Hippophae rhamnoides fruit powder oral instant film and preparation method thereof

Abstract

The invention discloses a hippophae rhamnoides fruit powder oral instant film and a preparation method thereof. The preparation method of the hippophae rhamnoides fruit powder oral instant film comprises the following steps: preparing a dispersion liquid of potato pregelatinized starch, dispersing, adding hippophae rhamnoides fruit powder and sorbitol, and continuously dispersing to obtain a film forming liquid; and pouring the film forming liquid into a culture dish, and drying to obtain the film. The mass concentration of the potato pregelatinized starch in the dispersion liquid is 1-4% (w / v, g / mL), the addition amount of the sea buckthorn fruit powder is 10-20% of the mass of the potato pregelatinized starch, the addition amount of the sorbitol is 25-35% of the mass of the potato pregelatinized starch, the dispersion time of the dispersion liquid is 20-40 min, and the drying temperature is 30-40 DEG C. Based on unique physicochemical properties and rich bioactive components of the sea buckthorn fruit powder, the sea buckthorn fruit powder can play an excellent drug carrier role in the oral instant film, the requirements of the market for an efficient and convenient oral administration mode are met, and the sea buckthorn fruit powder oral instant film has the advantages of being easy to store, transport and use and the like.

Description

Technical Field

[0001] The invention relates to an oral instant seabuckthorn fruit powder film and a preparation method thereof, belonging to the technical field of new food material development. Background Art

[0002] Oral fast dissolving films (OFDF), also known as orally disintegrating films, mouth dissolving films, oral thin films, oral dispersible films and oral strips, are generally prepared into polymer films the size of stamps, which can be cut at will when taken. They are a new type of solid rapid-release preparations absorbed by the oral mucosa. Oral fast dissolving films are divided into three types: oral films, sublingual films and buccal films. Oral films release active ingredients directly into the oral cavity or gastrointestinal tract. The working principle of sublingual films and buccal films is to absorb active ingredients through the proximal mucosa, avoiding the first metabolism or gastrointestinal degradation, so as to quickly exert the therapeutic effect.

[0003] As a new platform for delivering active substances, oral fast-dissolving films have many advantages. Compared with other oral solid preparations, fast-dissolving films can dissolve quickly in the mouth without the need for water, reducing the risk of inhalation or choking; nutrients are released quickly, with high bioavailability, and can quickly and accurately exert their functionality; they are accurately measured, portable, and easy to use, and consumers have a high degree of acceptance. With the advancement of science and technology and the accelerated pace of people's lives, oral fast-dissolving films have gradually become a hot topic of research with their unique advantages.

[0004] At present, researchers have gradually deepened their exploration of oral fast-dissolving films. The country has focused on the application of natural and synthetic polymers, such as the selection and optimization of film-forming materials such as pregelatinized starch and hydroxypropyl methylcellulose. New structural materials such as nanofiber membranes have also been introduced into the preparation of oral fast-dissolving films. The regulation of loading efficiency and release kinetics for different drugs is also a hot topic of research, which includes the study of the interaction between drugs and film-forming materials, as well as the regulation of loading efficiency and release kinetics for different drugs. Foreign scholars have used a variety of analytical methods such as scanning electron microscopy, differential scanning calorimetry and X-ray diffraction analysis to focus on the effects of different environmental factors on the performance of fast-dissolving films. International research on oral fast-dissolving films covers the optimization of preparation processes and performance analysis, and also explores in depth its application potential in the actual medical and health field.

[0005] Since 2000, many new film products have been developed at home and abroad: caffeine film, diphenhydramine hydrochloride film, glipizide oral adhesive film, metoclopramide rapid release film, dexamethasone oral fast dissolving film and prochlorperazine oral disintegrating film, etc. These research works provide valuable scientific basis and technical support for the development of new oral fast dissolving film nutrient delivery system, indicating the great application prospect of oral fast dissolving film in future health products.

