S3. The stabilized extract is mixed with medium-chain triglycerides, Tween 80 and lecithin, and then homogenized under high pressure to form a nanoemulsion.
[0029] Furthermore, take the stabilized extract, add 15% by volume of medium-chain triglycerides as the oil phase, and then add 2.0% by mass of Tween 80 and 1.0% by mass of soybean lecithin. First, the pre-emulsion is formed by high-speed shearing at 10,000 rpm for 5 minutes. Then, the pre-emulsion is homogenized three times by high-pressure homogenizer at 80 MPa pressure to obtain O / W type nanoemulsion with uniform particle size and semi-transparent milky white appearance.
[0030] It should be noted that by constructing a nanoemulsion with natural phospholipids and nonionic surfactants as the interface, the existing ternary stable system is further encapsulated in hydrophobic microregions, forming a dual barrier of "core encapsulation + outer emulsification", which effectively blocks oxygen penetration and photocatalysis, significantly improves the physicochemical stability of calvalactone in the liquid stage, and improves its water dispersibility.
[0031] S4. Spray the nanoemulsion into liquid nitrogen for instantaneous freezing to form frozen microparticles.
[0032] Furthermore, during the instantaneous freezing process, the nanoemulsion is sprayed into a depth of 5cm to 10cm below the liquid nitrogen surface through a stainless steel nozzle with an aperture of 0.2mm to 0.5mm at a constant flow rate, so that the droplets are frozen in a completely submerged state, avoiding particle deformation or aggregation caused by gas-liquid interface disturbance. The frozen microparticles are kept in liquid nitrogen for no less than 30 seconds to ensure that the internal temperature is uniformly reduced to below -190°C, forming a glassy amorphous structure, thereby completely preserving the microscopic dispersion state of the nanoemulsion.
[0033] It should be noted that the use of liquid nitrogen deep immersion instantaneous freezing avoids the emulsion breaking, local concentration of active ingredients, or phase separation caused by the slow growth of ice crystals during conventional freezing. This allows the nanostructure to be "frozen and preserved" in the solid state, providing structural integrity assurance for subsequent low-temperature drying and preventing loss of activity.
[0034] S5. Transfer the frozen microparticles to a vacuum drying system and perform sublimation drying under low temperature conditions to obtain a low-moisture stable powder.
[0035] Furthermore, the frozen microparticles are transferred to the freeze-drying chamber tray within 5 minutes to avoid temperature rise; Set the initial shelf temperature to -45°C, control the system vacuum degree to below 10Pa, and perform primary drying for 12 hours; The shelf temperature was then raised to 25°C, and the drying process continued for 6 hours until the product moisture content was below 2%, resulting in a loose, porous, light yellow, low-moisture stable powder.
[0036] It should be noted that by using low-temperature vacuum sublimation drying throughout the process, the high-temperature thermal stress in hot air drying or spray drying is completely avoided, effectively preventing the ring opening, isomerization, or oxidative degradation of calvalactone. The resulting powder has low water activity, high specific surface area, and good resolubility, extending the product shelf life and maintaining the integrity of the drug efficacy.
[0037] S6. The low-moisture stable powder is subjected to particle size preparation and homogenization treatment to obtain stable kava pepper root extract.
[0038] Furthermore, the low-moisture stable powder is passed through a 300-mesh sieve to remove agglomerated particles; The sieved material was then fed into a three-dimensional motion mixer and mixed at 20 rpm for 15 minutes to ensure uniform particle size distribution and consistent component content, thus obtaining stabilized kava pepper root extract.
[0039] It should be noted that by using sieving and three-dimensional mixing operations, the problem of local component segregation or particle size unevenness that may occur during freeze-drying is eliminated, ensuring that the extract meets the requirements of industrial formulation in terms of flowability, filling capacity and dosage uniformity, thereby improving product quality consistency and production controllability.
[0040] S7. The stabilized kava root extract is packaged in a light-proof and moisture-proof container to complete the preparation.
[0041] Furthermore, the stabilized kava root extract is packaged in single-dose form using aluminum-plastic composite film bags, with the amount per bag set according to the formulation requirements. Before sealing, high-purity nitrogen is introduced into the bag to replace the internal air, and then heat-sealed. The packaging materials used have a water vapor permeability of less than 0.5 g / (m²).2 With performance including 24h) and visible light transmittance of less than 1%, the product is guaranteed to be stable for a long time under normal temperature storage conditions.
