Active ingredients of throat-clearing and throat-moistening lozenge and preparation method and application thereof

Abstract

This invention relates to the fields of food and health food, and provides a throat-soothing lozenge, its preparation method, and its application. The preparation method involves water extraction of honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit, using a specific range of alcohol precipitation temperature and settling time to maximize the retention of the active ingredients chlorogenic acid and total saponins, ensuring the product's efficacy, improving its quality, and generating significant economic and social benefits. Products made using the active ingredients of this invention have promising applications in improving oral and / or throat health.

Description

Technical Field

[0001] This invention relates to an active ingredient in a throat-soothing lozenge, its preparation method, and its application, belonging to the field of food and health food. Background Technology

[0002] The water extraction and alcohol precipitation process of traditional Chinese medicine is a key technical step in the extraction and purification of Chinese medicinal herbs. Its core lies in effectively separating the active ingredients from impurities by controlling the ethanol concentration and temperature. In existing technologies, the selection range for alcohol precipitation temperature is relatively wide, generally between 0℃ and 60℃. Temperature control has a significant impact on the retention of active ingredients and the removal of impurities. For example, the study "Alcohol Precipitation, Deproteinization Process and Antioxidant Activity of Pine Needle Polysaccharide from Cedarwood" investigated the effect of different alcohol precipitation temperatures on the polysaccharide yield, including 20℃, 40℃, and 60℃. The experimental results showed that the alcohol precipitation temperature had a significant impact on the polysaccharide yield, with a higher yield at 40℃. This indicates that within the range of 0℃ to 60℃, temperature variations affect the retention of active ingredients. The study "Optimization of Alcohol Precipitation Process of Honeysuckle and Artemisia annua (Jinqing) in Retoxin Injection using Box-Behnken Response Surface Methodology" investigated the effect of settling temperature on the alcohol precipitation effect when optimizing the alcohol precipitation process of Retoxin Injection, finding that 30℃ is a suitable settling temperature. The study "Optimization of Alcohol Precipitation Process of Honeysuckle Extract in Qingkailing Injection using Orthogonal Experimental Method" investigated the effect of the temperature of the decoction when adding alcohol on the alcohol precipitation effect when optimizing the alcohol precipitation process of honeysuckle extract, an intermediate in Qingkailing Injection, ultimately determining the optimal alcohol precipitation process parameters as a decoction temperature of 20℃ when adding alcohol. At this temperature, the loss of active ingredients is minimal, the precipitation and settling rates are moderate, and the settling time is reasonable. Furthermore, patent CN105353800A (A Method for Controlling Cold Settling Temperature in the Alcohol Precipitation Process of Traditional Chinese Medicine) proposes that the cold settling temperature range can be set from 0℃ to 15℃ during the alcohol precipitation process of traditional Chinese medicine to ensure sufficient precipitate and rapid sedimentation of impurities. These studies indicate that controlling the alcohol precipitation temperature has a significant impact on the retention of active ingredients and the removal of impurities. Low-temperature alcohol precipitation helps reduce the solubility of impurities, thereby improving the purity of the extract. However, excessively low temperatures may lead to the loss of some active ingredients, affecting the efficacy of the final product. High-temperature alcohol precipitation, on the other hand, can accelerate the precipitation process of impurities and improve precipitation efficiency. However, excessively high temperatures may damage heat-sensitive active ingredients, reducing the quality and stability of the extract.

[0003] Patent CN111097002A discloses a throat-soothing and moisturizing traditional Chinese medicine composition made from medicinal and edible herbs such as honeysuckle, scrophularia, and chebula. The preparation process includes water extraction, alcohol precipitation, and concentration. The alcohol precipitation process uses 70% ethanol at a temperature of 2-10℃ and a settling time of 48 hours. While this method can achieve the enrichment of active ingredients and the removal of impurities, researchers have found the following problems in industrial production: 1) The original alcohol precipitation temperature of 2-10℃ is prone to instability due to temperature fluctuations in large-scale production, resulting in significant differences in active ingredients (such as chlorogenic acid and total saponins) and yield between different batches of products. 2) The original settling time of 48 hours is too narrow, failing to fully consider the impact of differences in herbal components on sedimentation kinetics and lacking control over the settling time range, which is detrimental to parameter control in large-scale production. Summary of the Invention

[0004] Based on the technology of patent CN111097002A, this invention further studies the alcohol precipitation process, reduces the fluctuation of the yield and effective ingredients, further improves the stability of product batches during mass production, and improves product quality.

