A herbal medicine, Glycetract, and its manufacturing process

Abstract

Abstract This invention belongs to the field of herbal extraction technology and relates to a herbal medicine, Glycetract, and its manufacturing process. The invention provides a preparation method for the Glycetract of the herbal medicine, using polyols as the extraction solvent, combined with ultrasonic treatment, heating, and / or percolation. The method provided by the invention significantly increases the content of active ingredients in the Glycetract product, enhances production efficiency, reduces production costs, and notably improves the safety of the production environment while promoting environmental sustainability and protection. It enables the industrial-scale and commercial production of Glycetract products. Abstract This invention belongs to the field of herbal extraction technology and relates to a herbal medicine, Glycetract, and its manufacturing process. The invention provides a preparation method for the Glycetract of the herbal medicine, using polyols as the extraction solvent, combined with ultrasonic treatment, heating, and / or percolation. The method provided by the invention significantly increases the content of active ingredients in the Glycetract product, enhances production efficiency, reduces production costs, and notably improves the safety of the production environment while promoting environmental sustainability and protection. It enables the industrial-scale and commercial production of Glycetract products. 20 24 25 98 96 11 N ov 2 02 4 2 0 2 4 2 5 9 8 9 6 1 1 N o v 2 0 2 4 2 0 2 4 2 5 9 8 9 6 1 1 N o v 2 0 2 4