[0042] It should be noted that by using high-barrier packaging and inert gas protection, the three major degradation factors of moisture, oxygen and light are blocked from the final stage, so that the stabilized kava root extract can maintain high activity and sensory quality even after long-term storage at room temperature, meeting the comprehensive requirements of commercial products for stability, safety and user experience.
[0043] Example 2 is the second embodiment of the present invention. This embodiment provides a stabilized kava root extract and its preparation method, including the following steps: Take 1.0 kg of dried kava pepper root, crush it to a particle size of 3 mm, put it into a 5 L supercritical extraction vessel, introduce food-grade carbon dioxide, and dynamically extract for 90 minutes under the conditions of 35 MPa pressure and 50°C temperature. Then, statically soak for 15 minutes, circulate twice, depressurize and recover carbon dioxide, take out the solid material, and measure the lipid content to be 0.7%, thus obtaining the defatted material.
[0044] The defatted material was added to a reflux extraction vessel at a material-to-liquid ratio of 1:10 (g / mL) with a 7:3 ethanol-water mixture. Simultaneously, β-cyclodextrin (added at an estimated molar ratio of 1.2:1 for the total calovalins), rosmarinic acid (1.0% of the total extract mass), and ascorbyl palmitate (0.5% of the total extract mass) were added. The mixture was heated to 75°C and refluxed for 90 minutes. The residue was removed by filtration, yielding a clear, microemulsion-like stabilized extract. HPLC analysis showed that the total content of the six major calovalins was 63.2%.
[0045] Take 500 mL of the stabilized extract, add 75 mL of medium chain triglycerides (MCT), then add 11.5 g of Tween 80 and 5.8 g of soybean lecithin, and shear at 10000 rpm for 5 minutes to form colostrum; Subsequently, the mixture was homogenized three times at 80 MPa using a high-pressure homogenizer to obtain a semi-transparent O / W nanoemulsion with an average particle size of 112 nm and a PDI of 0.16.
[0046] The nanoemulsion was sprayed into liquid nitrogen at a flow rate of 0.5 mL / s through a stainless steel nozzle with an aperture of 0.3 mm to a depth of 8 cm below the surface of the liquid nitrogen. The droplets instantly froze into spherical microparticles. After standing in liquid nitrogen for 40 seconds, the microparticles were collected to obtain white frozen microparticles.
[0047] The frozen microparticles were rapidly transferred to a freeze-drying tray and fed into a vacuum freeze-drying system within 5 minutes. The shelf temperature was set to -45°C and the vacuum degree to ≤10Pa, and the initial drying was carried out for 12 hours. The temperature was then raised to 25°C, and the powder was dried for 6 hours to obtain a light yellow, loose powder with a moisture content of 1.8%.
[0048] The obtained powder was passed through a 300-mesh sieve, and the sieved material was put into a three-dimensional mixer and mixed at 20 rpm for 15 minutes to obtain a stable kava root extract with uniform particle size and composition.
[0049] The total content of the six calvalactones was 61.5%, with a relative standard deviation (RSD) of 2.8%.
[0050] The extract was dispensed into aluminum-plastic composite film bags (water vapor permeability 0.4 g / (m²)). 2 • 24h), transmittance 0.8%, nitrogen-filled and sealed. After accelerated storage at 40°C and 75%RH for 90 days, the total retention rate of calvalactone was 87.6%. After reconstitution, the solution was clear without precipitation, the pH value was stable at 5.9, and there was no off-odor or darkening of color, indicating that the product has excellent long-term stability and formulation suitability.
[0051] Comparative Example 1: 1.0 kg of defatted peppercorn root material from the same batch as in Example 2 was extracted by reflux for 90 minutes (75°C) using a 7:3 ethanol-water mixed solvent at a material-to-liquid ratio of 1:10. No β-cyclodextrin, rosmarinic acid, or ascorbyl palmitate was added. After extraction, the extract was filtered to obtain a common extract. Subsequent steps were the same as in Example 2: MCT, Tween 80, and lecithin were added to form a nanoemulsion, which was then frozen in liquid nitrogen, lyophilized, and granulated to obtain a powder product. The total content of kavalactone in the obtained extract was only 48.3%. After accelerated stability testing (40°C / 75%RH, 90 days), the retention rate decreased to 51.2%, and the reconstituted solution showed significant turbidity and slight browning. This result indicates that the lack of in-situ molecular protection led to degradation during extraction and storage.