[0006] Seabuckthorn fruit powder is a powdered product obtained by drying seabuckthorn pulp using vacuum freeze drying technology or spray drying. It retains the inherent aroma and taste of seabuckthorn fruit. When brewed and drunk, it has a slight smell and a slightly sour taste, which is not astringent or greasy, but is sweet and sour and very appetizing. Its raw material, seabuckthorn (Hippophae rhamnoides L.), is a dried mature fruit of the seabuckthorn plant of the Elaeagnaceae family. my country was the first to study its medical value, and recorded its many effects such as benefiting the lungs, removing phlegm, and treating wind-heat. For example, seabuckthorn is recorded in many medical classics such as "Jingzhu Benzhang" and "Sibu Yidian". Seabuckthorn is one of the varieties that can be used as both medicine and food. In addition to medicinal use, it can also be used as a natural vitamin, especially seabuckthorn fruit is rich in vitamin C, so it is called the "king of vitamin C". However, the traditional way of taking seabuckthorn fruit powder has limitations such as inferior flavor, poor taste, inconvenient storage, low utilization rate and poor solubility. Therefore, it is necessary to explore a simple, healthy and new type of seabuckthorn fruit powder functional food to meet the ever-changing needs of the current market and consumers. Summary of the invention

[0007] The purpose of the present invention is to provide a sea buckthorn fruit powder oral instant film and a preparation method thereof. Based on the unique physicochemical properties and rich bioactive ingredients of the sea buckthorn fruit powder, the sea buckthorn fruit powder can play an excellent role as a drug carrier in the oral instant film, meet the market demand for efficient and convenient oral drug delivery, and has the advantages of easy storage, transportation and use.

[0008] The method for preparing the seabuckthorn fruit powder oral instant film provided by the present invention comprises the following steps:

[0009] Prepare a dispersion of potato pregelatinized starch, add seabuckthorn fruit powder and sorbitol after dispersion, and continue to disperse the film-forming liquid; pour the film-forming liquid into a culture dish and dry it to obtain the film-forming liquid.

[0010] Preferably, in the dispersion, the mass concentration of the pregelatinized potato starch is 1-4% (w / v, g / mL).

[0011] Preferably, the added amount of the seabuckthorn fruit powder is 10-20% of the mass of the pregelatinized potato starch.

[0012] Preferably, the added amount of the sorbitol is 25-35% of the mass of the pregelatinized potato starch.

[0013] Preferably, the dispersion time of the dispersion liquid is 20 to 40 minutes.

[0014] Preferably, the drying temperature is 30-40°C.

[0015] More preferably, the amount of seabuckthorn fruit powder added is 15% of the mass of the potato pregelatinized starch, the amount of sorbitol added is 30% of the mass of the potato pregelatinized starch, the dispersion time of the dispersion is 32 minutes, and the drying temperature is 36°C.

[0016] The present invention investigates the effects of drying temperature, increasing the amount of seabuckthorn fruit powder, increasing the amount of sorbitol, the dispersion temperature of starch, the dispersion time of starch, and the temperature of heating after adding seabuckthorn fruit powder and sorbitol on the sensory evaluation of the seabuckthorn fruit powder oral instant film. After detailed experimental analysis and statistical processing, it is found that the amount of seabuckthorn fruit powder added, the amount of sorbitol added, the starch dispersion time and the drying temperature have a significant effect on the sensory evaluation of the instant film. Therefore, the present invention selects these four factors to carry out the response surface experiment.