[0005] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0006] A method for preparing the active ingredient of a throat-soothing lozenge includes the following steps:

[0007] Take honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit according to the formula, decoct and extract to obtain the extract:

[0008] After concentrating the extract, add ethanol to make the alcohol content 70%, and let it stand at 7-9℃ for 24-60 hours to carry out alcohol precipitation.

[0009] After alcohol precipitation, the mixture is filtered, concentrated, and dried to obtain a dry paste. The dry paste, together with menthol, constitutes the active ingredient of the throat lozenge.

[0010] Further, the formula is as follows: honeysuckle 30-42 parts; scrophularia 30-42 parts; Terminalia chebula 25-35 parts; platycodon 15-21 parts; amla 15-21 parts; monk fruit 2.5-3.5 parts; menthol 0.1-0.14 parts.

[0011] Furthermore, the formula is as follows: 30 parts honeysuckle; 42 parts scrophularia; 25 parts Terminalia chebula; 21 parts platycodon; 15 parts amla; 3.5 parts monk fruit; and 0.1 parts menthol.

[0012] Furthermore, the formula is as follows: 42 parts honeysuckle; 30 parts scrophularia; 35 parts Terminalia chebula; 15 parts platycodon; 21 parts amla; 2.5 parts monk fruit; and 0.14 parts menthol.

[0013] Furthermore, the formula is as follows: 36 parts honeysuckle; 36 parts scrophularia; 30 parts Terminalia chebula; 18 parts platycodon; 18 parts amla; 3 parts monk fruit; and 0.12 parts menthol.

[0014] Furthermore, the decoction extraction involves two extractions with water, each lasting one hour. The first extraction uses 12 times the amount of water, and the second extraction uses 10 times the amount of water.

[0015] Furthermore, the conditions for concentrating the extract were a temperature of 60–80°C and a vacuum of 0.04–0.08 MPa, resulting in a relative density of 1.08–1.12 for the clear extract.

[0016] Furthermore, the conditions for concentrating the filtrate after alcohol precipitation are a temperature of 60–80°C and a vacuum of 0.04–0.08 MPa, resulting in a viscous paste with a relative density of 1.20–1.30.

[0017] Compared to existing technologies, this invention uses water extraction to extract honeysuckle, scrophularia, chebula, platycodon, emblica, and monk fruit, employing a specific alcohol precipitation temperature range and time. This makes the entire preparation process more stable, reducing batch-to-batch variations caused by alcohol precipitation temperature fluctuations in large-scale production and ensuring product quality stability. Furthermore, the specific alcohol precipitation temperature range of this invention not only significantly increases the yield of the dry extract but also maximizes the retention of active ingredients chlorogenic acid and total saponins. This enhances the throat-soothing and moisturizing effects of the lozenges, better relieving throat discomfort symptoms, improving product quality and efficacy, and contributing to increased market competitiveness and significant economic and social benefits.

[0018] The present invention also provides an active ingredient for a throat lozenge, which is prepared by the above-described preparation method.

[0019] The present invention also provides a method for preparing a throat-soothing lozenge, wherein the active ingredients of the above-mentioned throat-soothing lozenge are combined with excipients, lubricants and sweeteners to form tablets using conventional formulation methods.

[0020] Furthermore, the excipients include lactose, dextrin, and erythritol.

[0021] Furthermore, the lubricant is magnesium stearate, and the sweetener is sucralose.

[0022] Furthermore, the present invention also provides the application of the above-mentioned active ingredients of the throat lozenges in the preparation of products for improving oral and / or throat health.

[0023] The synergistic effects of the various medicinal ingredients in this invention, through anti-inflammatory, antibacterial, heat-clearing and detoxifying effects, can, on the one hand, maintain the health of the oral mucosa, reduce bacterial growth, keep the mouth clean and moist, and effectively relieve symptoms such as oral ulcers and oral inflammation, thereby improving oral health; on the other hand, it can reduce inflammation and discomfort in the throat, relieve symptoms such as sore throat, dry throat, hoarseness, cough and difficulty swallowing, thereby improving throat health.

