Lozenges for treating dry, itchy, sore throat and preparation method thereof

Abstract

The application relates to the technical field of traditional Chinese medicines, in particular to a lozenge for treating throat dryness, itching and pain and a preparation method thereof. The lozenge for treating throat dryness, itching and pain and the phyllanthus emblica dry extract powder prepared by the preparation method have a significantly improved content of gallic acid, the restriction on the production place of fresh phyllanthus emblica is broken, the production scale and the application range are expanded, the process flow is simple, the operation is convenient, and the lozenge has high practicability and economic value.

Description

Technical Field

[0001] This application relates to the field of traditional Chinese medicine technology, specifically to a lozenge for treating dry, itchy, and painful throat and its preparation method. Background Technology

[0002] Dry, itchy, and sore throat are common symptoms that can be caused by a variety of factors, including but not limited to chronic pharyngitis, inflammation of the pharyngeal lymphoid follicles, tonsillitis, and allergies. These symptoms can affect daily life, causing hoarseness, difficulty swallowing, and may even lead to nausea and coughing.

[0003] Compound Phyllanthus emblica throat lozenges are a traditional Chinese medicine, approved by the State Food and Drug Administration under license number B20020422, and conforming to the national drug standard WS-5401(B-0401)-2014Z. Through its effects of clearing heat and detoxifying, reducing swelling and relieving pain, Compound Phyllanthus emblica throat lozenges can effectively alleviate throat discomfort such as dryness, itching, and pain, including symptoms like sore throat, dry and itchy throat, burning sensation in the throat, foreign body sensation, and dry cough with little phlegm. Because it acts directly on the throat, it can exert its effects for a long time, thus having a significant advantage in the adjunctive treatment of throat diseases.

[0004] Phyllanthus emblica extract powder is an important raw material in compound Phyllanthus emblica throat lozenges. It is obtained by juicing, concentrating, and drying fresh Phyllanthus emblica fruit. According to the national drug standard WS-5401(B-0401)-2014Z of the State Food and Drug Administration, the active ingredient gallic acid in Phyllanthus emblica extract powder must not be less than 1.5% to ensure the efficacy of the drug. Fresh Phyllanthus emblica contains a large amount of tannins, which are a class of natural polyphenolic compounds that can form insoluble complexes with proteins. Gallic acid is a simple form of tannic acid, belonging to the hydroxybenzoic acid class of compounds, and is a building block in the complex molecular structure of many tannins. During the process of preparing Phyllanthus emblica extract powder from fresh fruit, some of the tannins are also converted into gallic acid, ultimately obtaining Phyllanthus emblica extract powder with the required gallic acid content.

[0005] However, fresh amla fruit is prone to rotting during long-distance transportation. As the rotting progresses, the tannins (a type of plant polyphenol) in amla are gradually oxidized and decomposed, resulting in a decrease in the gallic acid content in the dried amla extract powder, which no longer meets the relevant content regulations. This, in turn, affects the efficacy of the lozenges in treating dry, itchy, and sore throats.

[0006] Therefore, there is an urgent need to develop a lozenge that can effectively treat dry, itchy, and painful throat. Summary of the Invention

[0007] Based on this, one or more embodiments of this application provide a lozenge for treating dry, itchy, and sore throat and a method for preparing the same. The lozenge has few restrictions on raw materials, is simple to prepare, and can effectively relieve throat discomfort symptoms such as dryness, itching, and sore throat.

[0008] The technical solution of this application includes the following:

[0009] A method for preparing Phyllanthus emblica extract powder includes the following steps:

[0010] S100: Mix pitted fresh amla with water, juice, filter, and obtain fresh amla juice and amla residue;

[0011] S200: Mix the amla residue with water, stir, and filter to obtain amla residue liquid;

[0012] S300: Combine the fresh amla juice and the amla residue liquid, concentrate the combined mixture to 8Be~10Be to obtain the first amla concentrate, heat the first amla concentrate at 100℃~105℃ for 2h~4h to obtain the second amla concentrate, concentrate the second amla concentrate to 18Be~22Be to obtain the third amla concentrate;

[0013] S400: Spray dry the third concentrated amla extract to obtain amla powder.

[0014] A dried amla extract powder prepared by the method described above.

[0015] A lozenge for treating dry, itchy, and sore throat contains, by weight percentage:

[0016] Compound dry powder 15%~20%;

[0017] The above-mentioned amla extract powder contains 2%~4%;

[0018] Gelatin sugar powder 50%~55%;

[0019] Dextrin 20%~25%;

[0020] Menthol 0.5%~0.7%;

[0021] Borneol 0.1%~0.3%; and

[0022] 1%~3% silicon dioxide;

[0023] The compound dry powder is an aqueous extract of a mixture of the traditional Chinese medicines Scrophularia ningpoensis, Platycodon grandiflorus, and Glycyrrhiza uralensis.

[0024] Optionally, the gelatin sugar powder contains gelatin and sugar powder in a weight ratio of (3.5~4):100;

[0025] Alternatively, the sugar powder may be sucrose powder.

