Red raspberry effervescent granules and preparation process thereof
The preparation process of effervescent granules of red raspberry extract was optimized by response surface methodology, which solved the problem of red raspberry fruit softening due to easy dehydration and achieved the stability and rapid disintegration of red raspberry extract, making it suitable for the development of functional foods.
Patent Information
- Application Number
- CN202511306286.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-12
- Publication Date
- 2025-12-26
AI Technical Summary
In the existing technology, red raspberry fruits have a limited shelf life due to their high water content, fast respiration rate, and fragile texture, making them prone to dehydration and softening. Furthermore, the processing of them into juice, jam, and other products does not adequately preserve their bioactive components. There is a lack of research on using effervescent particle technology to deliver red raspberry extracts.
The preparation process of effervescent granules of red raspberry extract was optimized using response surface methodology. By granulating acidic and alkaline granules separately, mannitol was used as a diluent, and polyethylene glycol 6000 and povidone K30 were used as binders and flavoring agents to form an acid-base reaction, ensuring the stability and rapid disintegration of the red raspberry extract.
The prepared red raspberry extract effervescent granules effectively isolate acid-base reactions during storage, improve the long-term stability of anthocyanins, ensure rapid disintegration and good foaming effect, enhance the physical stability and flowability of the product, have a good taste, and are suitable for the development of functional foods.
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Figure CN121197267A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of effervescent granule preparation technology, specifically relating to a red raspberry effervescent granule and its preparation process. Background Technology
[0002] Red raspberries Rubus idaeus L.), Rosaceae family, Rubus genus ( Rubus spp. Red raspberry (Rubus idaeus) is a perennial deciduous fruit tree, also known as wild raspberry. Its unripe fruit, after processing, becomes the traditional Chinese medicine Fupenzi. The fruit is a spherical aggregate of numerous drupes, turning deep red when ripe and easily detaching from the receptacle. As a berry with both medicinal and edible value, the nutritional system of red raspberry consists of various bioactive substances, including polyphenols, vitamins, minerals, fructose, and its unique component raspberry ketone. Polyphenols are abundant in red raspberries. Natural polyphenols with multiple phenolic hydroxyl groups in their molecular structure exhibit significant antioxidant activity by preferentially reacting with free radicals, thus preventing lipid peroxidation products from attacking biomolecules such as proteins, nucleic acids, and lipids. Therefore, they play a crucial role in preventing cardiovascular disease, lowering blood lipids, and regulating lipid metabolism. Numerous studies have shown that consuming red raspberries can reduce oxidative stress, dyslipidemia, inflammation, and hypertension, while also regulating the gut microbiota. Studies have shown that silver nanoparticles synthesized using red raspberry fruit extracts have effective antioxidant activity against DPPH free radicals (DEMIRBAS A, YILMAZ V, ILDIZ N, et al. Anthocyanins-rich berry extracts directed formation of Ag NPs with the investigation of their antioxidant and antimicrobial activities[J]. Journal of Molecular Liquids, 2017, 248: 1044-1049.). However, red raspberries are highly perishable due to their high water content, rapid respiration rate, and fragile texture. They are extremely prone to dehydration and softening after harvesting, losing freshness, and even at 0℃, their storage period is extremely limited. This perishable characteristic has led to the processing of red raspberries into products such as juice, jam, vinegar, wine, canned goods, and chewable tablets. Although these processed products retain the color and flavor of the fruit to some extent, they still have significant shortcomings in the retention of bioactive components. With technological advancements, freeze-drying technology, through low-temperature vacuum dehydration, can maximize the preservation of the activity of heat-sensitive bioactive substances (such as proteins, polyphenols, and vitamins). This technology combines excellent bioactivity protection capabilities, physical structural stability, long-term storage, and convenient transportation, and has been widely applied in the pharmaceutical, food, and scientific research fields.
[0003] Effervescent formulations have garnered significant attention due to their small size, portability, ease of administration, pleasant taste, and high patient compliance. Effervescent granules, a typical example, work by reacting an organic acid with a weak base (usually a carbonate / bicarbonate) to release CO2, forming an effervescent solution. This dosage form combines the rapid disintegration of effervescent tablets with the high portability of ordinary granules, while overcoming the limitations of effervescent tablets, such as larger size, complex manufacturing processes, stringent moisture-proof packaging requirements, and potentially longer disintegration times. Furthermore, effervescent granules offer advantages such as low cost, easy encapsulation of active ingredients, rapid release, high bioavailability, and a pleasant taste. Their applications extend beyond pharmaceutical preparations to the development of health foods, such as red ginger effervescent granules, pomegranate effervescent granules, and vitamin C effervescent granules. However, research on the delivery of red raspberry extract using effervescent granule technology remains relatively scarce. Therefore, there is an urgent need to research and develop a preparation process for red raspberry extract effervescent granules with antioxidant functions. Summary of the Invention
[0004] To address the aforementioned technical problems, the purpose of this invention is to provide a response surface methodology-based optimization method for the preparation process of effervescent granules made from red raspberry extract. This study used freeze-dried red raspberry extract powder as raw material, screened the basic formulation dosage based on single-factor experiments, and then optimized the effervescent granule preparation process using response surface methodology. The influencing factors and related quality indicators on the effervescent granule preparation process were investigated, aiming to provide a reference for the market launch of this product.