[0017] On the basis of the single factor experiment, the present invention adopts the response surface experiment to further optimize the process formula of preparing the sea buckthorn fruit powder oral instant film, and determines the optimal process conditions for preparing the sea buckthorn fruit powder instant film: adding 15% (w / w) sea buckthorn fruit powder, adding 30% (w / w) sorbitol, starch dispersion time of 32min, and drying temperature of 36°C. Under this formula, the prepared sea buckthorn fruit powder oral instant film has a complete appearance, a smooth surface, a proper sea buckthorn fruit flavor, melts in the mouth, and has a proper sweet and sour taste. The sensory score of the optimized instant film is 83.97±0.32 points, the thickness is 0.0493±0.0015mm, the disintegration time is 6.53±0.06s, the moisture content is 8.443±0.073%, and the scavenging ability of free radicals is 54.21±0.94%. The experimental results verify the accuracy of the Box-Behnken design response surface experiment prediction, and the fitting model is significantly higher than the experimental model, indicating that the prediction results are more accurate. The experiment showed that the sea buckthorn fruit powder oral fast-dissolving film had good reproducibility under the predicted conditions, and the deviation from the predicted results was small. Therefore, it can be considered that the Box-Behnken design response surface experiment prediction conditions are suitable for optimizing the sea buckthorn fruit powder oral fast-dissolving film formula. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the process of the present invention.

[0019] Figure 2 It is the sensory evaluation radar chart (left) and the average sensory total score chart (right) of the oral instant dissolving films with different drying temperatures.

[0020] Figure 3It is the sensory evaluation radar chart (left) and the average sensory total score chart (right) of the oral instant dissolving film with different addition amounts of sea buckthorn fruit powder.

[0021] Figure 4 The sensory evaluation radar chart (left) and the average sensory total score chart (right) of the oral instant dissolving films with different sorbitol addition amounts.

[0022] Figure 5 It is the sensory evaluation radar chart (left) and the average sensory total score chart (right) of the oral instant dissolving films with different starch dispersion temperatures.

[0023] Figure 6 It is the sensory evaluation radar chart (left) and the average sensory total score chart (right) of the oral instant dissolving film with different starch dispersion time.

[0024] Figure 7 It is the sensory evaluation radar chart (left) and the average value chart of the total sensory score (right) of the oral instant dissolving film at different heating temperatures after the addition of additives.

[0025] Figure 8 The contour lines (left) and response surface diagram (right) of the amount of sea buckthorn fruit powder added (A) and sorbitol added (B).

[0026] Fig. 9 The figures are the contour lines (left) and response surface diagram (right) of sea buckthorn fruit powder addition amount (A) and starch dispersion time (C).

[0027] Fig.10 The figure below shows the contour lines (left) and response surface diagram (right) of sea buckthorn fruit powder addition amount (A) and drying temperature (D).

[0028] Fig.11 The contour lines (left) and response surface diagram (right) of sorbitol addition amount (B) and starch dispersion time (C) are shown.

[0029] Fig.12 The contour lines (left) and response surface diagram (right) of sorbitol addition amount (B) and drying temperature (D) are shown.

[0030] Fig.13 The starch dispersion temperature (C) and drying temperature (D) contour lines (left) and response surface diagram (right). DETAILED DESCRIPTION

[0031] The method of sensory evaluation in the following examples is as follows:

[0032] The sensory evaluation of the seabuckthorn fruit powder oral instant film was conducted by 10 trained personnel, who designed a sensory evaluation table to conduct sensory evaluation on the seabuckthorn fruit powder oral instant film in terms of appearance, taste, flavor, mouthfeel, and disintegration time. The specific scoring criteria are shown in Table 1.

[0033] Table 1 Sensory scoring standard for seabuckthorn fruit powder oral instant film

[0034]

[0035] The thickness of the seabuckthorn fruit powder oral instant film in the following examples is determined as follows:

[0036] The thickness of the sea buckthorn fruit powder oral instant film is measured with a digital micrometer to ensure the quality and standard of the product. During the measurement process, 10 locations are randomly selected from each film, and the thickness of each location is measured separately. At least 3 sets of parallel experiments are tested for each sample to ensure the accuracy and reliability of the measurement results. The measurement data needs to be recorded and analyzed in detail to provide reference and guidance for subsequent production and quality control.

