Functional throat moistening candy of immature bitter orange based on high naringin content and preparation process thereof

Abstract

This invention discloses a functional throat lozenge based on high naringin content Citrus reticulata extract and its preparation process, relating to the field of food processing technology. This invention uses Citrus reticulata extract as the principal ingredient, combined with Citrus reticulata peel extract and Luo Han Guo concentrated juice as assistant ingredients, Ophiopogon japonicus extract and Glycyrrhiza uralensis extract as adjuvant ingredients, and menthol as the guiding ingredient. The principal ingredient targets and addresses the core symptoms of excessive phlegm and throat obstruction. The assistant ingredients synergistically enhance the effects of expectoration, cough relief, lung clearing, and throat soothing. The adjuvant ingredients counteract the warming and drying properties of the principal and assistant ingredients, compensating for their biases and guiding the medicinal effects upward to the throat. Simultaneously, the effects of each ingredient complement each other, fundamentally solving the problems of chaotic formulations, unclear core effects, and easy depletion of body fluids in existing products. This results in a product that is mild in nature and suitable for long-term consumption, possessing expectoration, cough relief, throat clearing, and throat soothing effects.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, specifically to functional throat lozenges based on high naringin content citrus peel and their preparation process. Background Technology

[0002] Functional throat lozenges, as a snack food for relieving throat discomfort, have seen continuous growth in market demand. Currently, commercially available throat lozenges mainly fall into two categories: one type uses cooling agents such as menthol and eucalyptus oil as the main ingredients, temporarily masking throat discomfort through physical cooling; the other type adds extracts of some traditional Chinese medicine herbs for soothing and moisturizing the throat. However, existing products generally suffer from problems such as limited efficacy, unclear mechanisms of action, and difficulty in balancing taste and efficacy, failing to meet consumers' demand for healthy foods that combine significant efficacy with a good taste.

[0003] The existing functional throat lozenges have the following technical defects: The lack of synergistic mechanisms among the ingredients leads to unstable product efficacy, making it difficult to fundamentally relieve symptoms such as excessive phlegm, cough, and sore throat.

[0004] Insufficient processing of the drying properties of Chinese medicinal materials, such as the use of warm and drying herbs like tangerine peel and dried tangerine peel without proper formulation, can easily deplete body fluids with long-term use, leading to discomfort such as dry mouth and throat, thus reducing the product's target audience.

[0005] The products are limited in form, mostly traditional hard candies or lozenges. The inherent bitterness of the Chinese medicinal herbs is difficult to mask, requiring the addition of large amounts of artificial sweeteners or flavorings to correct the taste, which contradicts the current consumer philosophy of pursuing natural and healthy products.

[0006] Currently, the research and development of functional throat lozenges still faces technical challenges such as unscientific formulation, low retention rate of effective ingredients, and poor taste. Therefore, developing a product with clear efficacy, mild properties, and excellent taste has become an urgent problem to be solved in this field. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a functional throat lozenge based on high naringin content Citrus reticulata extract and its preparation process. It utilizes Citrus reticulata extract as the principal ingredient, rich in naringin, which has strong expectorant, antitussive, and qi-regulating effects, playing a core therapeutic role in symptoms such as excessive phlegm, cough, and throat obstruction. It uses Citrus reticulata extract and Luo Han Guo concentrated juice as secondary ingredients; Citrus reticulata assists the principal ingredient in enhancing its expectorant and qi-regulating effects, while Luo Han Guo clears heat, moistens the lungs, soothes the throat, and improves voice; its natural sweetness reduces the need for artificial sweeteners. It also includes Ophiopogon japonicus extract. With licorice extract as an adjuvant, Ophiopogon japonicus nourishes yin and moistens the lungs, benefits the stomach and promotes the production of body fluids, and plays an auxiliary role in addressing the drawbacks of the warm and drying herbs such as Citrus reticulata peel and Citrus tangerine peel that easily deplete body fluids. Licorice tonifies the spleen and replenishes qi, eliminates phlegm and relieves cough, and can harmonize the properties of various herbs. Menthol is used as the guiding herb, and its cooling sensation can directly act on the throat, guiding the medicine upward and providing immediate relief. The various active ingredients form a synergistic effect mechanism, which not only ensures the product's significant efficacy for symptoms such as throat discomfort, excessive phlegm and cough, but also avoids the side effects caused by long-term use of a single warm and drying herb, thus expanding the product's applicable population.

[0008] To solve the above-mentioned technical problems, the present invention provides the following technical solution: On one hand, a functional throat lozenge based on high naringin content citrus peel, the throat lozenge being composed of active ingredients and food-grade excipients, with the following mass percentages for each ingredient: Active ingredients: Citrus reticulata extract 30%, Citrus reticulata peel extract 15%, Monk fruit concentrate 8%, Ophiopogon japonicus extract 15%, Glycyrrhiza uralensis extract 10%, Menthol 0.5%; Food-grade excipients: sweet base 20%-21%, lubricant 0.5%-1%, filler and binder 0%-1%.

[0009] Furthermore, the sweet base is a combination of honey powder and rock sugar powder, or isomalt; when the sweet base is a combination of honey powder and rock sugar powder, the mass percentage of honey powder is 10%-10.5% and the mass percentage of rock sugar powder is 10%-10.5%.

[0010] Furthermore, the lubricant is food-grade magnesium stearate, and the filler binder is food-grade microcrystalline cellulose.

[0011] Furthermore, the naringin content in the Citrus reticulata extract is ≥10% by mass; The glycyrrhizic acid content in the licorice extract is ≥5% by mass. The mogroside content in the concentrated mogroside juice is ≥1%.

[0012] Furthermore, the moisture content of the finished throat lozenge is ≤5.0%, and the disintegration time is 10-30 minutes.