[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows: This invention provides effervescent granules of red raspberry extract, comprising acid granules and alkaline granules. The acid granules contain the active ingredient, freeze-dried red raspberry extract powder, the acidic disintegrant citric acid, the diluent mannitol, and a binder. The alkaline granules contain the alkaline disintegrant sodium bicarbonate encapsulated by an inclusion agent, the diluent mannitol, and the binder. Based on the total weight of the effervescent granules, the weight percentages of each component are: freeze-dried red raspberry extract powder 15-25%, mannitol 40-60%, binder 2-6%, disintegrant 30-40%, flavoring agent 0.5-2%, and inclusion agent 0.1-1%. The weight ratio of mannitol in the acid granules to the alkaline granules is 1:1.5-1.5:1, the weight ratio of the binder in the acid granules to the alkaline granules is 1:1.5-1.5:1, and the weight ratio of the acidic disintegrant citric acid to the alkaline disintegrant sodium bicarbonate is 1:1.5-1.5:1.
[0006] Based on the above technical solution, further, based on the total weight of the effervescent granules, the weight percentage of each component is as follows: 15-21% freeze-dried red raspberry extract powder, 40-50% mannitol, 3-5% binder, 30-40% disintegrant, 0.5-2% flavoring agent, and 0.1-0.5% inclusion agent.
[0007] Based on the above technical solution, further, the weight ratio of mannitol in acid particles to alkali particles is 1:1, the weight ratio of binder in acid particles to alkali particles is 1:1, and the weight ratio of acidic disintegrant citric acid to alkali disintegrant sodium bicarbonate is 1:1.3.
[0008] Based on the above technical solution, the incorporating agent is polyethylene glycol 6000, the adhesive is polyvinylpyrrolidone K30 (PVP-K30), and the flavoring agent is acesulfame potassium.
[0009] The present invention also provides a preparation process for the above-mentioned raspberry extract effervescent granules, comprising the following steps: S1: Mix red raspberry extract freeze-dried powder, acidic disintegrant citric acid and diluent mannitol evenly, add a solution containing binder to make wet acid granules, and dry to obtain acid granules; S2: Mix the encapsulated alkaline disintegrant sodium bicarbonate with the diluent mannitol evenly, add the solution containing the binder to make wet alkaline granules, and dry them to obtain alkaline granules. S3: Mix the obtained acid granules, alkali granules and flavoring agent evenly to obtain red raspberry extract effervescent granules.
[0010] Based on the above technical solution, further, the adhesive-containing solution mentioned in S1 and S2 is a 5~6% PVP-K30 anhydrous ethanol solution.
[0011] Based on the above technical solution, the process of preparing wet acid granules in S1 and wet alkali granules in S2 is the same. Specifically, the process is as follows: add a solution containing binder to the obtained mixture, stir continuously until a soft material with uniform plasticity is formed, and granulate the obtained soft material through a 20-40 mesh sieve.
[0012] Based on the above technical solution, further, the drying described in S1 and S2 specifically refers to drying in a constant temperature drying oven at 40~80℃.
[0013] Based on the above technical solution, the specific preparation process of the included alkaline disintegrant sodium bicarbonate in S2 is as follows: weigh polyethylene glycol 6000 and heat it in a water bath to melt it, pour in sodium bicarbonate, stir it quickly, and after cooling and solidification, grind and crush it, and pass it through a 20-40 mesh sieve to obtain the product.
[0014] This invention fully preserves the active ingredients of red raspberry extract during the preparation process and combines them with the functions of excipients to create a natural nutritional food that combines deliciousness and health benefits. Furthermore, the effervescent granules produced by this invention possess the unique aroma of red raspberries, have a balanced sweet and sour taste, are neither astringent nor bitter, have a unique flavor, and contain no pigments or preservatives. They also enhance the body's immunity, aligning with the current development trend of functional foods. Simultaneously, the preparation process of this invention is scientifically sound, simple, easy to implement, low-cost, and highly efficient, providing a valuable reference for the development of subsequent functional foods.