[0037] The method for determining the disintegration time of the seabuckthorn fruit powder oral fast-dissolving film in the following examples is as follows:

[0038] Refer to the test method of Garcia et al.: The instant dissolving film is fixed between two square glass sheets with a square (2×2 cm) hole in the middle and placed in a culture dish. 300 μL of distilled water at room temperature (37°C) is dropped on the surface of the instant dissolving film exposed to the square hole. When the distilled water passes through the instant dissolving film, the moment when the edge touches the culture dish is recorded as the disintegration time of the instant dissolving film.

[0039] The method for determining the moisture content of the seabuckthorn fruit powder oral instant film in the following examples is as follows:

[0040] The method of Homez-Jara et al. was referred to and partially modified. The finished film of the same size and weight (W0) was used, and the sample was dried in an electric hot air drying oven at 100°C for 12 hours, and then its weight was re-weighed (W1). Three sets of parallel experiments were performed for each formula. The water content of the finished film was calculated as follows:

[0041] Moisture content (%) = (W0-W1) / W0×100

[0042] The method for determining the antioxidant properties of the seabuckthorn fruit powder oral instant film in the following examples is as follows: The DPPH method can be used to evaluate the removal effect of the instant film on DPPH free radicals:

[0043] (1) Preparation of sample solution

[0044] The instant dissolving film was stored in a vacuum drying oven at a temperature of 40° C. and a relative humidity of 75%. Before the experiment, 0.1 g of the instant dissolving film was dissolved in 12.5 mL of distilled water to prepare a sample solution.

[0045] (2) Preparation of DPPH working solution

[0046] Weigh 0.0039 g DPPH and prepare it into 0.2 mM DPPH working solution with anhydrous ethanol. Take 25 mL DPPH working solution in a 50 mL volumetric flask and dilute it to the mark with anhydrous ethanol to dilute it 2 times. Keep the whole process away from light and use the solution immediately after preparation.

[0047] (3)Measure absorbance

[0048] Mix 2400 μL of DPPH working solution with 150 μL of instant membrane solution and 450 μL of distilled water. After standing for 1 hour, measure the absorbance of the sample solution at 517 μm. Repeat all experiments 3 times. The total antioxidant capacity is calculated as follows.

[0049] Total antioxidant capacity (%) = [A0-(A1-A2)] / A0

[0050] Where: A0—absorbance of DPPH working solution and distilled water at 517nm;

[0051] A1—Absorbance of sample solution, DPPH working solution and distilled water at 517nm;

[0052] A2—Absorbance of sample solution and distilled water at 517nm.

[0053] Example 1, single factor experiment

[0054] (1) Effect of drying temperature on sensory evaluation of seabuckthorn fruit powder oral instant film

[0055] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / vg / mL) starch dispersion, and stir at 60°C for 20 minutes with a constant temperature magnetic stirrer. After the starch is evenly dispersed, add 20% sea buckthorn fruit powder (w / w, based on the mass of starch) and 30% sorbitol (w / w, based on the mass of starch) to the conical flask. Continue to use a constant temperature magnetic stirrer to disperse the film liquid, and set the dispersion temperature to 60°C. After 6 minutes, pour the film-forming liquid into a culture dish and put it into an electric blast drying oven. The drying temperatures are set to 25°C, 30°C, 35°C, 40°C, 45°C, and 50°C, respectively. After the oral instant film is prepared, it is necessary to perform a balancing treatment of the sea buckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and a relative humidity of 50%, and lasts for 3 to 5 days.