[0026] A method for preparing a lozenge for treating dry, itchy, and sore throat, as described above, includes the following steps:

[0027] Weigh out each ingredient according to the formula for lozenges used to treat dry, itchy, and sore throats described above;

[0028] The compound dry powder, the amla dry extract powder, the gelatin sugar powder, the dextrin and the first alcohol solvent are mixed to obtain a soft material, and the soft material is granulated to obtain the first wet granules.

[0029] The first wet particles were dried using a fluidized bed dryer to obtain the first dry particles.

[0030] The menthol and borneol were dissolved in a second alcohol solvent to prepare a borneol-menthol solution.

[0031] The borneol and menthol liquid is sprayed onto the first dry granules, then the silica is added and mixed, and the mixture is compressed into tablets.

[0032] The preparation method of the amla fruit extract powder of this application involves preparing amla fruit extract powder from fresh amla fruit through a suitable process. Using the preparation method of this application, it is not necessary to consider the freshness of the raw material amla fruit, and regardless of whether the tannins are lost due to long-distance transportation, amla fruit extract powder with qualified gallic acid content can be obtained in the end. This breaks the restriction on the origin of fresh amla fruit, reduces the restriction on the source of raw materials, and lowers the raw material procurement cost.

[0033] Traditional methods for preparing Phyllanthus emblica extract powder, even when using fresh Phyllanthus emblica with qualified tannins as raw materials, can only yield Phyllanthus emblica extract powder with a gallic acid content of 1.3% to 1.4%, which still does not meet the legal standards. The preparation method of this application significantly improves the content of gallic acid in the Phyllanthus emblica extract powder to 7.9% to 8.2%.

[0034] Furthermore, the traditional method for preparing Phyllanthus emblica extract powder was used to prepare Phyllanthus emblica extract powder, which was then used to prepare lozenges. The gallic acid content in these lozenges was 0.09~0.45 mg / tablet, which did not meet the legal standard. However, the method for preparing Phyllanthus emblica extract powder of this application was used to prepare Phyllanthus emblica extract powder, which was then used to prepare lozenges. The gallic acid content in these lozenges was significantly increased to 2.59~2.76 mg / tablet.

[0035] The preparation method provided in this application is suitable for preparing lozenges for treating dry, itchy, and painful throats. The preparation process is simple, easy to operate, and easy to control product quality. It is a safe and reliable preparation method suitable for industrial production.

[0036] The gallic acid content in the Phyllanthus emblica extract powder and lozenges for treating dry, itchy, and painful throats in this application is significantly increased, which has a positive promoting effect on fully exerting the efficacy of the lozenges and is conducive to the further clinical promotion and application of this type of drug. Attached Figure Description

[0037] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0038] Figure 1 The graph shows the effect of concentration temperature, concentration time, and spray drying temperature on the preparation of Phyllanthus emblica dry extract powder according to an embodiment of this application. Detailed Implementation

[0039] The present application is further described below with reference to embodiments and examples. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the application. Furthermore, it should be understood that after reading the teachings of this application, those skilled in the art can make various alterations or modifications to this application, and these equivalent forms also fall within the protection scope of the appended claims.

[0040] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.

[0041] the term

[0042] Unless otherwise stated or in case of contradiction, the terms or phrases used herein shall have the following meanings:

[0043] The term “and / or” as used herein includes any one of two or more of the related listed items, as well as any and all combinations of the related listed items, wherein any and all combinations include any two related listed items, any more related listed items, or a combination of all related listed items.

[0044] In this application, "further" is used to describe the purpose and indicate differences in content, but should not be construed as a limitation on the scope of protection of this application.

[0045] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.

[0046] In this application, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, optional numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.

[0047] In this application, weight can be a well-known unit of mass in the chemical industry, such as μg, mg, g, or kg.

[0048] In this application, the F-value is the critical value in the F-distribution table, commonly used in the F-test of analysis of variance (ANOVA). These values ​​represent the critical values ​​of the F-distribution for a given number of degrees of freedom (df) at different significance levels (α level). For example, F... 0.1 (2,2)=9.0 means that at a significance level of 0.1, when both groups have 2 degrees of freedom, the critical value of the F-distribution is 9.0. 0.05 (2,2)=19.0 means that the critical value is 19.0 at a significance level of 0.05. F 0.01 (2,2)=99.0 means that the critical value is 99.0 at a significance level of 0.01.

[0049] One aspect of this application provides a method for preparing Phyllanthus emblica extract powder, comprising the following steps:

[0050] S100: Mix pitted fresh amla with water, juice, filter, and obtain fresh amla juice and amla residue;

[0051] S200: Mix the amla residue with water, stir, filter, and obtain amla residue liquid;

[0052] S300: Combine fresh amla juice and amla residue liquid, concentrate the combined mixture to 8Be~10Be to obtain the first amla concentrate, heat the first amla concentrate at 100℃~105℃ for 2h~4h to obtain the second amla concentrate, concentrate the second amla concentrate to 18Be~22Be to obtain the third amla concentrate;

[0053] S400: Spray-dry the third concentrated solution of Phyllanthus emblica to obtain Phyllanthus emblica dry extract powder.