[0015] Red raspberry extract, as the main active ingredient, possesses various health benefits, but its poor chemical stability makes it susceptible to degradation and inactivation due to factors such as acidity, alkalinity, moisture, and temperature. Traditional homogenization or wet granulation processes for effervescent granules cannot meet its stability requirements. This invention innovatively employs a compound formulation structure where "acid granules" and "alkali granules" are granulated independently. The acid source (citric acid), along with the red raspberry extract and diluent (mannitol), are granulated together to form the "acid granule group." The alkali source (sodium bicarbonate) and remaining excipients are granulated to form the "alkali granule group." Finally, the dried granules are physically mixed to obtain the final product. By physically isolating the reaction precursors, the acid (H+) is effectively isolated during storage. + Source) and alkali (HCO3) - The acid and alkali particles react rapidly with water in the solid state to prevent the release of water or CO2, thus avoiding hydrolysis or oxidative degradation of anthocyanins. This minimizes the exposure of raspberry extract to unfavorable microenvironments (local high acidity or high alkaliity) during preparation and storage, significantly improving the long-term stability of anthocyanins and the product's shelf life. When in use, the acid and alkali particles come into rapid contact with water and undergo a highly efficient acid-base reaction, generating sufficient CO2 to ensure rapid disintegration and good foaming effect.
[0016] Addressing the limitations of traditional effervescent granules, which commonly use lactose as a diluent, such as its suitability for lactose-intolerant individuals and the tendency of microcrystalline cellulose (MCC) to absorb moisture and clump, severely impacting the physical stability (hygroscopicity) and disintegration properties of effervescent granules, this invention utilizes mannitol as a diluent. Mannitol, being a non-lactose source, broadens the product's target population. Its significantly lower hygroscopicity compared to MCC greatly reduces the risk of clumping and improves the product's physical stability and flowability. Furthermore, mannitol itself has a certain disintegration-promoting effect, synergistically ensuring good disintegration with the optimized acid-base system. Simultaneously, mannitol possesses health benefits such as low calories and anti-caries properties, synergistically complementing the health benefits of anthocyanins.
[0017] Traditional single-process granulation (such as wet granulation) cannot simultaneously meet the requirements of anthocyanin stability protection, isolation of acid-base reaction precursors, and guarantee of final disintegration and foaming performance. Conventional processes are prone to quality instability (such as anthocyanin degradation, particle clumping, and slow disintegration). This invention systematically integrates the core scheme of separate granulation of acid / base particles with diluent optimization (mannitol) and specific disintegrants (citric acid + sodium bicarbonate) to form a complete preparation process. This process is not a simple superposition of elements, but effectively combines the low hygroscopicity, suitable taste, and disintegration-aiding properties of mannitol with the efficient disintegration and foaming ability of the citric acid / sodium bicarbonate system through the core means of "separate granulation". Ultimately, it achieves multiple synergistic effects of effective protection of unstable active pharmaceutical ingredients (improved stability), enhanced physical stability of the product (anti-hygroscopic clumping), optimized disintegration speed and foaming volume, and lactose-free formulation, thus improving the core contradictions faced by traditional effervescent granules when applied to highly active and unstable ingredients.
[0018] Compared with the prior art, the present invention has the following beneficial effects: This invention uses freeze-dried powder of natural raspberry extract as raw material to develop an effervescent granule formulation of raspberry extract. The method combines single-factor experiments and response surface methodology to screen the optimal process conditions for jam preparation: 20 g of raspberry extract, 1 g of acesulfame potassium, 48.5 g of mannitol (the weight ratio of mannitol in acid granules to alkali granules is 1:1), 4 g of binder (the weight ratio of binder in acid granules to alkali granules is 1:1, 5.8% PVP-K30 anhydrous ethanol solution), 35 g of disintegrant (acid-alkali ratio of 1:1.3), and 0.2 g of PEG. The sensory score of the effervescent granules prepared under these optimized conditions was 93 points, which highly matched the model prediction (93.67 points). The results of measuring the angle of repose of the freeze-dried red raspberry extract powder and the effervescent granules showed that, compared to the original angle of repose of 31.89° for the freeze-dried red raspberry powder, the angle of repose of the effervescent granules was significantly reduced to 14-19° after process optimization using single-factor experiments and response surface methodology, indicating a significant improvement in the flowability of the effervescent granules. This improvement effectively enhanced the flow uniformity of red raspberry extract in filling equipment, demonstrating that process optimization of effervescent granules can achieve a dual improvement in production stability and quality. Furthermore, the resulting effervescent granules, when mixed with water, produced a light pink solution with a pleasant sweet and sour taste and no off-odors; the solution was also uniform, providing a theoretical basis for future product development. Attached Figure Description
[0019] To more clearly illustrate the embodiments of the present invention, the accompanying drawings involved in the embodiments will be briefly described below.
[0020] Figure 1This is a process flow diagram for preparing the red raspberry extract effervescent granules of the present invention.
[0021] Figure 2 The effect of the amount of red raspberry extract added on the sensory score of red raspberry extract effervescent granules is shown in the figure.