[0013] Furthermore, the preparation steps of the Citrus reticulata extract are as follows: The cleaned raw material of Citrus reticulata is washed, dried and crushed to obtain Citrus reticulata coarse powder of 20-40 mesh; The obtained crude tangerine peel powder was put into an extraction tank, and 8-12 times the amount of solvent was added. Dynamic countercurrent extraction was carried out at 70-95℃ for 2-3 times, each time for 1-2 hours. The extracts were then combined. The obtained extract was filtered, and the filtrate was concentrated under vacuum at 60-65℃ to a thick paste with a relative density of 1.10-1.15, thus obtaining the Citrus reticulata extract. The solvent is purified water or an ethanol-water solution with a volume fraction of 30%-50%.

[0014] On the other hand, based on the preparation process of functional throat lozenges with high naringin content, the steps of this preparation process are as follows: S100. Raw material pretreatment: The raw materials of Citrus reticulata peel, dried tangerine peel, licorice, and Ophiopogon japonicus are cleaned, washed, dried, and pulverized to obtain raw material powder of 20-40 mesh; the raw material of Luo Han Guo is processed by breaking the shell and removing the pulp to obtain Luo Han Guo raw material. S200, Extraction of effective components: Combine the raw material powders of Citrus reticulata peel, Citrus reticulata peel, Glycyrrhiza uralensis and Ophiopogon japonicus obtained from S100, and use extraction technology to extract the effective components to obtain a mixed extract. Separately extract the raw material of Siraitia grosvenorii to obtain Siraitia grosvenorii extract. S300. Concentration and purification of extract: Vacuum low-temperature concentration and purification of the obtained mixed extract to obtain mixed Chinese herbal extract; concentration of the obtained monk fruit extract to obtain monk fruit concentrate. S400, Ingredients and Mixing: Add the obtained mixed Chinese herbal extract, Luo Han Guo concentrated juice, sweet matrix and filler binder into a jacketed kettle, mix evenly to obtain a soft material; S500, Granulation and Drying: The obtained soft material is granulated and dried at low temperature to obtain dried granules. Menthol and lubricant are added to the dried granules, and after being fully mixed, they are compressed into tablets to obtain throat lozenges. S600 Packaging and Storage Procedures: Seal the throat lozenges and store them in a cool, dry place.

[0015] Furthermore, in step S200, the extraction technique is any one of dynamic countercurrent extraction, ultrasound-assisted extraction, or thermal reflux extraction; The solvent used for extraction is purified water or an ethanol-water solution with a volume fraction of 30%-50%; The extraction process parameters are as follows: material-liquid ratio 1:8~1:12, water extraction temperature 85-95℃, alcohol extraction temperature 70-80℃, extraction times 2-3 times, extraction time 1-2 hours per extraction.

[0016] Furthermore, in S300, the vacuum low-temperature concentration process is carried out at a temperature of 60-65°C, and the relative density of the mixed Chinese herbal extract obtained after concentration is 1.10-1.15. The relative density is detected at 25°C. The purification process employs centrifugal separation or membrane filtration technology to remove macromolecular impurities from the extract.

[0017] Compared with existing technologies, this functional throat lozenge based on high naringin content tangerine peel and its preparation process have the following beneficial effects: I. This invention uses Citrus reticulata peel extract as the principal ingredient, which is rich in naringin, possessing strong expectorant, antitussive, and qi-regulating effects. It plays a core therapeutic role in treating symptoms such as excessive phlegm, cough, and throat obstruction. Citrus reticulata peel extract and monk fruit concentrate are used as adjuvant ingredients. Citrus reticulata peel assists the principal ingredient in enhancing its expectorant and qi-regulating effects, while monk fruit clears heat, moistens the lungs, soothes the throat, and improves voice. Its natural sweetness reduces the need for artificial sweeteners. Ophiopogon japonicus extract and licorice extract are used as adjuvant ingredients. Ophiopogon japonicus nourishes yin, moistens the lungs, benefits the stomach, and promotes the production of body fluids. This product addresses the drawbacks of warm and drying herbs like tangerine peel and dried tangerine peel, which can easily deplete body fluids. Licorice root tonifies the spleen and replenishes qi, eliminates phlegm and relieves cough, and harmonizes the properties of other herbs. Menthol is used as the guiding herb, and its cooling sensation can directly act on the throat, guiding the medicine upwards and providing immediate relief. The various active ingredients form a synergistic effect, ensuring the product's significant efficacy for symptoms such as throat discomfort, excessive phlegm, and cough, while avoiding the side effects of long-term use of a single warm and drying herb, thus expanding the product's target population.

[0018] II. This invention employs dynamic countercurrent, ultrasonic-assisted, or thermal reflux extraction techniques, using water or ethanol-water solutions as solvents. It precisely controls the material-to-liquid ratio, extraction temperature, and number of extractions to maximize the enrichment of water-soluble and alcohol-soluble active ingredients of naringin in Citrus reticulata peel. Then, through vacuum low-temperature concentration, centrifugation, and membrane filtration purification techniques, it removes large molecular impurities and bitter substances from the extract while protecting the heat-sensitive active ingredients from damage. Combined with the natural sweetness of Luo Han Guo and the taste-correcting effect of the sweet base, it solves the problems of low retention rate of active ingredients and residual bitterness of traditional Chinese medicine. This ensures the stable content of active ingredients in the product and optimizes the taste.

[0019] Other advantages, objectives and features of the invention will be set forth in part in the description which follows, and in part will be apparent to those skilled in the art from the following examination or study, or may be learned from the practice of the invention. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.

[0021] Figure 1 The flowchart shows the preparation process of functional throat lozenges based on high naringin content tangerine peel. Figure 2 This is a flowchart illustrating the preparation steps of the Citrus reticulata extract in this invention. Detailed Implementation

[0022] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with the accompanying drawings and preferred embodiments, is provided below.