[0056] Effect of drying temperature on sensory evaluation of seabuckthorn fruit powder oral instant film Figure 2As shown. According to the results on the left, the drying temperature has a significant effect on the appearance and taste of the instant film, and also has a certain effect on the taste and disintegration time, while the effect on the flavor is not obvious. As shown in the right figure, with the increase of the drying temperature, the sensory score shows a trend of first rising and then falling. When the temperature reaches 35°C, the instant film has a complete appearance, a smooth surface, a smooth and fresh taste, and a refreshing taste. At this time, the sensory score reaches the highest point. When the drying temperature is higher than 35°C, the higher the temperature, the faster the film-forming liquid evaporates, causing the film-forming polymer to be fixed prematurely, resulting in an incomplete surface of the instant film, fine cracks, a large number of tiny holes and protruding particles, affecting the sensory score of the film; when the drying temperature is lower than 35°C, the lower the temperature, the slower the movement of the polymer molecules, and the difficulty of cross-linking, which is not conducive to the formation of a regular network dense structure, nor is it conducive to the full expansion of the polymer molecules. Therefore, in the process of producing instant films, in order to ensure the stability and durability of the instant film matrix, the drying temperature conditions in the production process should be strictly controlled according to the different models and specifications of the film matrix. Therefore, a drying temperature of 35°C was selected for the next experiment.

[0057] (2) Effect of seabuckthorn fruit powder addition amount on sensory evaluation of seabuckthorn fruit powder oral instant film

[0058] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / v) starch dispersion, and stir at 60°C for 20 minutes with a constant temperature magnetic stirrer. After the starch is evenly dispersed, add 25% (w / w, based on the mass of starch) of sorbitol to the conical flask, and add sea buckthorn fruit powder to the film liquid at a ratio of 10%, 15%, 20%, 25%, 30%, and 35% (w / w, based on the mass of starch). Continue to use a constant temperature magnetic stirrer to disperse the film liquid, set the dispersion temperature to 60°C, pour the film-forming liquid into a culture dish after 6 minutes, put it into an electric blast drying oven, and set the drying temperature to 35°C. After the oral instant film is prepared, it is necessary to perform a balancing treatment of the sea buckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and a relative humidity of 50%, and lasts for 3 to 5 days.

[0059] Effect of the amount of seabuckthorn fruit powder added on the sensory evaluation of seabuckthorn fruit powder oral instant film Figure 3As shown. As can be seen from the left figure, the amount of sea buckthorn fruit powder added has a great influence on the taste and flavor of the instant film, has a certain effect on the taste, and has little effect on its appearance and disintegration time. The right figure shows that the sensory score shows a trend of first suppressing and then rising with the increase of the amount of sea buckthorn fruit powder added. When 15% sea buckthorn fruit powder is added to the instant film, the instant film has a sweet and appropriate sea buckthorn fruit flavor, with appropriate sourness and sweetness, melts in the mouth, and is refreshing. At this time, the sensory score is the highest. Sea buckthorn fruit has a unique fruity aroma and flavor and can be used as a food sweetener. Adding different amounts of sea buckthorn fruit powder will affect the taste and flavor of the instant film. Too low will lose the flavor, and too high will affect the taste because of the sweetness. Therefore, 15% of sea buckthorn fruit powder was selected for the next experiment.

[0060] (3) Effect of sorbitol addition on sensory evaluation of seabuckthorn fruit powder oral fast-dissolving film

[0061] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / v) starch dispersion, and stir at 60°C for 20 minutes with a constant temperature magnetic stirrer. After the starch is evenly dispersed, add 15% (w / w, based on the mass of starch) seabuckthorn fruit powder to the conical flask, and add sorbitol to the film solution at a ratio of 10%, 15%, 20%, 25%, 30%, and 35% (w / w, based on the mass of starch). Continue to use a constant temperature magnetic stirrer to disperse the film solution, set the dispersion temperature to 60°C, pour the film-forming solution into a culture dish after 6 minutes, put it into an electric blast drying oven, and set the drying temperature to 35°C. After the oral instant film is prepared, it is necessary to balance the seabuckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and a relative humidity of 50%, and lasts for 3 to 5 days.