[0022] Figure 3 The effect of the ratio of PEG6000 to alkaline disintegrant on the sensory score of red raspberry extract effervescent granules is shown in the figure.
[0023] Figure 4 The graph shows the effect of pH ratio on the sensory score of red raspberry extract effervescent granules.
[0024] Figure 5 The effect of mannitol addition on the sensory score of red raspberry extract effervescent granules is shown in the figure.
[0025] Figure 6 The graph shows the effect of different binder concentrations on the sensory scores of red raspberry extract effervescent granules.
[0026] Figure 7 Response surface plot and contour plot of the interaction between the amount of red raspberry extract and the amount of mannitol added on the sensory score.
[0027] Figure 8 Response surface plots and contour plots showing the effect of the interaction between the amount of red raspberry extract added and the concentration of binder on sensory scores.
[0028] Figure 9 Response surface plot and contour plot of the interaction between mannitol addition and binder concentration on sensory score.
[0029] Figure 10 The graph shows the DPPH free radical scavenging ability of red raspberry extract. Detailed Implementation
[0030] The present invention will be described in detail below with reference to the embodiments. However, the implementation of the present invention is not limited thereto. Obviously, the embodiments described below are only some embodiments of the present invention. For those skilled in the art, other similar embodiments can be obtained without creative effort and all fall within the protection scope of the present invention.
[0031] Example 1 Red raspberry extract was purchased from Hansuyuan (Shaanxi) Biotechnology Co., Ltd. Sodium bicarbonate and mannitol (analytical grade) were purchased from Tianjin Hengxing Chemical Reagent Manufacturing Co., Ltd. Polyethylene glycol 6000 (analytical grade) was purchased from Sinopharm Chemical Reagent Co., Ltd. PVP-K30 (food grade) was purchased from Ulanqab Kema New Materials Co., Ltd. Anhydrous ethanol (analytical grade) was purchased from Lianlong Bohua (Tianjin) Pharmaceutical Chemical Co., Ltd.
[0032] Reference Figure 1 This embodiment provides a process for preparing red raspberry effervescent granules, comprising, by weight: 5.4 g of freeze-dried red raspberry powder, 52.6 g of mannitol (26.3 g of mannitol in acid granules and 26.3 g of mannitol in alkali granules), 4.4 g of binder PVP-K30 (using a 6% PVP-K30 anhydrous ethanol solution, with a binder weight ratio of 1:1 in acid and alkali granules), 34 g of disintegrant (citric acid in acid granules and sodium bicarbonate in alkali granules in a mass ratio of 1:1.3), and 3.6 g of inclusion agent PEG6000. First, the acid granules are prepared: freeze-dried red raspberry extract powder, citric acid, and a portion of mannitol are placed in a mixing device and stirred at a predetermined speed until uniformly mixed; then, an anhydrous ethanol solution of povidone K30 is added to the mixture as a binder, and stirring is continued until a soft material with uniform plasticity is formed; the obtained soft material is granulated through a 20-mesh sieve to obtain wet acid granules; then, the wet acid granules are dried at 60°C, and the moisture content of the granules is controlled to meet the standard requirements to obtain dry acid granules; at the same time, a certain amount of PEG6000 is weighed and heated to melt in a water bath. After completing the above steps, sodium bicarbonate is poured in, stirred rapidly, and after cooling and solidification, it is ground and pulverized through a mortar and pestle and passed through a 40-mesh sieve for later use. Next, the alkaline granules are prepared: Equal amounts of mannitol from the encapsulated sodium bicarbonate and acid granules are added to a mixing device and thoroughly mixed. Then, an anhydrous ethanol solution of povidone K30 is added as a binder, and the mixture is stirred until a uniform soft mass is formed. This soft mass is then granulated through a 20-mesh sieve to obtain wet alkaline granules. The wet alkaline granules are dried at 60°C until the moisture content meets the set range, finally obtaining dried alkaline granules. Finally, mixing and packaging are performed. The dried acid and alkaline granules are quantitatively filled into the two independent channels of a dual-channel granule filling machine and immediately sealed to obtain a unit dose of double-packaged red raspberry extract effervescent granules.
[0033] Example 2 The single-factor experiment specifically used sensory scores as the evaluation index. With other factors and levels kept constant, the addition amount of effervescent granules was determined by the effects of the proportion of red raspberry extract, the proportion of mannitol, the pH ratio, the ratio of PEG6000 to basic disintegrant, and the concentration of binder on the sensory scores of effervescent granules.
[0034] 1. Single-factor experiment (1) The specific operation method and steps are the same as those in Example 1 for particle preparation. Under the condition that the influencing factors are 1 g of acesulfame potassium, 48.5 g of mannitol (the weight ratio of mannitol in acid particles to alkali particles is 1:1), 4 g of 6% PVP-K30 anhydrous ethanol solution (the weight ratio of binder in acid particles to alkali particles is 1:1), 35 g of disintegrant (the acid-base ratio is 1:1.3) and 0.2 g of PEG 6000 inclusion agent, different amounts of red raspberry extract (5 g, 10 g, 15 g, 20 g, 25 g) are added to conduct single-factor experiments on this effervescent granule. Sensory evaluation is carried out on the effervescent granules with different contents of red raspberry extract. The optimal amount of red raspberry extract is determined based on the evaluation results.