[0023] To address the shortcomings of existing functional throat lozenges, such as limited and unstable efficacy, the depletion of body fluids due to the use of warming and drying herbs, difficulty in balancing taste and efficacy, low retention of effective ingredients, and reliance on artificial flavoring, this invention first describes its application scenario. This invention is primarily applied to the research and development and production of functional throat lozenges in the food processing industry. In this scenario, commercially available throat lozenges either rely solely on cooling agents to temporarily mask throat discomfort or use unscientific combinations of Chinese medicinal herbs. These methods fail to fundamentally alleviate symptoms such as excessive phlegm, cough, and sore throat, and also suffer from limitations in the target population and contradict the consumer philosophy of natural health, severely hindering the product upgrade and market development of functional throat lozenges.

[0024] This invention combines the scientific formulation of medicinal and edible raw materials such as Citrus reticulata peel, dried tangerine peel, and monk fruit, the content limitation of highly active ingredients, and efficient extraction and vacuum low-temperature concentration and purification technologies such as dynamic countercurrent extraction. The aim is to achieve functional throat lozenges based on high naringin content Citrus reticulata peel and a suitable preparation process, which have significant efficacy, mild taste, excellent mouthfeel, and high retention rate of effective ingredients.

[0025] Specifically, this invention provides a functional throat lozenge based on high naringin content Citrus reticulata peel extract. By weight percentage, it consists of active ingredients and food-grade excipients. The active ingredients are: Citrus reticulata peel extract 30%, Citrus reticulata peel extract 15%, Luo Han Guo concentrated juice 8%, Ophiopogon japonicus extract 15%, Glycyrrhiza uralensis extract 10%, and Menthol 0.5%. The food-grade excipients are: sweetener base 20%-21%, lubricant 0.5%-1%, and filler / binder 0%-1%. The sweetener base is a combination of honey powder and rock sugar powder or isomaltitol, and the lubricant is food-grade hard... Magnesium fatty acid, the filler binder is food-grade microcrystalline cellulose; the naringin content in the Citrus reticulata extract is ≥10%, the glycyrrhizic acid content in the licorice extract is ≥5%, and the mogroside content in the monk fruit concentrate is ≥1%; the moisture content of the finished throat lozenge is ≤5.0%, the disintegration time is 10-30 min, and the Citrus reticulata extract is obtained by cleaning and pulverizing, dynamic countercurrent extraction with 8-12 times the amount of solvent, filtration, and vacuum concentration at 60-65℃ to a thick paste with a relative density of 1.10-1.15, the solvent being purified water or 30%-50% ethanol-water solution.

[0026] like Figure 1 As shown, the present invention also provides a preparation process for functional throat lozenges based on high naringin content citrus peel, the steps of which are as follows: S100. Raw material pretreatment: Select, wash, dry and grind the tangerine peel, dried tangerine peel, licorice and ophiopogon japonicus into 20-40 mesh powder; and remove the pulp from the shell of the monk fruit. S200. Extraction of active ingredients: Combine the powders of four raw materials, including Citrus reticulata peel, and use dynamic countercurrent, ultrasonic-assisted, or hot reflux extraction technology. Use purified water or 30%-50% ethanol-water solution as solvent, and extract at a material-liquid ratio of 1:8~1:12. Water extraction at 85-95℃ / ethanol extraction at 70-80℃ for 2-3 times, 1-2 hours each time, to obtain a mixed extract. Luo Han Guo is extracted separately to obtain Luo Han Guo extract. S300. Concentration and purification of extract: The mixed extract is concentrated under vacuum at 60-65℃ to a mixed Chinese herbal extract with a relative density of 1.10-1.15 at 25℃, and then purified by centrifugation or membrane filtration. The monk fruit extract is concentrated separately into monk fruit concentrate. S400, Ingredients and Mixing: Mix the Chinese herbal extract, Luo Han Guo concentrated juice, sweet base, and filler binder into a jacketed kettle and mix evenly to obtain a soft material; S500, Granulation and Drying: The soft material is granulated and dried at low temperature. Menthol and lubricant are added to the dried granules, mixed evenly, and then compressed into tablets to obtain throat lozenges. S600 Packaging and Storage: The throat lozenges should be sealed in a sealed package and stored in a cool, dry place.

[0027] At the same time, such as Figure 2 As shown, the present invention also discloses the preparation steps of Citrus reticulata extract as follows: The cleaned raw material of Citrus reticulata is washed, dried and crushed to obtain Citrus reticulata coarse powder of 20-40 mesh; The obtained crude tangerine peel powder is put into an extraction tank, and 8-12 times the amount of purified water or ethanol-water solution with a volume fraction of 30%-50% is added. Dynamic countercurrent extraction is used, and the extraction is carried out 2-3 times at 70-95℃, each time for 1-2 hours. The extracts are combined. The obtained extract was filtered, and the filtrate was concentrated under vacuum at 60-65℃ to a thick paste with a relative density of 1.10-1.15, thus obtaining the Citrus reticulata extract.

[0028] In the specific implementation process, the present invention will be further described in detail below with reference to specific embodiments, comparative examples and effect verification experiments. In all embodiments and comparative examples of the present invention, the raw materials and reagents used are of the same standard: Example 1 This embodiment is a basic preferred embodiment of the present invention. Its core purpose is to verify the feasibility, stability of the preparation process and quality control of conventional sugar-containing functional throat lozenges based on the theory of monarch, minister, assistant and guide in traditional Chinese medicine. This embodiment adopts conventional and mature industrial processes such as hot reflux extraction, vacuum low temperature concentration and fluidized bed drying to prepare basic throat lozenges with the core effects of clearing the throat, moisturizing the throat, resolving phlegm and relieving cough, providing basic parameter support for mass production of the product.