[0052] Comparative Example 2: After completing the in-situ stabilization extraction described in Example 1, no medium-chain triglycerides, Tween 80, or lecithin were added, and no high-pressure homogenization was performed. Instead, the stabilized extract was directly sprayed into liquid nitrogen for freezing, and then dried into powder under the same freeze-drying conditions. The resulting powder was in hard lumps with poor flowability. After reconstitution, obvious stratification and flocculent precipitation occurred within 24 hours. The total content of calvalactone was 55.3%, and the retention rate after 90-day accelerated testing was 66.8%, which was much lower than the 87.3% in Example 1. This result indicates that the lack of an interfacial encapsulation structure of nanoemulsion makes it impossible to maintain the uniform dispersion of active ingredients during freezing and drying, resulting in physical instability and loss of activity.
[0053] Comparative Example 3: After completing all the preliminary steps of Example 1 (including in-situ steady-state extraction and nanoemulsification), the nanoemulsion was dried in a vacuum oven at 60°C for 12 hours without being frozen with liquid nitrogen to obtain a solid powder. The resulting product was dark yellow in color and had a slight burnt smell. HPLC analysis showed that the total content of kavalin was only 45.2%, with heat-sensitive components such as kavain and yangonin losing more than 50%. The retention rate was less than 58% after 90 days of accelerated stability testing. This result indicates that even if a steady-state system is constructed in the early stage, thermal stress introduced during the final drying process will still destroy the lactone ring structure, confirming that low-temperature freeze-drying-sublimation drying is a necessary condition to ensure the high activity of the product.
[0054] In summary, this invention introduces β-cyclodextrin, rosmarinic acid, and ascorbyl palmitate simultaneously during the reflux extraction of defatted materials with an ethanol-water mixed solvent. This allows the dissolved calvaline to form a stable ternary system of "polyphenol-lipid-cyclodextrin" at the molecular level, achieving synergistic protection through inclusion isolation, free radical scavenging, and interfacial antioxidant activity. This fundamentally blocks degradation pathways such as oxidation, photolysis, and hydrolysis. Subsequently, the stabilized extract is homogenized with medium-chain triglycerides, Tween 80, and lecithin under high pressure to construct an O / W nanoemulsion. This further forms a multi-layered physical barrier at the nanoscale, consisting of "inclusion core – phospholipid interface – oil phase microregions," enhancing the dispersion stability and environmental tolerance of the liquid intermediate.
[0055] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.
Claims
1. A stabilized kava root extract, characterized in that: The extract consists of the following components in parts by weight: 100 parts of dried kava pepper root extract, 80–150 parts of β-cyclodextrin, 0.5–2.0 parts of rosmarinic acid, and 0.2–1.0 parts of ascorbate palmitate.
2. A method for preparing a stabilized kava root extract, as described in claim 1, characterized in that: include: Supercritical carbon dioxide degreasing was performed on kava pepper roots to obtain degreased material; The defatted material was heated and refluxed with an ethanol-water mixed solvent for extraction. β-cyclodextrin, rosmarinic acid and ascorbate palmitate were added simultaneously during the extraction process to allow the dissolved calvalactone to form a polyphenol-lipid-cyclodextrin ternary stable system in situ, thus obtaining a stable extract. The stabilized extract was mixed with medium-chain triglycerides, Tween 80 and lecithin, and then homogenized under high pressure to form a nanoemulsion. Nanoemulsions are sprayed into liquid nitrogen for instantaneous freezing to form frozen microparticles; The frozen microparticles were transferred to a vacuum drying system and sublimated under low temperature conditions to obtain a low-moisture stable powder. Particle size adjustment and homogenization were performed on low-moisture stable powder to obtain stable kava root extract; The stabilized kava root extract was packaged in a light-proof and moisture-proof container to complete the preparation.
3. The method for preparing stabilized kava root extract as described in claim 2, characterized in that: The specific steps for supercritical carbon dioxide degreasing of kava pepper roots to obtain degreased material are as follows: The dried kava roots were crushed to a particle size of 2 mm to 4 mm and then loaded into a supercritical extraction vessel. Carbon dioxide fluid was introduced, and dynamic extraction was carried out for 60 to 120 minutes under conditions of pressure of 30 MPa to 40 MPa and temperature of 45°C to 55°C, followed by 10 to 20 minutes of static soaking. After extraction, the pressure is released to recover carbon dioxide, and the solid material is removed to obtain a defatted material with a lipid content of less than 1%.