[0024] The research content of the alcohol precipitation process of this invention is as follows:

[0025] I. Investigation of alcohol precipitation temperature

[0026] 1. Sample preparation

[0027] Weigh out 36 kg of honeysuckle, 36 kg of scrophularia, 30 kg of Terminalia chebula, 18 kg of platycodon, 18 kg of amla, and 3 kg of monk fruit. Extract and concentrate with water. Divide the concentrate into 10 equal portions, each yielding 10,000 tablets of 0.8 g / tablet. Take 4 portions of the concentrate and precipitate them with alcohol at 1-3℃, 4-6℃, 7-9℃, and 10-12℃ respectively for 48 hours. After precipitation, filter and collect the filtrate. Recover ethanol under reduced pressure. The mixture was concentrated (at 60°C and under a vacuum of 0.08 MPa) to obtain a thick paste. The thick paste was then dried (at 110°C and under a vacuum of 0.10 MPa) to obtain a dry paste. The dry paste powder, lactose, dextrin, and erythritol were mixed according to conventional formulation methods, granulated, and after granulation, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose were added. The mixture was then mixed evenly, compressed into tablets, and each tablet was weighed 0.8g to obtain throat lozenges.

[0028] 2. Evaluation Indicators

[0029] The yield of the extract and the content of chlorogenic acid and total saponins in the dried extract were measured, and the content of chlorogenic acid and total saponins per 10,000 tablets was calculated. The specific testing methods are as follows:

[0030] (1) Ointment yield

[0031] The calculation formula is: Extract yield (%) = (Weight of dry extract / Weight of medicinal materials) × 100%

[0032] (2) Chlorogenic acid content

[0033] Chromatographic conditions: Column: ODS C18 column, 250 mm × 4.6 mm, 5 μm; Mobile phase: 0.5% acetic acid solution: acetonitrile = 9:1 (V / V); Flow rate: 1.0 mL / min; Column temperature: 35 ℃; Detection wavelength: 327 nm; Injection volume: 10 μL.

[0034] Preparation of standard solution: Weigh 0.02 g of chlorogenic acid standard into a 100.0 mL volumetric flask, dissolve and dilute to volume with the mobile phase, i.e., each mL contains 0.2 mg of chlorogenic acid;

[0035] Preparation of test solution: Take 10 tablets, grind them into a fine powder, weigh 0.2g, put them into a 25.0mL volumetric flask, add 20mL of 70% methanol, sonicate for 30 minutes, dilute to volume with 70% methanol, filter through a 0.45μm microporous membrane, and use the filtrate as the test solution.

[0036] Preparation of standard curve: Take chlorogenic acid standard solution, dilute it with mobile phase and make up to volume in volumetric flasks a series of standard solutions with concentrations of 2.00, 10.0, 20.0, 40.0 and 80.0 μg / mL, respectively, for high performance liquid chromatography determination. Plot the standard curve with the measured peak area as the ordinate and the corresponding standard solution concentration as the abscissa.

[0037] Determination: Inject the standard solution and sample solution into the liquid chromatograph, determine the content of chlorogenic acid in the sample, and calculate the result.

[0038] (3) Total saponins were determined by the following ultraviolet-visible spectrophotometric method.

[0039] 1) Preparation of standard solution: Weigh 0.020 g of ginsenoside Re standard, dissolve it in methanol and make up to 10.0 mL, that is, each mL contains 2.0 mg of ginsenoside Re;

[0040] 2) Preparation of test solution: Take 10 tablets, grind them into a fine powder, take 1.5g, put them into a 100mL volumetric flask, add 70mL of water, sonicate for 40 minutes, then dilute to 100mL with water, let stand, and use the supernatant as the test solution.

[0041] 3) Column chromatography: Use a glass chromatography column packed with 3 cm of Amberlite-XAD-2 macroporous resin and topped with 1 cm of neutral alumina. First, wash the column with 25 mL of 70% ethanol and discard the eluent. Then, wash the column with 25 mL of water and discard the eluent. Add 1.0 mL of the test solution, wash the column with 25 mL of water and discard the eluent. Elute the ginsenosides with 25 mL of 70% ethanol, collect the eluent in an evaporating dish, and evaporate to dryness in a 60°C water bath.