[0029] The functional throat lozenges with high naringin content prepared in this embodiment are based on a total weight of 1000g of finished throat lozenges. The precise ingredient formulas are as follows: 300g of Citrus reticulata extract, 150g of Citrus reticulata peel extract, 80g of Luo Han Guo concentrated juice, 150g of Ophiopogon japonicus extract, 100g of Glycyrrhiza uralensis extract, 5g of Menthol, 105g of Honey powder, 105g of Rock sugar powder, and 5g of Food-grade Magnesium Stearate. The total weight of all ingredients is 1000g, and the total percentage by weight is 100%.

[0030] The preparation process in this embodiment is as follows: Raw material pretreatment steps: Take tangerine peel, dried tangerine peel, licorice, and ophiopogon japonicus as raw materials. First, manually clean them to remove moldy parts, impurities, and non-medicinal parts. After washing twice with purified water, dry them in a 60℃ forced-air drying oven for 4 hours. After the moisture content of the raw materials is tested to be ≤8%, they are discharged. Use a universal pulverizer to pulverize the dried raw materials and pass them through a 30-mesh standard sieve to obtain uniform powder of the four raw materials. Seal and set aside for later use. Take monk fruit, mechanically break the shell to separate the shell and pulp, and take the pulp as monk fruit raw material for later use.

[0031] Extraction steps of effective components: All the raw material powders of Citrus reticulata peel, Citrus reticulata peel, Glycyrrhiza uralensis, and Ophiopogon japonicus obtained from pretreatment were put into a multi-functional extraction tank. Hot reflux extraction technology was used to extract the effective components, with purified water as the extraction solvent. The material-to-liquid ratio was controlled at 1:10. The heating and stirring devices were turned on, and the temperature was raised to 90℃ and then kept at that temperature for extraction. The first extraction lasted 1.5 hours. After extraction, the extract was released. The same proportion of purified water was added to the extraction tank again, and a second extraction was performed with the same parameters for 1.5 hours. The two extracts were combined to obtain a mixed extract. The Luo Han Guo pulp obtained from pretreatment was put into a separate extraction tank and extracted separately using the same hot reflux extraction process to obtain Luo Han Guo extract.

[0032] Concentration and purification steps of the extract: The mixed extract was pumped into a vacuum low-temperature concentration tank, and the concentration temperature was controlled at 62℃ and the vacuum degree inside the tank was -0.08MPa for vacuum concentration. During the concentration process, the relative density of the extract was continuously monitored. The concentration was stopped when the relative density of the mixed Chinese herbal extract was 1.12 at 25℃. The mixed Chinese herbal extract was then sent to a centrifuge and centrifuged at 4000r / min for 15min to remove macromolecular impurities and residues, resulting in a clear mixed Chinese herbal extract, which was then sealed for later use. The monk fruit extract was concentrated using the same vacuum low-temperature concentration process to a monk fruit concentrate with a relative density of 1.10 at 25℃, which was then set aside for later use.

[0033] Ingredients and mixing steps: Put all the prepared mixed Chinese herbal extract and monk fruit concentrate into a constant temperature jacketed kettle, then add honey powder and rock sugar powder according to the formula, turn on the constant temperature stirring device, control the temperature inside the kettle to 45℃, the stirring speed to 40r / min, and continue stirring for 25min to make the materials completely and evenly mixed to obtain a soft material.

[0034] Granulation and drying steps: The prepared soft material is fed into a gyratory pellet mill and granulated using a 16-mesh standard sieve to obtain uniform wet granules; the wet granules are immediately fed into a fluidized bed dryer, the inlet air temperature is controlled at 55℃, and drying is continued until the moisture content of the granules is 3.2% by mass, at which point drying is stopped; the dried granules are then sized using a 14-mesh standard sieve to remove coarse and fine powder, resulting in uniformly sized dried granules, which are then sealed for later use.

[0035] Total mixing and tableting steps: Weigh menthol and completely dissolve it in 5 times its weight of food-grade ethanol to prepare a menthol ethanol solution; send the sized and dried granules into a mixer, first spray the menthol ethanol solution evenly into the granules, premix for 5 minutes, then add the formulated amount of food-grade magnesium stearate, and continue mixing for 13 minutes, for a total mixing time of 18 minutes, to ensure the material is completely uniform; send the mixed granules into a high-speed rotary tableting machine, adjust the tableting parameters, control the weight of the throat lozenges to 1.0 g / tablet, the tablet hardness to 4 kg, and the disintegration time to 20 minutes, and check the tablet weight difference every 15 minutes during the tableting process, finally obtaining the throat lozenges.

[0036] Packaging and storage steps: The prepared throat lozenges are sent to a clean packaging workshop and sealed using an aluminum-plastic blister packaging machine. The packaging specification is 12 tablets per blister pack. After packaging, the outer box is sealed. The finished product is stored in a cool, dry, and ventilated warehouse with a temperature ≤25℃ and a relative humidity ≤60%.

[0037] This embodiment strictly follows the core formula and preparation process of the present invention, and successfully prepares the finished product of Huajuhong functional throat lozenges. The sensory indicators of the finished product are: light brownish-yellow color, uniform color, with the inherent herbal aroma of Huajuhong and tangerine peel, pure minty coolness, moderate sweetness, slightly herbal aftertaste, no bitterness, delicate taste, and good chewing properties. The physicochemical indicators of the finished product are: moisture content 3.2% by mass, disintegration time 20 min. According to high performance liquid chromatography, the content of naringin in the finished product is 32.6 mg / tablet, glycyrrhizic acid content is 5.8 mg / tablet, and mogroside content is 0.92 mg / tablet.

[0038] Example 2 This embodiment is a sugar-free derivative embodiment of the present invention. Its core purpose is to address the needs of people controlling their blood sugar and consumers of sugar-free foods. While retaining the compatibility of the core functional ingredients and the core preparation process, the sweetening matrix is ​​replaced with sugar-free isomaltitol. This verifies the material compatibility, process stability, and finished product quality of the sugar-free formula, thereby expanding the product's applicable population and consumption scenarios.