[0035] Sensory evaluation, as a scientific method for food quality analysis, is a method in which trained evaluators use their sensory systems (sight, smell, taste, touch, etc.) to scientifically analyze a product. This red raspberry extract effervescent granules underwent sensory quality evaluation by a panel of individuals of different genders, ages, and with food-related professional backgrounds. Panel members were selected based on criteria including good health, no unhealthy habits, sensitive taste, and received sensory evaluation technical guidance before the formal evaluation. During the sensory evaluation, panel members used small cups to take small amounts of each sample, tasted them, and after evaluating each sample, spat it out and rinsed their mouths with warm purified water to remove any food residue. Maintaining a fresh oral environment helps evaluators obtain more accurate results during sensory evaluation. Sensory scores were based on three aspects: effervescence time, clarity, and taste. Scores were based on a 100-point scale, and the final average score was taken as the panel's score to ensure the fairness and accuracy of the evaluation results.
[0036] Table 1 Sensory Evaluation Table of Red Raspberry Extract Effervescent Granules
[0037] The effect of different amounts of red raspberry extract added on the sensory scores of effervescent granules is as follows: Figure 2As shown, when the amount of red raspberry extract added is within the range of 5-20 g, the sensory score of the granules gradually increases with the increase of the amount of red raspberry extract added. When the amount of red raspberry extract added is 20 g, the sensory score reaches the highest score (92 points), and the effervescent granules after brewing are bright in color, showing the pink color of red raspberries, and have a moderately sweet and sour taste. However, when the amount of red raspberry extract added is greater than 20 g, the sour and astringent taste of the effervescent granules is slightly enhanced, causing the sensory score to decrease. This indicates that anthocyanins are both functional ingredients and may introduce unpleasant flavors if added in excess. It is necessary to balance their efficacy and palatability to determine the optimal amount to add.
[0038] (2) The specific operation method and steps are the same as those in Example 1 for particle preparation. Under the condition that other influencing factors remain unchanged, different ratios of PEG6000 to basic disintegrant (sodium bicarbonate) (0.1:1, 0.3:1, 0.5:1, 0.7:1, 0.9:1) are set to conduct single-factor experiments on this effervescent granule. Sensory evaluation is performed on the above different granules, and the optimal ratio of PEG6000 to basic disintegrant is determined based on the evaluation results.
[0039] The results are as follows Figure 3 As shown, when the ratio of PEG6000 to basic disintegrant is 0.7:1, the sensory score of the granules reaches 88 points; while when the ratio is reduced or increased, the sensory score remains above 85 points, which suggests that different ratios of PEG6000 to basic disintegrant have little impact on the sensory score of granules.
[0040] (3) The specific operation method and steps are the same as those in Example 1 for particle preparation. Under the condition that other influencing factors remain unchanged, different acid-base ratios (0.5, 0.67, 1, 1.33, 2) are set to conduct single-factor experiments on this effervescent granule. Sensory evaluation is performed on the above different granules, and the optimal acid-base ratio is determined based on the evaluation results.
[0041] The effects of different pH ratios on the sensory scores of effervescent granules are as follows: Figure 4 As shown, when the pH ratio gradually increases within the range of 0.5 to 1.0, the sensory score of effervescent granules shows a gradual change trend; when the pH ratio increases to 1.33, the sensory score reaches its highest point (90 points); however, when the pH ratio increases to 2.0, the sour taste of the granules intensifies, and the score decreases. Based on this, the optimal pH ratio for effervescent granules is determined to be 1:1.33.
[0042] (4) The specific operation method and steps are the same as those in Example 1 for particle preparation. Under the condition that other influencing factors remain unchanged, different amounts of mannitol are set (10 g, 30 g, 50 g, 70 g, 90 g, wherein each group of mannitol is divided into two equal parts and added when preparing acid granules and alkali granules respectively) to conduct single-factor experiments on this effervescent granule. Sensory evaluation is carried out on the effervescent granules with different amounts of mannitol added, and the optimal amount of mannitol is determined based on the evaluation results.
[0043] The effect of different mannitol addition amounts on the sensory scores of effervescent granules is as follows: Figure 5 As shown, the sensory scores for effervescent granules with mannitol addition ranging from 10 to 50 g increased with increasing mannitol content, reaching a maximum of 93 points at 50 g. However, the sensory scores decreased when the mannitol addition exceeded 50 g. The reason why the amount of mannitol added affects the sensory scores of effervescent granules may be that at low addition levels, the sweetness provided by mannitol is insufficient, resulting in a more sour and astringent taste; while at high addition levels, the excessive proportion of mannitol leads to a relative decrease in anthocyanin content and a lighter color.