Description

TECHNICAL FIELD This invention belongs to the field of herbal extraction technology and relates to a herbal medicine, Glycetract, and its manufacturing process. BACKGROUND OF THE INVENTION The active ingredients in herbal medicines include hydrophilic and lipophilic compounds. Lipid-soluble active components, such as alkylamides, kavalactones, long-chain polyphenols (like curcumin), isoflavones (such as tangeretin), tocopherols (including tocotrienols), retinoids, methyl naphthoquinones (like phylloquinone), carotenoids (such as astaxanthin), cinnamic acid derivatives (like caffeic acid phenethyl ester), diterpenes (such as propolis and phytol), terpenes (like squalene), coenzyme Q10, and alpha-lipoic acid, have been widely used in cosmetics and food products to deliver immune-boosting, whitening, anti-aging, and other active effects. Hydrophilic compounds can be extracted using water, while lipophilic compounds have poor solubility in water and thus require organic solvents for extraction. Among the various organic solvents, ethanol is one of the less toxic, edible options. Consequently, ethanol or ethanol-water solutions of different concentrations are currently recognised as effective and widely used solvents for extracting lipophilic active components in herbal medicines. Currently, in existing technology, ethanol is the most commonly used solvent. Although ethanol is safe for consumption in moderate amounts, it still possesses certain toxic and addictive properties, making it unsuitable for specific groups, such as pregnant women, children, and individuals from some religious communities. To avoid the ingestion of ethanol, a common practice in the industry is to first extract the active components of herbal medicine using ethanol. After the ethanol is evaporated from the extract, glycerin—a consumable solvent with polarity similar to that of ethanol—is used to resolubilise the concentrate, resulting in a liquid product that contains no or only trace amounts of ethanol, known as Glycetract. The advantage of Glycetract products is that they retain the lipid-soluble active components that dissolve in ethanol while containing no or only trace amounts of ethanol, making them 2024259896   11 Nov 2024 suitable for a broader range of consumers. In applications, Glycetract can be directly provided to practitioners or used as a raw material for final herbal medicine products. The manufacturing process of Glycetract primarily includes the following steps: 1. Depending on the lipophilicity of the target active components in different herbal medicines, ethanol-water solutions of varying concentrations are used for extraction. This step is typically carried out through percolation or maceration, a process that generally takes two weeks and often even longer. The resulting product is called a hydroethanolic extract. 2. Heating is used to evaporate the ethanol from the hydroethanolic extract. Depending on the batch size, this process usually takes several hours to several days, resulting in a product known as ethanol-evaporated concentrate. 3. Glycerin is added to the ethanol concentrate to replace the evaporated ethanol and water, thereby resolubilising the concentrate. 4. The insoluble precipitate is filtered out, and the resulting product is known as Glycetract. The advantages of this process are: 1. Even with safety concerns regarding the use and consumption of ethanol, ethanol-water solutions remain the most widely used solvents known for herbal extraction. 2. Lipophilic compounds, such as alkylamides and kavalactones, are insoluble in water; therefore, high concentrations of ethanol (such as 60% ethanol) are among the best choices for their extraction. 3. Glycerin has a polarity similar to that of ethanol, allowing it to effectively dissolve the active components extracted by ethanol. However, the drawbacks of this process are: 1. The majority of lipid-soluble active components, including alkylamides and kavalactones, are heat-sensitive compounds. When the ethanol extract is concentrated by heating, the active components may degrade due to the heat, leading to a significant decrease in their content and thus affecting the efficacy. 2. When resolubilising with glycerin, although glycerin's polarity is similar to that of ethanol, it is actually higher. As a result, some lipid-soluble components that dissolve in ethanol may not fully dissolve in glycerin, leading to the formation of precipitates and further loss of active ingredients. 3. Percolation or maceration takes two weeks or longer, and the concentration and evaporation of ethanol is also time-consuming, resulting in a lengthy overall process. 4. Ethanol is a flammable and explosive hazardous chemical, with a flash point of 13°C. Strict adherence to various safety operating guidelines is required during production, yet 2024259896   11 Nov 2024 safety risks still exist. Products containing high concentrations of ethanol must also comply with hazardous materials regulations during transportation. 5. Ethanol has a relatively low boiling point of 78°C, making it prone to evaporation during the production process, which can pose an inhalation risk to operators. 6. During the concentration and evaporation of ethanol, waste liquid and waste gas are generated, leading to environmental pollution from their discharge and treatment. 