[0039] The sugar-free, high-naringin-content Huajuhong functional throat lozenges prepared in this embodiment are based on a total weight of 1000g of finished throat lozenges. The precise ingredient formulas are as follows: 300g of Huajuhong extract, 150g of tangerine peel extract, 80g of monk fruit concentrate, 150g of Ophiopogon japonicus extract, 100g of licorice extract, 5g of menthol, 210g of isomaltitol, and 5g of food-grade magnesium stearate. The total weight of all ingredients is 1000g, and the total percentage by weight is 100%.

[0040] The preparation process in this embodiment is completely identical to that in Example 1, except that the sweet base in the ingredient and mixing steps is replaced with isomaltitol. The specific steps are as follows: Raw material pretreatment steps: The raw material pretreatment steps are completely consistent with those in Example 1, and 30-mesh raw material powders of Citrus reticulata peel, Citrus reticulata peel, Glycyrrhiza uralensis and Ophiopogon japonicus are obtained, as well as raw material of Siraitia grosvenorii pulp.

[0041] The extraction steps for the active ingredients are exactly the same as those in Example 1, resulting in a mixed extract and a monk fruit extract.

[0042] Extraction concentration and purification steps: The concentration and purification steps are completely consistent with those in Example 1, to obtain a clear mixed Chinese herbal extract and Luo Han Guo concentrated juice.

[0043] Ingredients and mixing steps: Put all the prepared mixed Chinese herbal extract and Luo Han Guo concentrated juice into a constant temperature jacketed kettle, then add isomaltulitol according to the formula, turn on the constant temperature stirring device, control the temperature inside the kettle at 45℃, the stirring speed at 40r / min, and continue stirring for 25min to make the materials completely and evenly mixed to obtain a soft material.

[0044] Granulation and drying steps: The granulation and drying steps are completely consistent with those in Example 1, and dried granules with a moisture content of 3.0% and uniform particle size are obtained.

[0045] Total mixing and tableting steps: The total mixing and tableting steps are completely consistent with those in Example 1. The weight of the throat lozenges is controlled at 1.0g / tablet, the hardness of the tablets is 4kg, and the disintegration time is 19min to obtain sugar-free throat lozenges.

[0046] Packaging and storage steps: The packaging and storage steps are exactly the same as those in Example 1. After the finished product is sealed, it is stored in a cool and dry warehouse.

[0047] This embodiment, while retaining the core efficacy, formulation, and core process of the present invention, successfully prepared a sugar-free functional throat lozenge. The sensory indicators of the finished product are: light brownish-yellow color, uniform color, inherent herbal aroma of tangerine peel and dried tangerine peel, pure minty coolness, refreshing sweetness without aftertaste, no obvious herbal bitterness, delicate taste, and good chewing properties. The physicochemical indicators of the finished product are: moisture content 3.0% by mass, disintegration time 19 min. Detection by high performance liquid chromatography shows that the content of naringin in the finished product is 31.9 mg / tablet, glycyrrhizic acid content is 5.7 mg / tablet, and mogroside content is 0.90 mg / tablet. The content of the core effective ingredients is not significantly different from that in Example 1, ensuring the stability of efficacy and effectively expanding the applicable population of the product, covering special consumer groups such as diabetic patients and people controlling blood sugar and losing weight.

[0048] Example 3 This embodiment is a process optimization embodiment of the present invention. The core purpose is to verify the enrichment effect of ultrasound-assisted alcohol extraction on alcohol-soluble active ingredients such as naringin, optimize key process parameters such as extraction, purification, and drying, compare the effects of different extraction processes on the content of active ingredients and taste quality of the product, further improve the core quality of the product, and at the same time verify the parameter flexibility and industrial adaptability of the preparation process of the present invention.

[0049] The functional throat lozenges with high naringin content prepared in this embodiment are based on a total weight of 1000g of finished throat lozenges. The precise formula of each raw material is as follows: 300g of Citrus reticulata extract, 150g of Citrus reticulata peel extract, 80g of Luo Han Guo concentrated juice, 150g of Ophiopogon japonicus extract, 100g of Glycyrrhiza uralensis extract, 5g of Menthol, 104g of honey powder, 104g of rock sugar powder, 6g of food-grade magnesium stearate, and 1g of food-grade microcrystalline cellulose. The total weight of all raw materials is 1000g, and the total weight percentage is 100%.

[0050] In this embodiment, the preparation process involves parameter optimization for the extraction, purification, and drying stages. The quality control standards for the remaining stages are consistent with those in Example 1. The specific steps are as follows: Raw material pretreatment steps: Take the raw materials of Citrus reticulata peel, dried tangerine peel, licorice, and Ophiopogon japonicus, clean, wash, and dry them, then crush them with a pulverizer and pass them through a 20-mesh standard sieve to obtain raw material powder, which is then sealed for later use; the raw material of Luo Han Guo is directly from commercially available Luo Han Guo concentrated juice, which does not require additional pretreatment or extraction.

[0051] Extraction steps of active ingredients: Put all the raw material powders of Citrus reticulata peel, Citrus reticulata peel, Glycyrrhiza uralensis and Ophiopogon japonicus obtained from the pretreatment into an ultrasonic-assisted extraction tank. Use ultrasonic-assisted extraction technology with 40% ethanol-water solution as the extraction solvent to balance the extraction efficiency of water-soluble and alcohol-soluble active ingredients. Control the material-liquid ratio at 1:12, the extraction temperature at 75℃, the ultrasonic power at 300W, and extract 3 times, with each extraction lasting 1 hour. Combine the three extracts to obtain a mixed extract.

[0052] Concentration and purification steps of the extract: The mixed extract is pumped into a vacuum low-temperature concentration tank, and the concentration temperature is controlled at 60℃ and the vacuum degree inside the tank is -0.09MPa. The concentration is carried out under reduced pressure, and the ethanol solvent is recovered at the same time. The concentration is stopped when the relative density of the mixed Chinese herbal extract is 1.15 at 25℃. The mixed Chinese herbal extract is then filtered and purified using a 0.45μm microfiltration membrane to remove macromolecular impurities, tannins and other substances that easily produce bitter taste, so as to obtain a mixed Chinese herbal extract with higher clarity. The extract is then sealed for later use.