[0054] In this article, the concentration unit for each concentrate is Baumé (Be), a unit used to measure liquid concentration, particularly when measuring the relative concentration of solid particles in a liquid. It is a dimensionless ratio defined as the ratio of the mass of the liquid to the mass of an equal volume of water. It is important to note that Baumé is not an absolute unit of measurement, but rather a relative concentration indicator. It depends on the density and composition of the solution. Since the density of a liquid changes with temperature, Baumé measurements are typically performed at a specific temperature.

[0055] In this paper, the Baumé degree of each concentrate was measured at 70℃~80℃.

[0056] In one embodiment, in S100, the weight ratio of pitted fresh amla to water is (1.8~2.2):1;

[0057] In S200, the weight ratio of Phyllanthus emblica residue to water is (0.8~1.2):1.

[0058] In one embodiment, S300 includes at least one of the following technical features:

[0059] (1) Under negative pressure and at 80℃~90℃, the combined liquids are concentrated to 8Be~10Be;

[0060] (2) Under normal pressure, heat the concentrated first amla extract at 100℃~105℃ for 2h~4h;

[0061] (3) Concentrate the second amla concentrate to 18Be~22Be under negative pressure and at 80℃~90℃;

[0062] Negative pressure refers to a pressure of -0.06MPa to -0.07MPa.

[0063] Normal pressure refers to atmospheric pressure, which is usually 0.1 MPa.

[0064] In one embodiment, the inlet air temperature of the spray dryer is 170°C to 180°C, and the outlet air temperature is 70°C to 90°C.

[0065] In another aspect of this application, a dried amla extract powder is prepared by any of the above-mentioned technical solutions.

[0066] In another aspect, this application provides a lozenge for treating dry, itchy, and sore throat, comprising, by weight percentage:

[0067] Compound dry powder 15%~20%;

[0068] The above-mentioned dried amla extract powder contains 2%~4%;

[0069] Gelatin sugar powder 50%~55%;

[0070] Dextrin 20%~25%;

[0071] Menthol 0.5%~0.7%;

[0072] Borneol 0.1%~0.3%; and

[0073] 1%~3% silicon dioxide;

[0074] Among them, the compound dry powder is an aqueous extract of a mixture of Scrophularia, Platycodon, and Glycyrrhiza;

[0075] Gelatin sugar powder contains gelatin and sugar powder in a weight ratio of (3.5~4):100;

[0076] Optionally, the powdered sugar is sucrose powder.

[0077] In one embodiment, the gelatin sugar powder is prepared by a method comprising the following steps:

[0078] Gelatin and water are mixed in a weight ratio of 1:(1.2~1.4), and heated to obtain an aqueous solution of gelatin;

[0079] A sucrose aqueous solution is prepared by mixing sucrose and water in a weight ratio of 1:(0.4~0.6) and heating.

[0080] A gelatin aqueous solution and a sucrose aqueous solution are mixed to obtain gelatin syrup;

[0081] Heat the gelatin syrup to 90℃~100℃, then add sucrose powder and mix. After mixing, dry at 55℃~65℃ and pulverize.

[0082] The weight ratio of sucrose powder to gelatin syrup is 100:(17~18).

[0083] In another aspect, this application provides a method for preparing a lozenge for treating dry, itchy, and sore throat according to any of the above-mentioned technical solutions, comprising the following steps:

[0084] Weigh out each ingredient according to the formula for the lozenges mentioned above;

[0085] The compound dry powder, amla dry extract powder, gelatin sugar powder, dextrin and the first alcohol solvent are mixed to obtain a soft material, and the soft material is granulated to obtain the first wet granules.

[0086] The first wet particles are dried to obtain the first dry particles;

[0087] A mixture of menthol and borneol was dissolved in a second alcohol solvent to prepare a borneol-menthol solution.

[0088] Spray the menthol and camphor liquid onto the first dry granules, then add silica and mix, then compress into tablets.

[0089] In one embodiment, the first wet particles are dried at 60°C to 65°C to obtain the first dry particles;

[0090] The moisture content of the first dry granules is ≤3%;

[0091] Optionally, the drying time is 10 min to 30 min.

[0092] Alternatively, drying equipment such as fluidized bed dryers, hot air drying ovens, and vacuum drying ovens can be used to dry the product until a certain degree of dryness is achieved (e.g., moisture content ≤ 3%).

[0093] In one embodiment, the first alcohol solvent is an aqueous solution of ethanol with a volume percentage of 75% to 90%;

[0094] The second alcohol solvent is an aqueous solution of ethanol with a volume percentage of 85% to 90%.

[0095] The following are some specific examples.

[0096] The raw materials and reagents involved in the following specific embodiments can be obtained commercially or prepared by those skilled in the art using known methods.

[0097] For experimental parameters not specified in the following specific embodiments, please refer to the guidelines given in this application document first, or refer to experimental manuals or other experimental methods known in the art, or refer to the experimental conditions recommended by the manufacturer.