7. The cost of food-grade ethanol is relatively high, resulting in increased production costs. In summary, it is necessary to develop a new manufacturing process for Glycetract by introducing a non-toxic, environmentally friendly, and cost-effective polyol solvent to directly extract lipid-soluble active components from herbal medicines. This approach would avoid the loss of active components associated with the evaporation of ethanol and resolubilisation, thereby increasing the content of effective ingredients. Additionally, the production process should be simplified and time-efficient, allowing for scalability to reduce costs. STATEMENT OF INVENTION To address the aforementioned technical issues, the present invention provides a new manufacturing process for Glycetract by introducing a non-toxic, environmentally friendly, and cost-effective polyol solvent to directly extract lipid-soluble active components from herbal medicines. This method avoids the loss of active ingredients associated with the evaporation of ethanol and resolubilisation, thereby increasing the content of effective components. Additionally, the production process is simplified, time-efficient, and scalable to reduce costs. The ultimate goal is to produce safe, effective, and affordable herbal medicine products for consumers. To achieve the above objectives, the present invention adopts the following technical solutions: Using a polyol as the extraction solvent, and simultaneously conducting ultrasonic treatment, lower temperature heating, and / or percolation / maceration. The preferred polyol is selected from the group including propylene glycol and glycerin. The specific method for preparing the herbal medicine Glycetract includes the following steps: S1> Preparation of the herbal material and solvent: Mill the herb to pass through a 50-200 mesh sieve. Prepare a polyol aqueous solution to be used as the extracting agent, wherein the 2024259896   11 Nov 2024 concentration of the polyol is 20-100% v / v. S2> Extraction Add the polyol aqueous solution (extracting agent) to the herbal material and stir well. Preferably, mix the solvent and herbal material in a volume ratio of 3:1 to 10:1. Use one of the following methods for extraction, with Method A being the preferred method. a. Ultrasonic treatment with a frequency range of 18-100 kHz for 0.5 to 3 hours; maintaining the temperature at 60°C ± 5°C. b. Heating treatment for 6 to 12 hours, maintaining the temperature at 60°C ± 5°C. c. Percolation at room temperature for 1 to 3 weeks. d. The obtained herbal solution is placed in a centrifuge for centrifugation to settle the residue, separating the supernatant. The supernatant is then filtered to obtain the final product, Glycetract. Compared with the current process, the present invention has the following technical advantages: 1. The present invention provides a complete manufacturing process for Glycetract using polyols as green extraction solvents. 2. Propylene glycol and glycerin are both small-molecule polyols. Propylene glycol is a colourless, odourless, slightly sweet transparent liquid widely used in the pharmaceutical, food, and cosmetic industries. It is a diol with three carbon atoms and two hydroxyl groups. There have been no reports of its use as a solvent for extracting lipid-soluble components in herbal medicines. Glycerin is a colourless, odourless, sweet-tasting viscous liquid that is commonly used as a food ingredient. It is a triol with three carbon atoms and three hydroxyl groups. Similarly, there have been no reports of its use as a solvent for extracting lipid-soluble components in herbal medicines. Considering that the polarity of propylene glycol and glycerin is similar to that of ethanol, and they are both small-molecule solvents, we are the first to utilise them as extracting solvents for lipid-soluble components in herbal medicines. Compared to ethanol, propylene glycol and glycerin have relatively higher molecular weights and are more viscous; thus, to enhance their extraction efficiency, ultrasonic or mild heating methods are employed to assist in the extraction process. 3. When extracting lipid-soluble active ingredients from herbal medicines using propylene glycol, the extraction rate is comparable to that of ethanol. The propylene glycol process does not require the heating and evaporation of ethanol, nor the subsequent re-dissolution with glycerin, thereby avoiding the loss of heat-sensitive active ingredients and those that 2024259896   11 Nov 2024 are insoluble in glycerin. As a result, the overall extraction rate is significantly improved compared to that with ethanol. 4. When extracting lipid-soluble active ingredients from herbal medicines using glycerin, the extraction rate is approximately 55% of that of ethanol. However, the glycerin process does not require the heating and evaporation of ethanol or the subsequent re-dissolution with glycerin, thereby avoiding the loss of heat-sensitive active ingredients and those that are insoluble in glycerin. Overall, the extraction rates achieved through ultrasonic and heating methods with glycerin are comparable to those obtained with ethanol. 5.  The consumption safety of propylene glycol and glycerin is higher than that of ethanol. 6.  The manufacturing process of using propylene glycol or glycerin takes a shorter time, has fewer process control points, and is highly efficient. 7. Propylene glycol and glycerin are not classified as flammable or explosive substances, with flash points of 107°C and 177°C, respectively, making them safer and more stable than ethanol. 8. Propylene glycol and glycerin have high boiling points of 188°C and 290°C, respectively, making them less likely to volatilise during production, resulting in an extremely low risk of inhalation for operators. 9. The manufacturing process of using propylene glycol or glycerin does not generate wastewater or exhaust gases, resulting in no negative impact on the environment. 