[0053] Ingredients and mixing steps: Put the prepared mixed Chinese herbal extract and standardized monk fruit concentrate into a constant temperature jacketed kettle, then add honey powder, rock sugar powder and food-grade microcrystalline cellulose according to the formula. Turn on the constant temperature stirring device, control the temperature inside the kettle at 50℃, and the stirring speed at 60r / min. Continue stirring for 20 minutes to make the materials completely and evenly mixed to obtain a soft material.

[0054] Granulation and drying steps: The prepared soft material is fed into a pellet mill and granulated using an 18-mesh standard sieve to obtain uniform wet granules; the wet granules are then fed into a vacuum drying oven, where the drying temperature is controlled at 60℃ and the vacuum degree at -0.08MPa for low-temperature vacuum drying until the moisture content of the granules is 2.8%, at which point drying is stopped; the dried granules are then sized using a 16-mesh standard sieve to obtain uniformly sized dried granules, which are then sealed for later use.

[0055] Mixing and tableting steps: Weigh the menthol according to the formula, dissolve it completely in food-grade ethanol, and spray it evenly into the dried granules. Then add the food-grade magnesium stearate according to the formula and mix it in a three-dimensional motion mixer for 15 minutes to ensure uniformity of materials. Feed the mixed granules into a high-speed tableting machine, adjust the tableting parameters, and control the weight of the throat lozenges to 2.0g / tablet, the tablet hardness to 5kg, and the disintegration time to 25min. Monitor the tablet weight difference throughout the tableting process to finally obtain the throat lozenges.

[0056] Packaging and storage steps: The prepared throat lozenges are individually sealed in food-grade aluminum foil bags. After packaging, the finished product is stored in a cool, dry, and ventilated place.

[0057] This embodiment successfully prepared high-quality functional throat lozenges containing tangerine peel by optimizing the extraction, purification, and drying processes. The sensory indicators of the finished product are: brownish-yellow color, uniform color, pure and rich herbal aroma, mild and lasting minty coolness, full sweetness, no bitterness or off-flavors, delicate and smooth texture, and good chewability. The physicochemical indicators of the finished product are: moisture content 2.8% and disintegration time 25 min. High-performance liquid chromatography (HPLC) analysis showed that the finished product contained 65.2 mg / tablet of naringin, 11.5 mg / tablet of glycyrrhizic acid, and 1.83 mg / tablet of mogroside, demonstrating superior enrichment of the core active ingredients. This embodiment verifies that ultrasound-assisted alcohol extraction can further improve the retention rate of core active ingredients such as naringin, and membrane filtration purification can further optimize the product's taste. Furthermore, the preparation process of this invention has good parameter adjustability and can be adapted to different production equipment and quality requirements according to industrialization needs.

[0058] Comparative Example 1 This comparative example is a control sample of commercially available regular menthol throat lozenges. The core purpose is to serve as a blank efficacy control group to eliminate the interference of cooling sensation on subjective evaluation, verify the core advantages of the product of this invention compared with commercially available ordinary throat lozenges without Chinese herbal efficacy ingredients in terms of long-term improvement of throat discomfort symptoms, expectoration and cough relief, and clarify the efficacy value of the product of this invention.

[0059] This comparative study uses commercially available common mint throat lozenges. The core formula of the product is: 45% white sugar, 40% glucose syrup, purified water, 0.6% menthol, citric acid, edible flavoring, and food additives (caramel color and gelatin). The weight of a single finished product is 1.0g / piece.

[0060] The basic information and testing indicators of the product in this comparative example are as follows: The finished product is light brown in color, has a strong minty coolness, is sweet, and has no herbal aroma; The physicochemical indicators of the finished product are: moisture content 2.5% by mass, disintegration time 15 min; The product was tested and found to contain no medicinal and edible active ingredients such as naringin, glycyrrhizic acid, or mogroside.

[0061] This comparative example of commercially available ordinary menthol throat lozenges only provides a temporary cooling sensation in the mouth and throat through menthol, without any long-lasting effects of soothing the throat, relieving phlegm, or stopping coughs. It fails to address the root causes of dry, itchy throat, excessive phlegm, and a feeling of something stuck in the throat. Furthermore, the product has a high sugar content and a strong sweet taste; long-term use may lead to a sticky mouth and dry throat. This comparative example will serve as a blank control group for subsequent efficacy verification experiments.

[0062] Comparative Example 2 This comparative example is a single-component tangerine peel throat lozenge without scientific formulation. The core purpose is to verify the necessity of the principal-assistant-adjuvant formulation system of this invention and the optimized extraction process, and to compare the differences in the content of active ingredients, taste quality, food safety, and symptom improvement effect with products that do not adopt optimized extraction and purification processes.

[0063] The Huajuhong throat lozenges prepared in this comparative example, based on a total finished product weight of 1000g, have the following formula: 200g Huajuhong raw material powder, 795g rock sugar powder, and 5g menthol. No other ingredients such as dried tangerine peel, Ophiopogon japonicus, licorice, or monk fruit were added. The formulation did not follow the theory of monarch, minister, assistant, and guide in the formulation of ingredients. Furthermore, no extraction, concentration, or purification processes were used. The preparation process was simply made by directly mixing and compressing the raw materials.

[0064] The specific steps of the preparation process for this comparative example are as follows: Raw material pretreatment: After crushing the raw material of Huajuhong (a type of tangerine peel), pass it through an 80-mesh sieve to obtain Huajuhong raw material powder. Crush the rock sugar powder and pass it through an 80-mesh sieve. Seal and store for later use.