[0042] 4) Color reaction: Add 0.2 mL of 5% vanillin-glacial acetic acid solution to the evaporated dish to dissolve the residue, then add 0.8 mL of perchloric acid, transfer to a 5 mL stoppered graduated centrifuge tube, heat in a 60°C water bath for 10 minutes, cool in an ice bath, and then add 5.0 mL of glacial acetic acid to obtain the final product.

[0043] 5) Determination: Perform column chromatography and colorimetric reaction on the standard solution using the same method as in steps 3) and 4). Measure the absorbance at 560 nm using UV-Vis spectrophotometry and calculate the total saponin content in the sample.

[0044] 3. Test Results

[0045] The results of extract yield, chlorogenic acid content, and total saponin content at different alcohol precipitation temperatures are shown in the table below:

[0046]

[0047] The above experimental results show that as the alcohol precipitation temperature increases, the yield of the extract increases, the chlorogenic acid content in the dry extract decreases, and the total saponin content in the dry extract does not change significantly. An alcohol precipitation temperature of 7-9℃ results in a moderate yield and the highest chlorogenic acid content per 10,000 tablets; an alcohol precipitation temperature of 4-6℃ results in the highest chlorogenic acid content per gram of dry extract, but a lower yield and the lowest effective ingredient content per 10,000 tablets; an alcohol precipitation temperature of 10-12℃ results in the highest yield, but the lowest chlorogenic acid content per gram of dry extract and the lowest effective ingredient content per 10,000 tablets compared to experiment #3; an alcohol precipitation temperature of 1-3℃ results in a low yield, and no content determination was performed. The alcohol precipitation temperature has a significant impact on the yield and content determination of this product. Considering both the yield and the effective ingredient content, experiment #3, with an alcohol precipitation temperature controlled at 7-9℃, is selected as the optimal alcohol precipitation temperature for this product.

[0048] Analyzing experiments 1-4 from the perspective of relative standard deviation, the RSD value of the yield of the product reached 38.01% at alcohol precipitation temperatures of 1-12℃; the RSD value of chlorogenic acid content per 10,000 tablets was as high as 26.24%, and the RSD value of total saponin content was 36.48%; the RSD value of chlorogenic acid content in the dry paste was 16.78%, indicating that the above-mentioned indicators have a high degree of dispersion and poor repeatability between product batches.

[0049] II. Investigation of alcohol precipitation settling time

[0050] The settling time of alcohol precipitation is also an important factor affecting the effect of alcohol precipitation. If the settling time is too short, the precipitation will be incomplete, and sometimes there may be suspension. The alcohol precipitation liquid will be turbid, which will affect filtration and lead to instability in the yield and content of the extract. If the alcohol precipitation time is too long, it may affect the content of active ingredients, breed bacteria and other microorganisms, and increase production costs due to the long time consumption. Therefore, it is necessary to determine the appropriate alcohol precipitation settling time according to the specific formulation.

[0051] 1. Experimental Research

[0052] Five samples prepared under the alcohol precipitation temperature test were subjected to alcohol precipitation at 7-9℃. The samples were allowed to stand for 24h, 36h, 48h, 60h, and 72h respectively. After precipitation, the samples were filtered, and the filtrate was collected. Ethanol was recovered under reduced pressure and concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste. The paste was dried (temperature 110℃, vacuum degree 0.10MPa) to obtain a dry paste. Following conventional formulation methods, the dry paste powder, lactose, dextrin, and erythritol were mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose were added, mixed thoroughly, and compressed into tablets, with each tablet weighing 0.8g.

[0053] 2. Evaluation Indicators

[0054] The yield of the extract and the content of chlorogenic acid and total saponins in the dry extract, as well as the content of chlorogenic acid and total saponins per 10,000 tablets, were calculated and determined according to the detection method under the alcohol precipitation temperature section. An additional indicator for the properties of the alcohol precipitation solution was added, mainly observing the ease of filtration and whether it was clear.