10. Propylene glycol and glycerin are less expensive compared to ethanol. DETAILED DESCRIPTION OF THE INVENTION Technical people in the field can refer to the content of this invention to appropriately modify the process parameters for implementation. It should be particularly noted that all similar substitutions and alterations are evident to those technical people in this field and are considered included within this invention. The methods and applications of the present invention have been described through preferred embodiments, and relevant personnel can clearly make modifications or suitable changes and combinations to the methods and applications described herein without departing from the content, essence, and scope of the invention to achieve and apply the technology of this invention. This embodiment takes the Glycetract products of Echinacea (purple coneflower) and Kava (Kava pepper) as examples. Target active ingredients: Echinacea: alkylamides; Kava: kavalactones The manufacturing process of the present invention: 1. Mill the dried Echinacea or Kava herb to pass through a 50-60 mesh sieve. 2024259896   11 Nov 2024 2. Prepare an aqueous solution of polyol as the extraction agent, wherein the concentration of the polyol is 85-90% v / v. 3. Add the extraction agent, an aqueous solution of polyol (specifically propylene glycol and glycerin), to the herb, and stir well; the volume ratio of the solvent to the medicinal material is 3:1 to 7:1. 4. Use any one of the following methods for extraction. a. Ultrasonic treatment with a frequency of 20 kHz for 1.0 to 1.5 hours, maintaining a temperature of 60°C ± 5°C. b. Heating treatment for 8 to 12 hours, maintaining a temperature of 60°C ± 5°C. c. Percolation or maceration at room temperature for 2 weeks. d. The obtained liquid is placed in a centrifuge to centrifuge, allowing the sediment to settle at the bottom and separating the supernatant; filtering the supernatant yields the finished plant medicine Glycetract from Echinacea or Kava. Specifically, the inventors have made the following specific implication. Embodiment 1 Preparation of Medicinal Material: Mill the dry Echinacea herb and pass it through a 50-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 85%. Extraction Process: Add the extraction agent to the herbal at a volume ratio of 7:1 and stir the mixture thoroughly to ensure even dispersion. Use an ultrasonic processor with a frequency of 20 kHz, treating the mixture for 1.0 hour while maintaining the temperature at 60°C ± 5°C. Centrifugation and Filtration: The obtained liquid is placed in a centrifuge, allowing the sediment to settle at the bottom. The supernatant is then filtered to yield the final product, the Echinacea Glycetract. Embodiment 2 Preparation of Medicinal Material: Mill the dry Echinacea herb and pass it through a 50-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 85%. Extraction Process: 2024259896   11 Nov 2024 Add the extraction agent to the herbal at a volume ratio of 6:1 and stir the mixture thoroughly to ensure even dispersion. Using the heating treatment method, the mixture is heated for 8 hours while maintaining a temperature of 60°C ± 5°C. Centrifugation and Filtration: The obtained liquid is placed in a centrifuge, allowing the sediment to settle at the bottom. The supernatant is then filtered to yield the final product, the Echinacea Glycetract. Embodiment 3 Preparation of Medicinal Material: Mill the dry Echinacea herb and pass it through a 50-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 85%. Extraction Process: Wet down the herb with the extraction agent at a volume ratio of 1:1 and stir the mixture thoroughly to ensure even dispersion. Pack the wetted herb into the selected percolators. Add the extraction agent to the percolators at a volume ratio of 2:1. Allow the menstruum to pass through the percolator. Start the maceration for 48 hours. Open the tap to collect the liquid. Press the herb and collect the liquid. Combine the liquid obtained from the percolator and the pressor. The liquid is then filtered to yield the final product, the Echinacea Glycetract. Embodiment 4 Preparation of Medicinal Material: Mill the dry Kava herb and pass it through a 60-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 90%. Extraction Process: Add the extraction agent to the herbal at a volume ratio of 7:1 and stir the mixture thoroughly to ensure even dispersion. Use an ultrasonic processor with a frequency of 20 kHz, treating the mixture for 1.5 hour 2024259896   11 Nov 2024 while maintaining the temperature at 60°C ± 5°C. Centrifugation and Filtration: The obtained liquid is placed in a centrifuge, allowing the sediment to settle at the bottom. The supernatant is then filtered to yield the final product, the Kava Glycetract. Embodiment 5 Preparation of Medicinal Material: Mill the dry Kava herb and pass it through a 60-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 90%. Extraction Process: Add the extraction agent to the herbal at a volume ratio of 6:1 and stir the mixture thoroughly to ensure even dispersion. Using the heating treatment method, the mixture is heated for 12 hours while maintaining a temperature of 60°C ± 5°C. Centrifugation and Filtration: The obtained liquid is placed in a centrifuge, allowing the sediment to settle at the bottom. The supernatant is then filtered to yield the final product, the Kava Glycetract. Embodiment 6 Preparation of Medicinal Material: Mill the dry Kava herb and pass it through a 50-mesh sieve. Preparation of Extraction Agent: Prepare an aqueous solution of propylene glycol and glycerin with a volume concentration of 90%. Extraction Process: Wet down the herb with the extraction agent at a volume ratio of 2:1 and stir the mixture thoroughly to ensure even dispersion. Pack the wetted herb into the selected percolators. Add the extraction agent to the percolators at a volume ratio of 2:1. Allow the menstruum to pass through the percolator. Start the maceration for 48 hours. Open the tap to collect the liquid. Press the herb and collect the liquid. Combine the liquid obtained from the percolator and the pressor. 2024259896   11 Nov 2024 The liquid is then filtered to yield the final product, the Kava Glycetract. Comparison with the current manufacturing process as below 1. Mill the dry Echinacea or Kava herb and pass it through a 50-mesh sieve. 2. Prepare 60% v / v ethanol aqueous solution as extraction solvent. 