[0098] Some of the equipment and testing instruments used in the following embodiments:

[0099] 3100C electronic balance, BS223S electronic balance, manual mini pitter, CH-18 pitter, PR-1.5 juicer, 5m 3 Multifunctional extraction tank, SJN-1000 triple-effect energy-saving concentrator, QPG-25 spray dryer unit, SP1500 laboratory spray dryer, WF-30B universal high-speed pulverizer, HZD800B automatic lifting hopper mixer, FL-200 fluidized bed dryer granulator, YK-160A swing granulator, GZPL40C high-speed rotary tablet press, Waters 2695-2998 high-performance liquid chromatograph.

[0100] Example 1

[0101] This embodiment verifies the preparation method of Phyllanthus emblica extract powder through orthogonal experiments and small-scale tests. The specific steps are as follows:

[0102] (1) Preliminary screening of the optimal concentration and spray drying conditions for Phyllanthus emblica extract powder

[0103] via L9(3) 4 Orthogonal experiments were conducted, with gallic acid content in the dry extract powder as the evaluation index. The optimal combination of factors such as concentration temperature, concentration time, and spray drying temperature was determined, and the preparation process of Phyllanthus emblica dry extract powder was optimized. The levels of each factor are shown in Table 1.

[0104] Table 1. Levels of Preparation Conditions

[0105]

[0106] 1) Results of orthogonal experiments

[0107] Table 2 Orthogonal Intuitive Analysis Table

[0108]

[0109] Table 3 Analysis of Variance

[0110]

[0111] In Table 3, F 0.1 (2,2)=9.0, F 0.05 (2,2)=19.0,F 0.01 (2,2)=99.0.

[0112] 2) Analysis of orthogonal experimental results

[0113] Using the gallic acid content in the dry powder as the evaluation index, an orthogonal experiment was conducted to explore the effects of concentration temperature, concentration time, and spray drying temperature on the gallic acid content in the dry powder. The range of the intuitive analysis table (see Table 2) shows that the order of importance of each factor is A (concentration temperature) > B (concentration time) > C (spray drying temperature). The results of the analysis of variance (see Table 3) show that factor A (concentration temperature) is significant, while the other two factors, B (concentration time) and C (spray drying temperature), have no significant effect. That is, concentration temperature is a significant influencing factor, while concentration time and spray drying temperature are not significant influencing factors within the selected range and can be adjusted according to the actual situation.

[0114] Figure 1 It is a graph showing the effect of concentration temperature, concentration time, and spray drying temperature. From Figure 1It is known that the gallic acid content in the dry extract increases with increasing concentration temperature. Based on actual production conditions, the initial concentration temperature is set at 80℃~90℃. The gallic acid content in the dry extract also increases with increasing concentration time. Considering the gallic acid content standard and the results of orthogonal content determination under various conditions, the initial concentration time is set at 3 hours or more. As the spray drying temperature increases from 170℃ to 180℃, the gallic acid content in the dry extract increases slowly. When the spray drying temperature reaches 190℃, the gallic acid content increases significantly. Taking into account the need for extraction efficiency and cost savings in actual production, the initial concentration and spray drying conditions for preparing Phyllanthus emblica dry extract are as follows: Fresh Phyllanthus emblica juice is concentrated under negative pressure in a vacuum concentration tank to 18Be~22Be (75℃~80℃), then concentrated at 90℃ under normal pressure for more than 3 hours, with a spray drying temperature of 170℃~180℃.

[0115] (2) Optimization of pilot-scale process

[0116] 1) Optimization methods and results of small-scale process

[0117] Two batches of fresh Phyllanthus emblica from Xishuangbanna, Yunnan Province, were used to optimize the concentration temperature, concentration time, and spray drying temperature using orthogonal optimization. Small-scale process optimization was also conducted. The preparation conditions and results are shown in Table 4.

[0118] Table 4 Results of the small-scale experiment

[0119]

[0120] 2) Analysis of small-scale optimization results

[0121] Tannins are substances that tannify leather, also known as tannic acid or tannins. With the continuous progress of modern research, it is now believed that tannins are plant polyphenols composed of glucose (and other polyols) esters of gallic acid (or its polymers), polymers of flavanols and their derivatives, and mixtures of both. Two batches of fresh Phyllanthus emblica from Xishuangbanna, Yunnan Province, were used for orthogonal optimization of the concentration temperature, concentration time, and spray drying temperature. The results showed that increasing the concentration temperature, concentration time, and spray drying temperature all facilitated the conversion of tannins to gallic acid, increasing the gallic acid content. The gallic acid content in the dry extract powder prepared from both batches of Phyllanthus emblica was qualified (see Table 4). The key point for qualified gallic acid in the dry extract powder was identified: the concentrated liquid (i.e., non-filtrate state) was heated at approximately 90°C under normal pressure for more than 3 hours. However, considering that prolonged concentration would increase energy consumption, production costs, and reduce production efficiency, the concentration time was tentatively set at 3 hours.