[0055] 3. Test Results

[0056] At the same alcohol precipitation temperature and with standing times of 12h, 24h, 36h, 48h, 60h, and 72h, the yield of the dry extract, chlorogenic acid content, total saponin content, and filtration results are shown in the table below:

[0057]

[0058] The above experimental results show that, under constant alcohol precipitation temperature, the alcohol precipitates in experiments 1 and 2, after standing for 12 hours and 24 hours respectively, exhibited turbidity, easily clogging the filter, resulting in slow processing, significant waste, and lower chlorogenic acid and total saponin content per 10,000 tablets. In experiments 3-6, the alcohol precipitates, after standing for 36 hours, 48 ​​hours, 60 hours, and 72 hours respectively, were clear with no suspended particles, showed no obvious filter clogging, and exhibited similar yield and chlorogenic acid and total saponin content per 10,000 tablets. Considering all test results and production costs, the optimal standing time for the alcohol precipitate was determined to be 24-60 hours. Detailed Implementation

[0059] Weigh out the medicinal materials required for preparing 10,000 tablets of the product, in a total of 6 portions, and prepare the samples within the determined range of alcohol precipitation temperature and time. Calculate the relative standard deviations of the extract yield, chlorogenic acid content, and total saponin content to verify the stability and accuracy of the alcohol precipitation process of this invention.

[0060] Example 1

[0061] This embodiment provides a method for preparing the active ingredients of throat lozenges, using an alcohol precipitation temperature of 7-9℃ and a settling time of 48 hours, specifically including the following steps:

[0062] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0063] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0064] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0065] Add ethanol to the clear paste to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 48 hours to carry out alcohol precipitation;

[0066] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0067] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0068] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0069] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0070] Example 2

[0071] This embodiment provides a method for preparing the active ingredients of throat lozenges, using an alcohol precipitation temperature of 7-9℃ and a settling time of 24 hours, specifically including the following steps:

[0072] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0073] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0074] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0075] Add ethanol to the clear extract to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 24 hours to carry out alcohol precipitation;

[0076] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and the mixture was concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0077] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0078] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0079] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0080] Example 3

[0081] This embodiment provides a method for preparing the active ingredient of a throat-soothing lozenge, using an alcohol precipitation temperature of 7-9℃ and a settling time of 36 hours, specifically including the following steps:

[0082] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0083] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0084] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0085] Add ethanol to the clear paste to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 36 hours to carry out alcohol precipitation;

[0086] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and the mixture was concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0087] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0088] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0089] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0090] Example 4

[0091] This embodiment provides a method for preparing the active ingredients of throat lozenges, using an alcohol precipitation temperature of 7-9℃ and a settling time of 60 hours, specifically including the following steps:

[0092] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0093] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0094] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0095] Add ethanol to the clear paste to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 60 hours to carry out alcohol precipitation;

[0096] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and the mixture was concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0097] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0098] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0099] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0100] Example 5

[0101] This embodiment provides a method for preparing the active ingredients of throat lozenges, using an alcohol precipitation temperature of 7-9℃ and a settling time of 54 hours, specifically including the following steps:

[0102] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0103] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0104] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0105] Add ethanol to the clear extract to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 54 hours to carry out alcohol precipitation;

[0106] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0107] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0108] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0109] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0110] Example 6

[0111] This embodiment provides a method for preparing the active ingredients of throat lozenges, using an alcohol precipitation temperature of 7-9℃ and a settling time of 30 hours, specifically including the following steps:

[0112] Formula: Honeysuckle 3.6kg; Scrophularia ningpoensis 3.6kg; Terminalia chebula 3kg; Platycodon grandiflorus 1.8kg; Phyllanthus emblica 1.8kg; Monk fruit 0.3kg.

[0113] Weigh out the following ingredients according to the formula: honeysuckle, scrophularia, terminalia fruit, platycodon, amla, and monk fruit. Extract twice with water, one hour each time. Add 12 times the amount of water for the first extraction and 10 times the amount of water for the second extraction. Filter the extract and set aside.

[0114] The extract was concentrated under reduced pressure (temperature 60℃, vacuum degree 0.08Mpa) to obtain a clear extract with a relative density of 1.08 to 1.12.

[0115] Add ethanol to the clear extract to make the alcohol content 70%, stir well, and let it stand at 7-9℃ for 30 hours to carry out alcohol precipitation;

[0116] After alcohol precipitation, the mixture was filtered, and the filtrate was collected. The ethanol was recovered under reduced pressure and concentrated (temperature 60℃, vacuum degree 0.08MPa) to obtain a thick paste with a relative density of 1.20 to 1.30.

[0117] The thick paste was dried and pulverized using a vacuum belt dryer (heating plate temperature of 110℃ and vacuum degree of 0.10MPa) to obtain a dry paste powder.