[0062] Effects of different amounts of sorbitol on sensory evaluation of seabuckthorn fruit powder oral instant film Figure 4 As shown. From the left figure, whether it is taste, mouthfeel or disintegration time, the amount of sorbitol added has a great impact on it, but has little effect on its appearance and flavor. The right figure shows that as the amount of sorbitol gradually increases, the sensory score shows a state of first depression and then rise. The instant film melts in the mouth, is refreshing, and has appropriate sweetness and sourness. When the disintegration time is the shortest and the sensory score is the highest, the sorbitol addition amount is 30%. Sorbitol is both a sweetener and a plasticizer. The stronger water absorption capacity is due to the gradual increase in sorbitol, and the content of hydrophilic groups in the instant film matrix is ​​also increasing. At the same time, the mobility of the starch chain is accelerated, and the diffusion rate of water molecules in the film matrix is ​​increased, which accelerates the disintegration of the instant film and can achieve the effect of melting in the mouth. However, if sorbitol continues to be added, the overall density of the film matrix will increase, the pores will decrease, the diffusion of water molecules in the film matrix will be inhibited, and the disintegration time of the instant film will be prolonged, resulting in a worse taste and an overly sweet taste. Therefore, the next experiment uses a 30% sorbitol addition amount.

[0063] (4) Effect of starch dispersion temperature on sensory evaluation of seabuckthorn fruit powder oral instant film

[0064] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / v) starch dispersion, stir with a constant temperature magnetic stirrer for 20 minutes, and set the dispersion temperature to 40°C, 50°C, 60°C, 70°C, and 80°C. After the starch is evenly dispersed, add 15% (w / w, based on the mass of starch) sea buckthorn fruit powder and 30% (w / w, based on the mass of starch) sorbitol to the conical flask. Continue to use a constant temperature magnetic stirrer to disperse the film liquid, set the dispersion temperature to 60°C, pour the film-forming liquid into a culture dish after 6 minutes, put it into an electric blast drying oven, and set the drying temperature to 35°C. After the oral instant film is prepared, it is necessary to balance the sea buckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and relative humidity of 50%, and last for 3 to 5 days.

[0065] Figure 5 The figure shows the sensory evaluation results of the sea buckthorn fruit powder oral instant film affected by the starch dispersion temperature. As can be seen from the left figure, the starch dispersion temperature has a certain influence on the taste and flavor of the instant film, but has little effect on other factors. The right figure shows that as the starch dispersion temperature increases, the sensory score shows a trend of first depression and then rise, but the trend is small and not significant. The highest sensory score is the instant film when the starch dispersion temperature is 50°C. Considering that it is more advantageous to add active ingredients with unstable physical and chemical properties at a lower temperature, as well as saving costs, the next experiment uses a starch dispersion temperature of 50°C.

[0066] (5) Effect of starch dispersion time on sensory evaluation of seabuckthorn fruit powder oral instant film

[0067] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / v) starch dispersion. Stir with a constant temperature magnetic stirrer at 50°C, and set the stirring time to 10min, 20min, 30min, 40min, and 50min respectively. After the starch is evenly dispersed, add 15% (w / w, based on the mass of starch) sea buckthorn fruit powder and 30% (w / w, based on the mass of starch) sorbitol to the conical flask. Continue to use a constant temperature magnetic stirrer to disperse the film liquid, set the dispersion temperature to 60°C, and after 6 minutes, pour the film-forming liquid into a culture dish and put it into an electric blast drying oven, and set the drying temperature to 35°C. After the oral instant film is prepared, it is necessary to perform a balancing treatment of the sea buckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and a relative humidity of 50%, and lasts for 3 to 5 days.