[0065] Mixing steps: Put the raw material powder of tangerine peel and the powdered rock sugar into the mixer and mix for 20 minutes. Then add the menthol pre-dissolved in ethanol and continue mixing for 10 minutes to obtain the mixed powder.

[0066] Tableting steps: The mixed powder is directly fed into the tableting machine, and the weight of the tablet is controlled to be 1.0g / tablet and the hardness is 4kg to obtain throat lozenges.

[0067] Packaging steps: Use aluminum-plastic blister packaging and store in a sealed container.

[0068] The Huajuhong throat lozenges prepared in this comparative example, because they did not employ an extraction and concentration process and were only made by directly adding raw material powder, had a naringin content of only 10.5 mg / tablet in the finished product, far lower than that of the product in the embodiment of this invention. The content of the core active ingredient was extremely low, failing to guarantee the core efficacy of expectoration and cough relief. Furthermore, due to the lack of complementary ingredients, the warming and drying properties of Huajuhong could not be controlled, and long-term consumption could easily lead to aggravated dry mouth and throat problems. In addition, the unpurified Huajuhong raw material powder had a strong bitter taste reminiscent of traditional Chinese medicine, resulting in a very poor product taste and low consumer acceptance. This comparative example will serve as a negative control group for subsequent efficacy verification experiments.

[0069] Effect verification test This verification experiment includes: detection of the content of core active ingredients to verify the enrichment effect of the process of this invention on active ingredients such as naringin; double-blind evaluation of taste and eating experience to verify the improvement effect of this invention on the bitterness of traditional Chinese medicine and its advantages in eating experience; and verification of the efficacy and safety of the food, verifying the improvement effect of the formulation system of this invention on symptoms of throat discomfort and its safety. The products of Examples 1, 2, and 3 of this invention were used as the experimental group, and the products of Comparative Examples 1 and 2 were used as the control group. Through standardized detection methods and evaluation systems, the application value of the technical solution of this invention compared with existing products was comprehensively verified.

[0070] Experimental Materials and Methods Test samples: The test group samples were the finished throat lozenges prepared in Examples 1, 2 and 3; the control group samples were the commercially available ordinary mint throat lozenges in Comparative Example 1 and the single-component orange-red throat lozenges prepared in Comparative Example 2.

[0071] Core efficacy ingredient content testing Detection method: High performance liquid chromatography (HPLC) was used to quantitatively detect the contents of naringin, glycyrrhizic acid and mogroside in each sample. Each sample was tested in parallel three times and the average value was taken.

[0072] Test subjects: 1.0g / tablet samples of Example 1 and Example 2, 2.0g / tablet samples of Example 3, and 1.0g / tablet samples of Comparative Example 2.

[0073] The content of the core active ingredient in the throat lozenges prepared in Examples 1 to 3, and the throat lozenge in Comparative Example 2, was determined by high performance liquid chromatography (HPLC). The results are shown in Table 1 below.

[0074] Table 1 Double-blind evaluation of taste and eating experience Evaluation subjects: 20 healthy volunteers aged 20-50 years old with no history of oral or throat diseases and no taste disorders will be recruited.

[0075] Evaluation Method: A double-blind test was conducted. All samples were removed from their packaging and randomly numbered. Volunteers took each sample in turn and rated it on four dimensions: cooling sensation, bitterness, sweetness, and duration of throat soothing. Each dimension was scored out of 10. A lower score for bitterness indicated a milder bitterness, while higher scores for the other dimensions indicated a better experience. After all samples were evaluated, the rating sheets were collected, and the average scores for each indicator were statistically analyzed. The results are shown in Table 2 below.

[0076] Table 2 Verification of edible efficacy and safety Subjects: Thirty subjects aged 22-45 years with symptoms of dry and itchy throat, excessive phlegm and cough, and foreign body sensation in the throat due to overuse of their voice were recruited. The symptoms lasted for ≥3 days. Subjects with serious throat diseases or allergies to the test materials were excluded. They were randomly divided into 3 groups of 10 people each. The samples were selected from those prepared in Example 1, Comparative Example 1, and Comparative Example 2, respectively.

[0077] Experimental method: Subjects in each group took one tablet of the corresponding sample three times a day for seven consecutive days. During the experiment, they were prohibited from taking other drugs or foods that improve throat discomfort. Changes in symptoms and occurrence of adverse reactions were recorded daily.

[0078] Evaluation criteria: The symptom improvement effectiveness was based on the subjective evaluation of the subjects. Significant relief or disappearance of symptoms was considered effective, while no improvement or worsening of symptoms was considered ineffective. Adverse reactions were mainly recorded as worsening of dry mouth, nausea, and oral discomfort. The incidence of adverse reactions was statistically analyzed, and the results are shown in Table 3 below:

[0079] Table 3 This verification experiment comprehensively verified the effectiveness of the technical solution of this invention in addressing the pain points of existing technologies through systematic testing across three dimensions. This invention significantly improves the retention rate and enrichment effect of core active ingredients, solving the problems of low content and unclear efficacy of active ingredients in existing products. Test results show that the products of Examples 1 and 2 of this invention have a single-grain naringin content more than three times that of the product of Comparative Example 2. The product of Example 3, after process optimization, further increases the unit content of naringin, while glycyrrhizic acid, mogroside, and other synergistic active ingredients can be stably detected. This result stems from the optimized extraction process of this invention. Through adaptable extraction technology and vacuum low-temperature concentration process, the active ingredients in raw materials such as Citrus reticulata peel are maximized. Compared to the simple process of directly feeding raw materials, this achieves efficient enrichment of active ingredients, providing a stable material basis for the core efficacy of the product and completely solving the problem of low retention rate of effective ingredients in existing Citrus reticulata peel-related products. The results of the human trial showed that the product of Example 1 of this invention had an efficacy rate of 60%, 70%, and 60% higher than that of Comparative Example 1 in improving dry and itchy throat, excessive phlegm and cough, and foreign body sensation in the throat, respectively, and 30%, 30%, and 40% higher than that of Comparative Example 2. At the same time, the incidence rate of adverse reaction of aggravated dry mouth in Example 1 was 0, which was far lower than the 60% incidence rate in Comparative Example 2, and there were no other adverse reactions. This result fully verifies that the principal drug of this invention, Citrus reticulata peel, directly targets the core symptoms of excessive phlegm and throat discomfort, while the assistant drugs synergistically enhance the efficacy. The adjuvant drugs, Ophiopogon japonicus and Glycyrrhiza uralensis, effectively restrain the warm and dry nature of Citrus reticulata peel and Citrus tangerine peel, avoiding depletion of body fluids. This achieves a combination of attacking and tonifying, with a mild nature and taste, ensuring both the core efficacy of clearing the throat, moistening the throat, resolving phlegm and relieving cough, and ensuring the safety of long-term consumption.