[0122] Meanwhile, during production, researchers discovered that by first concentrating fresh amla juice under negative pressure to 8-10 Be to slightly enrich the tannin concentration, it can be concentrated under normal pressure without strictly requiring initial negative pressure concentration to 20 Be followed by normal pressure concentration. On one hand, at 8-10 Be, the tannins are already at an optimal conversion concentration. On the other hand, during further normal pressure concentration, some water evaporates, and as heating continues, the concentrate gradually approaches 20 Be. After heating, a short period of negative pressure concentration (or even no further negative pressure concentration) is required to obtain the concentrate needed for spray drying (usually 18-22 Be). This adjustment does not compromise the conversion rate and efficiency of gallic acid while saving on production equipment costs and concentration time.

[0123] The adjusted preparation method for Phyllanthus emblica dry extract powder is as follows: Fresh Phyllanthus emblica juice is added to a concentrator and concentrated to a Baume degree of 8-10 Be. It is then concentrated at 90°C and atmospheric pressure for 3 hours, and further concentrated to 18-22 Be (70-80°C) to obtain a concentrated solution. The solution is then spray-dried at a temperature of 170°C to 180°C.

[0124] (3) Multiple batches of fresh Phyllanthus emblica from different origins were used for verification.

[0125] The method of preparing dried amla extract powder was used to screen fresh amla from different producing areas. The results are shown in Table 5.

[0126] Table 5. Results of Tannin and Gallic Acid Detection in Fresh Fruits from Different Origins and Dried Fruit Extracts

[0127]

[0128]

[0129] Multiple batches of small-scale experiments were conducted using an orthogonal and optimized method for preparing Phyllanthus emblica extract powder. When the tannin content of fresh Phyllanthus emblica fruit was ≥3.0%, the gallic acid content in the prepared Phyllanthus emblica extract powder met the quality standard requirements for Phyllanthus emblica extract powder in the National Drug Standard WS-5401(B-0401)-2014Z issued by the State Food and Drug Administration (i.e., the gallic acid content in the Phyllanthus emblica extract powder should not be less than 1.5%). When the tannin content of fresh fruit was <3.0%, the gallic acid content in the prepared Phyllanthus emblica extract powder did not meet this legal standard. Comparison of fresh fruit production areas revealed that batches with high tannin content and acceptable gallic acid content in the Phyllanthus emblica extract powder were concentrated in Yunnan province. Purchasing fresh Phyllanthus emblica fruit from Yunnan involves long-distance transportation, which increases the risk of spoilage. From the perspective of sustainable raw material procurement, limiting sourcing to a single production area is detrimental to the future development of this variety. Selecting suitable processing techniques to produce dry extract powder with qualified gallic acid content from fresh Phyllanthus emblica fruit with low tannin content is beneficial for the future development of this variety.

[0130] (4) Pilot-scale preparation process optimization

[0131] According to the results of the orthogonal experiment, the concentration temperature is a significant influencing factor. The gallic acid content of the dry extract powder increases with the increase of the concentration temperature. The key to the preparation of the amla concentrate is to heat the concentrate at 90℃ for more than 3 hours, change the temperature to 100℃, and add a pretreatment washing process for fresh fruit. The process is as follows: fresh amla are washed, pitted by an automatic pitting machine, and the pitted amla are juiced with water at a ratio of 2:1 and filtered to obtain fresh amla juice. After juicing, the amla pomace was mixed with water at a 1:1 ratio, stirred, washed, filtered, or centrifuged to obtain amla pomace liquid. The fresh amla juice and amla pomace liquid were combined, and the filtrate was concentrated under negative pressure at 80℃-90℃ to 8-10 Be, then concentrated at 100℃ and normal pressure for 3 hours. Concentration was continued at 80℃-90℃ under negative pressure to 18-22 Be (70-80℃) to obtain amla concentrate. The concentrate was filtered through a 60-mesh filter and spray-dried. The inlet air temperature of the spray drying tower was set at 170-180℃, and the outlet air temperature was controlled at 70-90℃ to obtain amla dry extract powder. The gallic acid content was tracked during the pilot-scale production process: Amla concentrate was sampled before, after, and after concentrations at 100℃ and normal pressure for 1 hour, 2 hours, and 3 hours, as well as the clear extract, and spray-dried in the laboratory. The gallic acid content of the dry extract powder was measured and tracked; the results are shown in Table 6.

[0132] Table 6. Content determination results of dry powder prepared from samples during pilot-scale testing.