[0068] Figure 6The results of sensory evaluation of the sea buckthorn fruit powder oral instant film are shown in the figure below, which is affected by the starch dispersion time. As can be seen from the left figure, the starch dispersion time has a great influence on the appearance and disintegration time of the instant film, and has a certain influence on the taste, flavor and mouthfeel, but the influence is not significant. The right figure shows that the sensory score shows a trend of first depression and then rise with the increase of the starch dispersion time. When the starch dispersion time is 30 minutes, the instant film has a complete appearance, a smooth surface, and a very fast disintegration rate, and the sensory score is the highest. When the starch dispersion time exceeds 30 minutes and continues to increase, the starch chain cross-linking is more sufficient, the film matrix forms a more complete network structure, the integrity of the film structure is improved, and the disintegration time of the instant film will increase significantly. When the starch dispersion time is less than 30 minutes and continues to decrease, the starch chain cross-linking is insufficient, the starch is prone to aggregation, the film structure becomes unstable, and the disintegration time of the instant film will be significantly shortened. In order to obtain better film-forming effect and stability, the next experiment should be carried out under the condition of a starch dispersion time of 30 minutes.

[0069] (6) Effect of heating temperature after adding seabuckthorn fruit powder and D-sorbitol on sensory evaluation of seabuckthorn fruit powder oral instant film

[0070] Pour a certain amount of potato pregelatinized starch into a conical flask, add distilled water to make a 2% (w / v) starch dispersion, and stir at 50°C for 30 minutes with a constant temperature magnetic stirrer. After the starch is evenly dispersed, add 15% (w / w, based on the mass of starch) sea buckthorn fruit powder and 30% (w / w, based on the mass of starch) sorbitol to the conical flask. Continue to disperse the film liquid with a constant temperature magnetic stirrer, and set the dispersion temperature to 30°C, 40°C, 50°C, 60°C, and 70°C respectively. After 6 minutes, pour the film-forming liquid into a culture dish and put it into an electric blast drying oven, and set the drying temperature to 35°C. After the oral instant film is prepared, it is necessary to balance the sea buckthorn fruit powder oral instant film. This process needs to be carried out at room temperature (23±2°C) and relative humidity of 50%, and last for 3 to 5 days.

[0071] Figure 7The figure shows the sensory evaluation results of the sea buckthorn fruit powder oral instant film affected by the heating temperature after adding sea buckthorn fruit powder and sorbitol. As can be seen from the left figure, the heating temperature after adding sea buckthorn fruit powder and sorbitol has a certain effect on the appearance and taste of the instant film, but has little effect on its taste, disintegration time and flavor. The right figure shows that with the continuous increase in temperature after the addition of sea buckthorn fruit powder and sorbitol, the sensory score shows a trend of first rising and then falling. When the heating temperature after adding sea buckthorn fruit powder and sorbitol is 50℃, the instant film has a complete appearance, a smooth surface, melts in the mouth, and is refreshing. At this time, the sensory score is the highest. As the temperature rises, the thermal motion of sea buckthorn fruit powder molecules and sorbitol molecules will be enhanced, which will promote the dispersion of sea buckthorn fruit powder and sorbitol molecules in the film matrix, which is conducive to the formation of a network structure of the film matrix, making it complete in appearance and smooth on the surface, thereby causing the strength of the instant film to increase. Therefore, the next experiment was carried out at a heating temperature of 50℃ after the addition of sea buckthorn fruit powder and sorbitol.

[0072] Example 2, response surface experiment

[0073] The preparation process of sea buckthorn fruit powder oral instant film was further optimized on the basis of single factor experiment. According to the Box-Behnken experimental design principle, Design Expert 13 software was used to design the experiment with sensory evaluation as the response value, including the amount of sea buckthorn fruit powder added, the amount of sorbitol used, the dispersion time of starch and the drying temperature, and 4 factors and 3 levels, to determine the optimal process parameters and prepare sea buckthorn fruit powder oral instant film with better sensory and performance.

[0074] 1. Response surface experiment

[0075] On the basis of the single factor experiment, the amount of seabuckthorn fruit powder added (A), the amount of sorbitol added (B), the dispersion time of starch (C) and the drying temperature (D) were selected as the four factors of the response surface experiment, and the sensory score (Y) was used as the evaluation index. The factor level table is shown in Table 2, and the scheme and results are shown in Table 3.