3. Wet down the herb with the extraction agent at a volume ratio of 1:1 and stir the mixture thoroughly to ensure even dispersion. 4. Pack the wetted herb into the selected percolators. 5. Add the extraction agent to the percolators at a volume ratio of 1.7:1. 6. Allow the menstruum to pass through the percolator. 7. Start the maceration for 48 hours. 8. Open the tap to collect the liquid. 9. Press the herb and collect the liquid. 10.Combine the liquid obtained from the percolator and the pressor. 11.The liquid is then filtered to yield hydroethanolic extract of Echinacea and Kava. 12. Heat the hydroethanolic extract of Echinacea or Kava until the ethanol content is below 1%, resulting in an ethanol concentrate of Echinacea or Kava. 13. Add glycerin to the above ethanol concentrate, with the amount being equal to the volume lost during the heating process to evaporate the ethanol. 14. Mix thoroughly, then filter to obtain the finished product of Glycetract of Echinacea or Kava. The active ingredients in the glycetract products prepared by the conventional extraction using ethanol and the invention using polyols were compared, with results shown in Table 1 and Table 2. Table 1 Comparison of the extraction rate of alkylamide in Echinacea Glycetract Extraction Extraction rate (%) Recovery rate after heating to evaporate ethanol and re-dissolving with glycerin (%) Overall extraction rate (%) Conventional method using ethanol percolation or maceration 0.20 50 0.10 Invention using ultrasonic 0.19 - 0.19 2024259896   11 Nov 2024 propylene glycol heating 0.18 - 0.18 percolation or maceration 0.17 - 0.17 Invention using glycerin percolation or maceration 0.11 - 0.11 ultrasonic 0.08 - 0.08 heating 0.06 - 0.06 In Table 1, during the conventional percolation or maceration using ethanol, the extraction rate of alkylamide from Echinacea is the highest, reaching 0.2%. However, during the heating step to evaporate ethanol, 50% of the alkylamide was lost, resulting in an overall extraction rate of 0.1%. In contrast, using the method of this invention, the extraction rate of alkylamide from Echinacea was 0.19% when extracted with ultrasonic treatment using propylene glycol, which is comparable to that of ethanol extraction. The extraction rates of alkylamide were 0.18% and 0.17% when using propylene glycol by heating and percolation / maceration methods, respectively. Although these rates are slightly lower than that of ethanol extraction, the method of this invention allows for direct extraction, eliminating the heating and re-dissolving steps. As a result, the overall extraction rates remain at 0.19%, 0.18%, and 0.17%, significantly higher than the current conventional ethanol extraction method's rate of 0.1%. When using the method of the invention with glycerin for extraction, the extraction rate of alkylamide from Echinacea is significantly lower than that obtained with ethanol extraction. Among these, the overall extraction rate of glycerin by ultrasonic extraction is 0.11%, which is still higher than that of the conventional method using ethanol. Therefore, propylene glycol is the preferred choice of solvent for Echinacea Glycetract. Table 2 Comparison of Kavalactone Extraction Rates in Kava Glycetract Extraction Extraction rate (%) Recovery rate after heating to evaporate ethanol and re-dissolving with glycerin (%) Overall extraction rate (%) Conventional method using percolation or maceration 4.21 65 2.74 2024259896   11 Nov 2024 ethanol Invention using propylene glycol ultrasonic 3.91 - 3.91 heating 3.75 - 3.75 percolation or maceration 3.62 - 3.42 Invention using glycerin percolation or maceration 2.39 - 2.39 ultrasonic 2.18 - 2.18 heating 1.39 - 1.39 In Table 2, during the conventional ethanol percolation or maceration, the extraction rate of kavalactone in Kava was the highest, reaching 4.21%. However, after the evaporation of ethanol, there was a loss of 35% of kavalactone, resulting in an overall extraction rate of 2.74%. In the method of this invention, when using propylene glycol for ultrasonic extraction, the extraction rate of kavalactone in Kava was 3.91%, which is close to that of ethanol extraction. The extraction rates when using propylene glycol for heating and percolation / maceration were 3.75% and 3.62%, slightly lower than that of ethanol extraction. Since the methods of this invention involves direct extraction without the steps of evaporating ethanol and re-dissolving, the overall extraction rates remain at 3.91%, 3.75%, and 3.62%, which are significantly higher than the conventional ethanol extraction method's 2.74%. When using the methods of this invention to extract kavalactone from Kava with glycerol, the extraction rate is significantly lower than that achieved with ethanol extraction. The overall extraction rate using glycerin for ultrasonic extraction is 2.39%, which is slightly lower than the conventional ethanol extraction method's rate of 2.74%. Therefore, propylene glycol is the preferred choice of solvent for Kava Glycetract. The manufacturing process provided by this invention significantly increases the content of active ingredients in the Glycetract products, improves production efficiency, and reduces production costs. It also notably enhances safety in the production environment and promotes environmental sustainability and protection. This enables the industrial scale and commercialisation of Glycetract products. Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention, but not to limit it. Although the present invention 2024259896   11 Nov 2024 has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: The technical solutions described in the foregoing embodiments can still be modified, or some or all of the technical features can be equivalently replaced; and these modifications or substitutions do not deviate from the essence of the corresponding technical solutions from the technical solutions of the embodiments of the present invention.