[0118] This embodiment also provides a method for preparing the throat-soothing lozenge, as follows:

[0119] Following conventional preparation methods, dry powder, lactose, dextrin, and erythritol are mixed, granulated, and sized. Then, 12g of menthol powder, appropriate amounts of magnesium stearate and sucralose are added, mixed evenly, and compressed into tablets, with each tablet weighing 0.8g, to obtain throat-soothing lozenges.

[0120] Examples 1-6 were tested according to the detection indicators under the alcohol precipitation settling time test. The ease of filtration of the alcohol precipitate and whether it became clear were observed. The yield of the paste and the content of chlorogenic acid and total saponins in the dry paste, the content of chlorogenic acid and total saponins per 10,000 tablets, and their relative standard deviations were calculated. The results are as follows:

[0121]

[0122] As shown in the table above, when six batches of samples were prepared at an alcohol precipitation temperature of 7-9℃ and a standing time of 24-60h, the RSD values ​​of the yield, chlorogenic acid content, and total saponin content were all less than 5%, which is much lower than the RSD values ​​of each indicator when the alcohol precipitation temperature was 1-12℃. This indicates that the alcohol precipitation temperature has a significant impact on the alcohol precipitation process. Products prepared using the alcohol precipitation parameters determined in this invention have better batch-to-batch stability, higher accuracy, and more stable quality, effectively solving the problems of large fluctuations in the yield and unstable content of the product during the production process.

[0123] The above technical content is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions or improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing the active ingredient of a throat-soothing lozenge, characterized in that, Includes the following steps: Take honeysuckle, scrophularia, chebula, platycodon, amla and monk fruit according to the formula, decoct and extract to obtain the extract; After concentrating the extract, add ethanol to make the alcohol content 70%, and let it stand at 7-9℃ for 24-60 hours to carry out alcohol precipitation. After alcohol precipitation, the mixture is filtered, concentrated, and dried to obtain a dry paste. The dry paste, together with menthol, constitutes the active ingredient of the throat lozenge.

2. The method for preparing the active ingredient of the throat lozenge as described in claim 1, characterized in that, The formula is as follows: honeysuckle 30-42 parts; scrophularia 30-42 parts; Terminalia chebula 25-35 parts; platycodon 15-21 parts; amla 15-21 parts; monk fruit 2.5-3.5 parts; menthol 0.1-0.14 parts.

3. The method for preparing the active ingredient of the throat-soothing lozenge as described in claim 2, characterized in that, The formula is as follows: Honeysuckle 30 parts; Scrophularia ningpoensis 42 parts; Terminalia chebula 25 parts; Platycodon grandiflorus 21 parts; Phyllanthus emblica 15 parts; Siraitia grosvenorii 3.5 parts; Menthol 0.1 parts.

4. The method for preparing the active ingredient of the throat-soothing lozenge as described in claim 2, characterized in that, The formula ratio is as follows: honeysuckle 36 parts; scrophularia 36 parts; Terminalia chebula 30 parts; platycodon 18 parts; amla 18 parts; monk fruit 3 parts; menthol 0.12 parts.

5. The method for preparing the active ingredient of the throat-soothing lozenge as described in claim 1, characterized in that, The decoction extraction involves two extractions with water, each lasting one hour. The first extraction uses 12 times the amount of water, and the second extraction uses 10 times the amount of water.

6. The method for preparing the active ingredient of the throat-soothing lozenge as described in claim 1, characterized in that, The conditions for concentrating the extract were a temperature of 60–80℃ and a vacuum of 0.04–0.08 MPa, and the relative density of the resulting clear extract was 1.08–1.

12.

7. The method for preparing the active ingredient of the throat lozenge as described in claim 1, characterized in that, The conditions for concentrating the filtrate after alcohol precipitation are a temperature of 60–80℃ and a vacuum of 0.04–0.08 MPa, and the relative density of the resulting thick paste is 1.20–1.

30.

8. An active ingredient in a throat lozenge, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 7.

9. A method for preparing a throat-soothing lozenge, characterized in that, The active ingredients of the throat-soothing lozenges according to claim 8, together with excipients, lubricants and sweeteners, are prepared into tablets using conventional formulation methods.

10. The use of the active ingredient of the throat lozenge according to claim 8 in the preparation of products for improving oral and / or throat health.

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