[0044] (5) The specific operation method and steps are the same as those in Example 1 for particle preparation. Under the condition that other influencing factors remain unchanged, the binder is (PVP-K30-ethanol solution). In the process of preparing the soft material, the addition amount of acid granules and alkali granules is 1:1. On this basis, different binder concentrations are set (1 is 75% ethanol solution; 2 is 4% PVP-K30 anhydrous ethanol solution; 3 is 6% PVP-K30 anhydrous ethanol solution; 4 is 8% PVP-K30 anhydrous ethanol solution; 5 is 100% anhydrous ethanol solution, where anhydrous ethanol refers to 100% ethanol solution). Single-factor experiments are carried out on this effervescent granule, and sensory evaluation is carried out on the effervescent granules with different binder concentrations. The optimal binder concentration is determined based on the evaluation results.
[0045] Different concentrations of PVP-K30-ethanol solution were used as binders, and the effects of different binder concentrations on the sensory scores of effervescent granules were discussed. The results are as follows: Figure 6 As shown, the sensory score was lower when using anhydrous ethanol and a 4% PVP-K30-ethanol solution as binders; however, the sensory score reached its maximum of 90 points when using a 6% PVP-K30-ethanol solution. The improved score is likely due to the effervescent granules prepared with a 6% PVP-K30-ethanol solution as a binder having moderate hardness, while also avoiding clumping caused by excessive binder, thus improving the sensory score. Further increasing the concentration of the PVP-K30-ethanol solution resulted in a lower sensory score, possibly because the excessively high concentration caused excessive granule adhesion, leading to a prolonged effervescence time.
[0046] 2. Response surface methodology optimization The response surface methodology (RSM) experiment was conducted based on the single-factor experiment. The sensory score of the red raspberry effervescent granules was used as the response value (Z), and the A-red raspberry extract addition amount, B-mannitol addition amount, and C-binder concentration were used as the experimental factors. The three-factor, three-level Box-Behnken RSM experiment was designed using DesignExpert 8.0.6 software to determine the red raspberry extract addition amount, B-mannitol addition amount, and C-binder concentration.
[0047] Based on the results of previous single-factor experiments, among five factors—the amount of red raspberry extract added, the ratio of PEG 6000 to basic disintegrant, the amount of mannitol added, the pH ratio, and the binder concentration—three factors with a significant impact on the preparation of red raspberry extract effervescent granules were selected. A three-level, three-factor response surface methodology was then conducted to further optimize the process. For each experimental point, three different levels (low, medium, and high) were used to test the factors to determine the optimal process parameters for sensory evaluation. The response surface methodology design is shown in Table 2.
[0048] Table 2. Experimental Design Table for 3-Factor, 3-Level Response Surface Analysis
[0049] Based on the results of the single-factor experiments, three factors were selected for response surface methodology: the amount of red raspberry extract added (A), the amount of mannitol added (B), and the concentration of binder (C). Sensory score (Y) was used as the response value. Design Expert 8.0.6 software was used to conduct a three-factor, three-level response surface methodology experiment on red raspberry effervescent granules according to the Box-Behnken experimental design principle. The factor design level table is shown in Table 3.
[0050] Table 3 Results of Response Surface Methodology Experiments
[0051] Table 4 shows the ANOVA analysis of the binomial model.
[0052] Note: ** indicates highly significant (P < 0.01), * indicates significant (P < 0.05).
[0053] Using Design Expert 8.0.6 software, a multivariate analysis was conducted with the amount of red raspberry extract added (A), mannitol added (B), and binder concentration (C) as variables, and sensory score (Y) as the response value. The quadratic regression equation was obtained: Sensory score Y = 93.40 + 0.1250 A - 0.6250 B - 1.75 C - 1.25 AB - 1.50 AC + 0.5000 BC - 2.83 A 2 -2.83 B 2 -4.07 C 2 The ANOVA results for the binomial model are shown in Table 4. The regression model is highly significant (P < 0.01), and the lack-of-fit term (P = 0.5969) is insignificant. The model's coefficient of determination R0 is also shown. 2 =0.9611, this data indicates a good fit, and the adjusted coefficient of determination is Adj R. 2 =0.9111, confirming a high degree of correlation between the predicted and actual values. Therefore, this regression model is suitable for analyzing the sensory scores of red raspberry extract effervescent granules by considering variables (red raspberry extract addition A, mannitol addition B, and binder concentration C). The data indicate that AC has a significant impact on the sensory scores of effervescent granules (P<0.05), and C and A... 2 B 2 C 2 The effect was highly significant (P < 0.01), while A, B, AB, and BC had no significant effect (P > 0.05). Furthermore, a larger F-value indicates a greater influence of the independent variable on the dependent variable, meaning a stronger explanatory power of the independent variable on the dependent variable. According to the regression analysis of variance, different factors had varying degrees of influence on the sensory scores of red raspberry extract effervescent granules, with the order of influence for the three factors being: binder concentration > mannitol addition > red raspberry extract addition. In conclusion, this regression model is effective and can be considered a feasible method for optimizing the preparation process of red raspberry extract effervescent granules.