Claims

2024259896   11 Nov 2024WHAT WE CLAIM IS1. A manufacturing process for preparing a herbal medicine, Glycetract, characterised by using polyols as the extraction solvent, combined with ultrasonic treatment, heating, or percolation / maceration.

2. The manufacturing process for preparing a herbal medicine, Glycetract, according to claim 1, characterised in that the polyol is selected from the group including propylene glycol and glycerin.

3. The manufacturing process for preparing a herbal medicine, Glycetract, according to claim1, characterised by comprising the following steps:S1> Preparation of herbal materials and solventMilling the herbal material and passing it through a 50-200 mesh sieve.Preparing an aqueous solution of polyol to be used as the extraction solvent.S2> ExtractionAdding the aqueous solution of polyol to the herbal material, wherein the volume concentration of the polyol is 20-100% v / v and stirring thoroughly.Performing ultrasonic treatment; and / or conducting heating treatment; and / or carrying out percolation / maceration treatment at room temperature.Placing the obtained herbal extract solution into a centrifuge for centrifugation to allow the herbal residue to settle at the bottom and separating the supernatant; filtering the supernatant to obtain the herbal medicine Glycetract.

4. The method for preparing a herbal medicine, Glycetract, according to claim 3, characterised in that, in step S2, the solvent and herbal material are mixed in a volume ratio ranging from 3:1 to 10:1.

5. The manufacturing process for preparing a herbal medicine, Glycetract, according to claim 3, characterised in that, in step S2, ultrasonic treatment is performed using an ultrasonic processing device with a frequency range of 18-100 kHz for 0.5 to 3 hours, with the temperature controlled at 60°C ± 5°C.

6. The method for preparing a herbal medicine, Glycetract, according to claim 3, characterised in that, in step S2, heating treatment is conducted for 6 to 12 hours, with the temperature controlled at 60°C ± 5°C.

7. The method for preparing a herbal medicine, Glycetract, according to claim 3, characterised in that, in step S2, percolation / maceration treatment is conducted at room temperature for 1 to 3 weeks.

8. A herbal medicine, Glycetract, prepared by any of the preparation methods described in claims 1 to 6.