[0133]

[0134] According to Table 6, the current concentration process (i.e., concentrating the amla juice filtrate at 80℃ under negative pressure for about 7 hours) to prepare amla dry extract powder from fresh amla raw materials with low tannin content cannot yield amla dry extract powder with qualified gallic acid content. The process of this invention concentrates the amla concentrate at 100℃ under normal pressure. The results show that the gallic acid content in the dry extract powder increases with the increase of concentration time at 100℃ under normal pressure. After 1 hour of concentration at 100℃ under normal pressure, the gallic acid content is close to the qualified level (the quality standard for amla dry extract powder in the National Drug Standard WS-5401(B-0401)-2014Z of the State Food and Drug Administration stipulates that the gallic acid content in amla dry extract powder should not be less than 1.5%). After 2 hours of concentration at 100℃ under normal pressure, the gallic acid content in the dry extract powder meets the legal standard. After 3 hours of concentration at 100℃ under normal pressure, the gallic acid content in the dry extract powder approaches its maximum stable value. The fresh amla fruit in this batch contained 1.7% tannins. After process adjustments, the content of amla extract powder was reduced to 2.1%. The final process for preparing amla extract powder was as follows: Wash the amla fruits with running water and remove the pits. Juice the pitted amla fruits to obtain juice and pomace. Juice the pomace again, combine the juices, filter, and discard the pomace to obtain amla juice. Add the amla juice and water to a concentrator at a ratio of 1:2 and concentrate to a Baume degree of 8-10 Be. Concentrate at 100℃ and normal pressure for 3 hours. After normal pressure concentration, continue concentration to 18-22 Be (70-80℃) to obtain a concentrated solution. Filter the concentrated solution through a 60-mesh sieve and spray dry it into powder (inlet air temperature 170-180℃, outlet air temperature 70-90℃).

[0135] Example 2

[0136] This embodiment provides a method for preparing a lozenge for treating dry, itchy, and painful throat, including the following steps:

[0137] (1) Preparation of compound dry powder: The prescribed amount of Scrophularia, Platycodon, and Glycyrrhiza were washed with running water and put into an extraction tank. Water was added and decocted twice. For the first decoction, 12 times the weight of the medicinal materials were added and boiled for 1 hour. The decoction was then filtered. For the second decoction, 10 times the weight of the medicinal materials were added and boiled for 1 hour. The decoction was then filtered. The two filtrates were combined and concentrated to 18-22 Be. The filtrates were then spray-dried. The inlet air temperature of the spray drying tower was set to 160-180℃ and the outlet air temperature was controlled to 70-90℃. The obtained spray-dried powder was pulverized through 80 mesh to obtain the compound dry powder.

[0138] (2) Preparation of Phyllanthus emblica extract powder: Fresh Phyllanthus emblica (tannin content 3.6%) of the prescribed amount is washed, and the pitted Phyllanthus emblica is juiced to obtain juice and pomace. The pomace is juiced again, and the juices are combined, filtered, and the pomace is discarded to obtain Phyllanthus emblica juice. Phyllanthus emblica juice and water are added to a concentrator at a ratio of 1:2 and concentrated to a Baume degree of 8-10 Be. Concentration is carried out at 100℃ and atmospheric pressure for 3 hours. After atmospheric pressure concentration is completed, concentration is continued to 18-22 Be (70-80℃) to obtain a concentrated solution. The concentrated solution is filtered through a 60-mesh filter and spray-dried into powder (inlet air temperature 170-180℃, outlet air temperature 70-90℃).

[0139] (3) Preparation of gelatin sugar powder: Add 5.42 kg of purified water to 4.06 kg of gelatin; add 2.7 kg of purified water to 5.42 kg of sucrose and heat them separately in a water bath until completely melted. Then mix the two syrups together and stir evenly. The total weight should be 17.6 kg. If it is insufficient, add hot water to make up the weight to obtain gelatin syrup. Put 100 kg of sucrose powder (60-100 mesh) and 17.6 kg of hot gelatin syrup into a trough mixer and mix evenly. Place it at 60℃ to dry. When it is about 50% dry, turn the gelatin sugar block and continue to dry until the moisture content is below 3%. Use a 30B universal pulverizer to pulverize the gelatin sugar block into 60 mesh gelatin sugar powder. The final gelatin sugar powder ratio is: gelatin: sugar powder = 1.9:50. Set aside.

[0140] (4) Mix 18% compound dry powder, 3% amla dry powder, 51.9% gelatin sugar powder and 24.3% dextrin in a wet mixing granulator for 1-5 minutes. Depending on the viscosity of the material, add an appropriate amount of 75%-90% ethanol and mix for 2-4 minutes to make a soft material. Then disperse the soft material through a 10-14 mesh sieve using a swing granulator to make wet granules. Dry the wet granules in a fluidized bed dryer at 60-65℃ for 10-30 minutes. After drying, sieve the granules through a 16-20 mesh sieve and continue to dry them in a fluidized bed dryer until the moisture content is qualified.

[0141] (5) Dissolve 0.6% menthol and 0.2% borneol in 85-90% ethanol and stir until completely dissolved. Place the granules in a trough mixer, spray in the borneol and menthol solution and mix evenly. Place the resulting granules and 2% silica in a multi-directional motion mixer and mix for 30 minutes. Compress the mixture into tablets to obtain lozenges for treating dry, itchy and sore throat.

[0142] Example 3

[0143] This embodiment provides a method for preparing a lozenge for treating dry, itchy, and painful throat. The operation steps are basically the same as in Embodiment 2, except that fresh amla fruit with a tannin content of 1.7-1.9% is used as raw material.