[0054] This embodiment uses response surface methodology and contour plots to evaluate the effects of the interaction between the amount of red raspberry extract, mannitol, and binder concentration on sensory scores. (1) Effect of the interaction between the amount of red raspberry extract and the amount of mannitol added on sensory scores The effects of red raspberry extract and mannitol additions on sensory scores and their interaction results are as follows: Figure 7 As shown in the figure, and combined with the analysis in Table 4, it can be seen that the interaction term between the two has no significant effect on the sensory score (P>0.05).
[0055] (2) Effect of the interaction between the amount of red raspberry extract added and the concentration of binder on sensory scores The response surfaces of red raspberry extract addition amount A and binder concentration C are as follows: Figure 8 As shown in the AC response surface, the sensory score initially increases slowly with increasing raspberry extract concentration, then decreases. With increasing binder concentration, the sensory score initially increases and then decreases. Both raspberry extract and binder concentrations significantly affect the sensory score, with a significant interaction (P<0.05). It is speculated that a better sensory score can be obtained with approximately 19.5–20.5 g of raspberry extract and approximately 5.3%–6.3% binder concentration. The gradient of sensory score change with increasing binder concentration for effervescent granules is greater than that for raspberry extract, suggesting that the binder concentration has a greater impact on the sensory score than the raspberry extract concentration.
[0056] (3) Effect of the interaction between mannitol addition and binder concentration on sensory scores The effects of mannitol addition and binder concentration on sensory scores and the interaction between the two, such as Figure 9 As shown in the figure, and combined with the analysis in Table 4, it can be seen that the interaction term between the two has no significant effect on the sensory score (P>0.05).
[0057] Optimal Process Validation: The response data was analyzed using the statistical software Design Expert 8.0.6. The optimal conditions for the three factors examined, determined through regression model analysis, were: 20.12 g of red raspberry extract, 48.4 g of mannitol, and 5.75% binder concentration, with a predicted score of 93.67. These conditions were then modified based on actual experimental conditions to 20 g of red raspberry extract, 48.5 g of mannitol, and 5.8% binder concentration. Red raspberry effervescent granules were prepared under these conditions, and three repeated experiments yielded an average sensory score of 93, which is close to the 93.67 predicted by the regression model. This indicates that the model and method have good feasibility. Example 3 The flowability of lyophilized red raspberry extract powder and effervescent granules was evaluated using the angle of repose. A smaller angle of repose indicates better flowability. Generally, granules are considered to have good flowability when the angle of repose is less than 30°.
[0058] Method for determining the angle of repose: Select a petri dish, fix the funnel so that the granules can flow out and fall into the center of the petri dish, pour the granules into the funnel until the tip of the cone formed by the granules touches the mouth of the funnel, measure the diameter of the bottom of the cone (2R) and the height of the cone (H), and calculate the angle of repose θ according to the formula tanθ=H / R. Repeat 3 times, record and take the average value.
[0059] The angle of repose of the freeze-dried red raspberry extract powder is shown in Table 5. The angle of repose was 31.89°, which is higher than 30°, indicating poor flowability of the raw material powder. This characteristic may lead to dosage deviations and material residue risks during quantitative dispensing of the freeze-dried powder, thereby increasing production losses.
[0060] Table 5. Results of Angle of Repose Measurement for Lyophilized Red Raspberry Extract Powder
[0061] After optimizing the effervescent granule process through single-factor experiments and response surface methodology, the results of the angle of repose measurements for the prepared effervescent granules are shown in Table 6-7. The angle of repose of the effervescent granules is in the range of 14~19°, which is significantly lower than that of the original freeze-dried powder, and the flowability of the effervescent granules is significantly improved. This improvement effectively enhances the flow uniformity of red raspberry extract in filling equipment, indicating that process optimization of effervescent granules can achieve a dual improvement in production process stability and quality.
[0062] Table 6 Results of repose angle determination for effervescent granules in single-factor experiments
[0063] Table 7 Results of Angle of Repose Measurement for Effervescent Granules in Response Surface Methodology Tests
[0064] Example 4 Prepare a 0.1 mmol / L DPPH solution and store it in a brown bottle, protected from light. Prepare solutions of different concentrations (0.5–16 mg / mL), with an equivalent concentration of vitamin C as a positive control. Add 100 μL of ethanol and 100 μL of DPPH solution, 100 μL of raspberry extract solution (0.5–16 mg / mL) and 100 μL of anhydrous ethanol, and 100 μL of raspberry extract solution and 100 μL of DPPH solution to each well of a 96-well plate, using ethanol as a blank control. React for 30 min in the dark, and measure the absorbance at 517 nm for each solution. Treat vitamin C at the same concentration as the raspberry extract solution in the same way as the sample solutions. The DPPH scavenging rate is expressed as SA (%) and calculated using the following formula.