[0080] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A functional throat lozenge based on high naringin content citrus peel, characterized in that, This throat lozenge is composed of active ingredients and food-grade excipients, with the following mass percentages for each ingredient: Active ingredients: Citrus reticulata extract 30%, Citrus reticulata peel extract 15%, Monk fruit concentrate 8%, Ophiopogon japonicus extract 15%, Glycyrrhiza uralensis extract 10%, Menthol 0.5%; Food-grade excipients: sweet base 20%-21%, lubricant 0.5%-1%, filler and binder 0%-1%.

2. The functional throat lozenge based on high naringin content of Citrus reticulata peel according to claim 1, characterized in that, The sweet base is a combination of honey powder and rock sugar powder, or isomalt; when the sweet base is a combination of honey powder and rock sugar powder, the mass percentage of honey powder is 10%-10.5% and the mass percentage of rock sugar powder is 10%-10.5%.

3. The functional throat lozenge based on high naringin content of Citrus reticulata peel according to claim 1, characterized in that, The lubricant is food-grade magnesium stearate, and the filler binder is food-grade microcrystalline cellulose.

4. The functional throat lozenge based on high naringin content of Citrus reticulata peel according to claim 1, characterized in that, The mass content of naringin in the Citrus reticulata extract is ≥10%; The glycyrrhizic acid content in the licorice extract is ≥5% by mass. The mogroside content in the concentrated mogroside juice is ≥1%.

5. The functional throat lozenge based on high naringin content of Citrus reticulata peel according to claim 1, characterized in that, The moisture content of the finished throat lozenge is ≤5.0%, and the disintegration time is 10-30 minutes.

6. The functional throat lozenge based on high naringin content of Citrus reticulata peel according to claim 4, characterized in that, The preparation steps of the Citrus reticulata extract are as follows: The cleaned raw material of Citrus reticulata is washed, dried and crushed to obtain Citrus reticulata coarse powder of 20-40 mesh; The obtained crude tangerine peel powder was put into an extraction tank, and 8-12 times the amount of solvent was added. Dynamic countercurrent extraction was carried out at 70-95℃ for 2-3 times, each time for 1-2 hours. The extracts were then combined. The obtained extract was filtered, and the filtrate was concentrated under vacuum at 60-65℃ to a thick paste with a relative density of 1.10-1.15, thus obtaining the Citrus reticulata extract. The solvent is purified water or an ethanol-water solution with a volume fraction of 30%-50%.

7. A preparation process for functional throat lozenges based on high naringin content citrus peel, applicable to the functional throat lozenges based on high naringin content citrus peel as described in any one of claims 1-6, characterized in that, The preparation process involves the following steps: S100. Raw material pretreatment: The raw materials of Citrus reticulata peel, dried tangerine peel, licorice, and Ophiopogon japonicus are cleaned, washed, dried, and pulverized to obtain raw material powder of 20-40 mesh; the raw material of Luo Han Guo is processed by breaking the shell and removing the pulp to obtain Luo Han Guo raw material. S200, Extraction of effective components: Combine the raw material powders of Citrus reticulata peel, Citrus reticulata peel, Glycyrrhiza uralensis and Ophiopogon japonicus obtained from S100, and use extraction technology to extract the effective components to obtain a mixed extract. Separately extract the raw material of Siraitia grosvenorii to obtain Siraitia grosvenorii extract. S300. Concentration and purification of extract: Vacuum low-temperature concentration and purification of the obtained mixed extract to obtain mixed Chinese herbal extract; concentration of the obtained monk fruit extract to obtain monk fruit concentrate. S400, Ingredients and Mixing: Add the obtained mixed Chinese herbal extract, Luo Han Guo concentrated juice, sweet matrix and filler binder into a jacketed kettle, mix evenly to obtain a soft material; S500, Granulation and Drying: The obtained soft material is granulated and dried at low temperature to obtain dried granules. Menthol and lubricant are added to the dried granules, and after being fully mixed, they are compressed into tablets to obtain throat lozenges. S600 Packaging and Storage Procedures: Seal the throat lozenges and store them in a cool, dry place.

8. The preparation process of functional throat lozenges based on high naringin content tangerine peel as described in claim 7, characterized in that, In S200, the extraction technology is any one of dynamic countercurrent extraction, ultrasonic-assisted extraction, or thermal reflux extraction; The solvent used for extraction is purified water or an ethanol-water solution with a volume fraction of 30%-50%; The extraction process parameters are as follows: material-liquid ratio 1:8~1:12, water extraction temperature 85-95℃, alcohol extraction temperature 70-80℃, extraction times 2-3 times, extraction time 1-2 hours per extraction.

9. The preparation process of functional throat lozenges based on high naringin content tangerine peel as described in claim 7, characterized in that, In S300, the vacuum low-temperature concentration process is carried out at a temperature of 60-65℃, and the relative density of the mixed Chinese herbal extract obtained after concentration is 1.10-1.

15. The relative density is detected at 25℃. The purification process uses centrifugation or membrane filtration technology to remove macromolecular impurities from the extract.

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