[0144] Comparative Example 1

[0145] This comparative example provides a method for preparing compound amla throat lozenges. The operation steps are basically the same as in Example 2, except that the amla dry extract powder is prepared using a traditional process, including the following steps: fresh amla (tannin content 3.6%), washed, pitted by an automatic pitting machine, juiced, filtered, and the filtrate concentrated at negative pressure at 80℃-90℃ to 18-22Be (70-80℃) to obtain amla concentrate. The concentrate is filtered through 60 mesh and then spray-dried, with the inlet air temperature of the spray drying tower set at 170-180℃.

[0146] Comparative Example 2

[0147] This comparative example provides a method for preparing lozenges for treating dry, itchy, and sore throat. The operation steps are basically the same as in Example 2, except that the dried amla powder is prepared using a traditional process, including the following steps: fresh amla (tannin content 1.7-1.9%) is washed, pitted using an automatic pitting machine, juiced, filtered, and the filtrate is concentrated under negative pressure at 80℃-90℃ to 18-22Be (70-80℃) to obtain amla concentrate. The concentrate is filtered through a 60-mesh filter and then spray-dried, with the inlet air temperature of the spray drying tower set at 170-180℃.

[0148] Comparative Example 3

[0149] This comparative example provides a method for preparing a lozenge for treating dry, itchy, and sore throat. The operation steps are basically the same as in Example 2, except that a traditional preparation process is used with the addition of gelatin and sugar powder, including the following steps: 18% compound dry powder, 3% Phyllanthus emblica dry extract powder, 50% sugar powder, and 24.3% dextrin are mixed in a wet mixing granulator for 1-5 minutes. An appropriate amount of 1.9% gelatin solution is added as a binder, and the mixture is mixed for 2-4 minutes to form a soft mass. The soft mass is then dispersed through a 10-14 mesh sieve using a gyratory granulator to form wet granules. The wet granules are dried in a fluidized bed dryer at 60-65°C for 10-30 minutes, then screened through a 16-20 mesh sieve, and further dried in a fluidized bed dryer until the moisture content is within acceptable limits.

[0150] II. Content Determination

[0151] The contents of tannins from fresh Phyllanthus emblica fruit, gallic acid from dried Phyllanthus emblica extract powder, and the contents of the finished product were determined for lozenges prepared in Examples 2-3 and Comparative Examples 1-2 for treating dry, itchy, and painful throats. The results are shown in Table 7.

[0152] Table 7. Determination of content indicators in Compound Phyllanthus emblica throat lozenges

[0153]

[0154] The standard in Table 7 is the content requirement of Compound Phyllanthus emblica Throat Lozenges in the National Drug Standard WS-5401(B-0401)-2014Z of the State Food and Drug Administration: Each tablet of this product contains not less than 0.45mg of Phyllanthus emblica extract powder, calculated as gallic acid.

[0155] As shown in Table 7, comparing the processing methods of Examples 2-3 and Comparative Examples 1-2, the results are as follows: 1. When fresh amla raw materials with unqualified tannins are prepared into amla dry extract powder, the current preparation process cannot obtain amla dry extract powder with qualified gallic acid content, while the preparation process of this application can obtain amla dry extract powder with qualified gallic acid content; 2. When fresh amla raw materials with qualified tannins are prepared into amla dry extract powder, the gallic acid content of amla dry extract powder prepared by the current preparation process is 1.30-1.40%, which does not meet the legal standard, while the gallic acid content of amla dry extract powder obtained by the preparation process of this application is increased to 7.9-8.2%; 3. The gallic acid content in lozenges used to treat dry, itchy, and sore throat obtained by the current preparation process is 0.09-0.42 mg / tablet, which does not meet the legal standard, while the gallic acid content in lozenges used to treat dry, itchy, and sore throat obtained by the preparation process of this application is increased to 2.59-2.76 mg / tablet.

[0156] III. Appearance Comparison

[0157] The granulation process and final product appearance of the lozenges prepared for treating dry, itchy, and painful throats in Comparative Example 2 and Comparative Example 3 are shown in Table 8.

[0158] Table 8 Comparison of the preparation process of Compound Phyllanthus emblica throat lozenges

[0159]

[0160] As can be seen from Table 8, comparing the treatment results of Example 2 and Comparative Example 3: when gelatin is directly added to the granulation process as a binder for lozenges used to treat dry, itchy, and painful throats, clumping and stringing occur during the granulation process, and the finished product is unqualified in appearance due to spots and white spots. The gelatin sugar powder preparation method of this application changes the way gelatin is added, and the granulation process is smooth, stable, and feasible, and the finished product has a qualified appearance.

[0161] In summary, the preparation method provided in this application is simple in process, convenient in operation, and easy in product quality control. It is a safe and reliable preparation method suitable for industrial production. In particular, the preparation process of the Phyllanthus emblica dry extract powder of this application is stable and feasible, and the gallic acid content in the dry extract powder is significantly increased. The gallic acid content in the compound Phyllanthus emblica throat lozenges is also significantly increased, ultimately ensuring that the gallic acid content in the lozenges used to treat dry, itchy, and sore throat meets the legal requirements. This application greatly increases the content of active ingredients in the lozenges, developing a lozenge with qualified active ingredients for treating dry, itchy, and sore throat, which has high practicality, economic value, and clinical application value.