4. The method for preparing stabilized kava root extract as described in claim 3, characterized in that: The defatted material is extracted by heating and refluxing with an ethanol-water mixed solvent, and β-cyclodextrin, rosmarinic acid, and ascorbate palmitate are added simultaneously during the extraction process. This allows the dissolved calvaline to form a stable ternary system of polyphenol-lipid-cyclodextrin in situ, resulting in a stable extract. The specific steps are as follows: The defatted material was mixed with an ethanol-water mixed solvent with a volume ratio of 7:3 at a material-to-liquid ratio of 1:10 and placed in a reflux extraction device; While heating to 75°C, β-cyclodextrin, rosmarinic acid, and ascorbyl palmitate were added to the extraction system. The amount of β-cyclodextrin added was calculated based on its molar ratio with kavalactone of 1.2:
1. The amount of rosmarinic acid added was 1.0% of the total mass of the extract, and the amount of ascorbyl palmitate added was 0.5% of the total mass of the extract. Maintain reflux for 90 minutes to allow calvalactone to be encapsulated and protected against oxidation during dissolution, resulting in a clear or microemulsion-like stabilized extract.
5. The method for preparing stabilized kava root extract as described in claim 4, characterized in that: The process involves mixing the stabilized extract with medium-chain triglycerides, Tween 80, and lecithin, followed by high-pressure homogenization to form a nanoemulsion. The specific steps are as follows: Take the stabilized extract, add 15% by volume of medium-chain triglycerides as the oil phase, and then add 2.0% by mass of Tween 80 and 1.0% by mass of soybean lecithin. First, the pre-emulsion is formed by high-speed shearing at 10,000 rpm for 5 minutes. Then, the pre-emulsion is homogenized three times by high-pressure homogenizer at 80 MPa pressure to obtain O / W type nanoemulsion with uniform particle size and semi-transparent milky white appearance.
6. The method for preparing stabilized kava root extract as described in claim 5, characterized in that: The specific steps for spraying the nanoemulsion into liquid nitrogen for instantaneous freezing to form frozen microparticles are as follows: The nanoemulsion was continuously sprayed into a stainless steel freezing tank containing liquid nitrogen at a flow rate of 0.5 mL / s using a pneumatic spray device. The droplets freeze instantly into spherical particles upon contact with liquid nitrogen, with particle sizes ranging from 50 μm to 200 μm. The entire spraying process is completed in a closed, low-temperature environment to prevent moisture condensation or oxidation interference.
7. The method for preparing stabilized kava root extract as described in claim 6, characterized in that: The specific steps for transferring the frozen microparticles to a vacuum drying system and performing sublimation drying at low temperature to obtain a low-moisture stable powder are as follows: The frozen microparticles are transferred to the freeze-drying chamber tray within 5 minutes to avoid temperature rise; Set the initial shelf temperature to -45°C, control the system vacuum degree to below 10Pa, and perform primary drying for 12 hours; The shelf temperature was then raised to 25°C, and the drying process continued for 6 hours until the product moisture content was below 2%, resulting in a loose, porous, light yellow, low-moisture stable powder.
8. The method for preparing stabilized kava root extract as described in claim 7, characterized in that: The process of particle size adjustment and homogenization of the low-moisture stable powder to obtain stable kava root extract involves the following steps: The low-moisture stable powder is passed through a 300-mesh sieve to remove agglomerated particles; The sieved material was then fed into a three-dimensional motion mixer and mixed at 20 rpm for 15 minutes to ensure uniform particle size distribution and consistent component content, thus obtaining stabilized kava pepper root extract.
9. The method for preparing the stabilized kava root extract as described in claim 8, characterized in that: The preparation process involves encapsulating the stabilized kava root extract in a light-proof and moisture-proof container. The specific steps are as follows: The stabilized pepper root extract was packaged in single doses using aluminum-plastic composite film bags, with the amount per bag set according to the formulation requirements. Before sealing, high-purity nitrogen is introduced into the bag to replace the internal air, and then heat-sealed. The packaging materials used have a water vapor permeability of less than 0.5 g / (m²). 2 With performance including 24h) and visible light transmittance of less than 1%, the product is guaranteed to be stable for a long time under normal temperature storage conditions.
10. The method for preparing the stabilized kava root extract as described in claim 9, characterized in that: The total content of the six major kavalactones in the stabilized kavalactin root extract is not less than 60%, and the dispersion system formed after the extract is redissolved in water shows no visible precipitation or phase separation after standing at 25°C for 24 hours, indicating that it has good physical redispersibility and formulation suitability.