[0065]
[0066] In the formula: A1 represents the absorbance value at 517 nm after the red raspberry extract solution is mixed with DPPH solution; A2 represents the absorbance value at 517 nm after the red raspberry extract solution is mixed with ethanol. The results are as follows Figure 10As shown, in the concentration range of 0.5–16 mg / mL, the DPPH free radical scavenging rate of red raspberry extract lyophilized powder and vitamin C increased with increasing working solution concentration. When the concentration reached 8 mg / mL, the maximum scavenging rate of red raspberry lyophilized powder reached 69.39%, while the scavenging rate of vitamin C remained relatively stable between 92% and 93%, with minimal fluctuations. These experimental results suggest that red raspberry extract lyophilized powder possesses certain antioxidant activity.
[0067] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A type of effervescent granules containing red raspberry extract, characterized in that, The product comprises acid granules and alkaline granules. The acid granules contain the active ingredient, freeze-dried red raspberry extract powder, the acidic disintegrant citric acid, the diluent mannitol, and a binder. The alkaline granules contain the alkaline disintegrant sodium bicarbonate encapsulated in an inclusion agent, the diluent mannitol, and a binder. Based on the total weight of the effervescent granules, the weight percentages of each component are: freeze-dried red raspberry extract powder 15-25%, mannitol 40-60%, binder 2-6%, disintegrant 30-40%, flavoring agent 0.5-2%, and inclusion agent 0.1-1%. The weight ratio of mannitol in the acid granules to the alkaline granules is 1:1.5-1.5:1; the weight ratio of the binder in the acid granules to the alkaline granules is 1:1.5-1.5:1; and the weight ratio of the acidic disintegrant citric acid to the alkaline disintegrant sodium bicarbonate is 1:1.5-1.5:
1.
2. The red raspberry extract effervescent granules according to claim 1, characterized in that, Based on the total weight of the effervescent granules, the weight percentages of each component are as follows: 15-21% freeze-dried red raspberry extract powder, 40-50% mannitol, 3-5% binder, 30-40% disintegrant, 0.5-2% flavoring agent, and 0.1-0.5% inclusion agent.
3. The red raspberry extract effervescent granules according to claim 1, characterized in that, The weight ratio of mannitol in acid particles to alkali particles is 1:1, the weight ratio of binder in acid particles to alkali particles is 1:1, and the weight ratio of acidic disintegrant citric acid to alkali disintegrant sodium bicarbonate is 1:1.
3.
4. The red raspberry extract effervescent granules according to claim 1, characterized in that, The inclusion agent is polyethylene glycol 6000, the binder is polyvinyl acetate K30 (PVP-K30), and the flavoring agent is acesulfame potassium.
5. The preparation process of the red raspberry extract effervescent granules according to any one of claims 1-4, characterized in that, Includes the following steps: S1: Mix red raspberry extract freeze-dried powder, acidic disintegrant citric acid and diluent mannitol evenly, add a solution containing binder to make wet acid granules, and dry to obtain acid granules; S2: Mix the encapsulated alkaline disintegrant sodium bicarbonate with the diluent mannitol evenly, add the solution containing the binder to make wet alkaline granules, and dry them to obtain alkaline granules. S3: Mix the obtained acid granules, alkali granules and flavoring agent evenly to obtain red raspberry extract effervescent granules.
6. The preparation process according to claim 5, characterized in that, The adhesive-containing solutions mentioned in S1 and S2 are 5-6% PVP-K30 anhydrous ethanol solutions.
7. The preparation process according to claim 5, characterized in that, The process for preparing wet acid granules in S1 and wet alkali granules in S2 is the same. Specifically, a solution containing binder is added to the resulting mixture, and the mixture is stirred continuously until a soft material with uniform plasticity is formed. The resulting soft material is then granulated by passing it through a 20-40 mesh sieve.
8. The preparation process according to claim 5, characterized in that, The drying process described in S1 and S2 specifically involves drying in a constant temperature drying oven at 40~80℃.
9. The preparation process according to claim 5, characterized in that, The specific preparation process of the inclusion alkaline disintegrant sodium bicarbonate described in S2 is as follows: Weigh polyethylene glycol 6000 and heat it in a water bath to melt it. Pour in sodium bicarbonate, stir it quickly, and after it cools and solidifies, grind it into powder and pass it through a 20-40 mesh sieve to obtain the product.