[0162] All references to this application are incorporated herein by reference as if each document were individually incorporated herein by reference. Unless they conflict with the purpose and / or technical solution of this application, all cited references are incorporated herein by reference in their entirety and for all purposes. When references are cited in this application, the definitions of relevant technical features, terms, nouns, phrases, etc., are also incorporated herein by reference. Examples and preferred embodiments of the cited technical features may also be incorporated herein by reference, but only to the extent that they enable the implementation of this application. It should be understood that when the cited content conflicts with the description in this application, this application shall prevail or modifications shall be made adaptably to the description in this application.

[0163] The technical features of the above-described embodiments and examples can be combined in any suitable manner. For the sake of brevity, not all possible combinations of the technical features in the above-described embodiments and examples are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0164] The embodiments described above merely illustrate several implementation methods of this application and should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Furthermore, it should be understood that after reading the above teachings, those skilled in the art can make various alterations or modifications to this application, and the equivalent forms obtained also fall within the protection scope of this application. It should also be understood that technical solutions obtained by those skilled in the art based on the technical solutions provided in this application through logical analysis, reasoning, or limited experimentation are all within the protection scope of the appended claims. Therefore, the protection scope of this patent application should be determined by the appended claims, and the specification can be used to interpret the content of the claims.

Claims

1. A method for preparing a dried amla extract powder, characterized in that, Includes the following steps: S100: Mix pitted fresh amla with water, juice, filter, and obtain fresh amla juice and amla residue; the weight ratio of pitted fresh amla to water is (1.8~2.2):1; S200: Mix the amla residue with water, stir, and filter to obtain amla residue liquid; the weight ratio of amla residue to water is (0.8~1.2):1; S300: Combine the fresh amla juice and the amla residue liquid, and concentrate the combined mixture to 8Be~10Be under negative pressure and 80℃~90℃ to obtain a first amla concentrate. Heat the first amla concentrate at 100℃~105℃ for 2h~4h under normal pressure to obtain a second amla concentrate. Concentrate the second amla concentrate to 18Be~22Be under negative pressure and 80℃~90℃ to obtain a third amla concentrate. The negative pressure refers to a pressure of -0.06MPa~-0.07MPa, and normal pressure refers to atmospheric pressure. S400: Spray dry the third concentrated amla extract to obtain amla powder.

2. The preparation method according to claim 1, characterized in that, The inlet air temperature of the spray dryer is 170℃~180℃, and the outlet air temperature is 70℃~90℃.

3. A dried amla extract powder prepared by the preparation method according to any one of claims 1 to 2.

4. A compound Phyllanthus emblica throat lozenge, characterized in that, Its composition, by weight percentage, is as follows: Compound dry powder 15%~20%; The dried amla extract powder according to claim 3 is 2%~4%; Gelatin sugar powder 50%~55%; Dextrin 20%~25%; Menthol 0.5%~0.7%; Borneol 0.1%~0.3%; as well as 1%~3% silicon dioxide; The compound powder is an aqueous extract of a mixture of Scrophularia, Platycodon, and Glycyrrhiza. The gelatin sugar powder contains gelatin and sucrose powder in a weight ratio of (3.5~4):100; The gelatin sugar powder is prepared by a method comprising the following steps: The gelatin and water are mixed at a weight ratio of 1:(1.2~1.4), and heated to obtain an aqueous solution of gelatin; Mix a portion of the sucrose powder and water at a weight ratio of 1:(0.4~0.6), heat, and obtain an aqueous solution of sucrose; The aqueous solution of gelatin and the aqueous solution of sucrose are mixed to obtain gelatin syrup; The gelatin syrup is heated in a water bath to 90℃~100℃, then the remaining sucrose powder is added and mixed. After mixing, it is dried at 55℃~65℃ and then pulverized.

5. A method for preparing the compound Phyllanthus emblica throat lozenges according to claim 4, characterized in that, Includes the following steps: Weigh each raw material according to the formula of the lozenges in claim 4; The compound dry powder, the amla dry extract powder, the gelatin sugar powder, the dextrin and the first alcohol solvent are mixed to obtain a soft material, and the soft material is granulated to obtain the first wet granules. The first wet particles are dried to obtain the first dry particles; The mixture of menthol and borneol is dissolved in a second alcohol solvent to prepare borneol-menthol solution; The borneol and menthol liquid is sprayed onto the first dry granules, then the silica is added and mixed, and the mixture is compressed into tablets.

6. The preparation method according to claim 5, characterized in that, The first wet granules are dried at 60℃~65℃ to obtain the first dry granules. The moisture content of the first dry granules is ≤3%.

7. The preparation method according to claim 6, characterized in that, The drying time is 10 to 30 minutes.

8. The preparation method according to any one of claims 5-7, characterized in that, The first alcohol solvent is an aqueous solution of ethanol with a volume percentage of 75% to 90%; The second alcohol solvent is an aqueous solution of ethanol with a volume percentage of 85% to 90%.

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