[0076] Table 2 Factor levels of response surface experiment

[0077]

[0078] Table 3 Scheme and results of response surface experiment

[0079]

[0080]

[0081]

[0082] 2. Regression model fitting and variance analysis

[0083] Design-Expert 13.0 was used to perform response surface analysis on the results in Table 4, and the quadratic multinomial regression equation of the sensory score (Y) of the seabuckthorn fruit powder oral instant film on the addition amount of seabuckthorn fruit powder (A), the addition amount of sorbitol (B), the dispersion time of starch (C), and the drying temperature (D) was obtained:

[0084] Y=+83.78-0.0583A-0.175B+0.6333C+0.1667D+0.05AB-0.15AC+0.625AD-0.3BC-0.425BD+0.4CD-1.79A2-1.81B2-1.1C2-1.3D2

[0085] It can be concluded from Table 4 that in the quadratic multinomial regression equation model with the sensory score of seabuckthorn fruit powder oral instant film as the response value, P < 0.0001 indicates that the predictive power of the model is extremely significant; the lack of fit term P = 0.5617 > 0.05, indicating that the difference in the lack of fit term is not significant; the correlation coefficient R 2 =0.9816, Corrected determination coefficient R 2 Adj =0.9633, and the coefficient of variation CV value is 0.3151%. These values ​​indicate that the model has a high degree of fit and a high degree of credibility, indicating that the model has a good reflection of the relationship between the factors of seabuckthorn fruit powder addition amount, sorbitol addition amount, starch dispersion time and drying temperature, and the model can well describe the influence of the formula of seabuckthorn fruit powder oral instant film on the total sensory score. From the F value in Table 4, it can be seen that the influence of the four factors on the sensory score of seabuckthorn fruit powder oral instant film is: C starch dispersion time > B sorbitol addition amount > D drying temperature > A seabuckthorn fruit powder additives.

[0086] Table 4 Variance analysis table of regression model coefficients

[0087]

[0088] Note: P<0.01, extremely significant difference (**); P<0.05, significant difference (*)

[0089] 3. Analysis of interaction of various factors on response surface

[0090] Based on the regression model designed by Design-Expert 13 software, the interaction of four factors, A (amount of seabuckthorn fruit powder added), B (amount of sorbitol added), C (dispersion time of starch) and D (drying temperature), was used to generate contour maps and response surface plots in order to analyze the influence of the interaction between different single factors in the sensory evaluation of seabuckthorn fruit powder oral instant film. Figures 8 to 13The contour plots and response surface plots are AB, AC, AD, BC, BD, and CD. These plots provide an in-depth analysis of the significant interactions between factors on sensory scores.

[0091] (1) Figure 8 When C (starch dispersion time) is 31.6224 min and D (drying temperature) is 35.6366 ° C, A (sea buckthorn fruit powder addition) and B (sorbitol addition) have an interactive effect on sensory evaluation. The contour map of A (sea buckthorn fruit powder addition) and B (sorbitol addition) is close to a circle, and the slope of the response surface is steep, indicating that the interaction between the two factors of sea buckthorn fruit powder addition and sorbitol addition has a certain effect on the sensory score of the response value, but the effect is not significant.

[0092] (2) Fig. 9 When B (sorbitol addition) is 29.5466% and D (drying temperature) is 35.6366℃, A (sea buckthorn fruit powder addition) and C (starch dispersion time) have an interactive effect on sensory evaluation. The contour lines of A (sea buckthorn fruit powder addition) and C (starch dispersion time) are close to ellipse, but the response surface curve is relatively flat, indicating that there is an interaction between the two factors of sea buckthorn fruit powder addition and starch dispersion time, but it is not significant.

[0093] (3) Fig.10 When B (sorbitol addition) is 29.5466% and C (starch dispersion time) is 31.6224min, A (sea buckthorn fruit powder addition) and D (drying temperature) have an interactive effect on sensory evaluation. The contour lines of A (sea buckthorn fruit powder addition) and D (drying temperature) are close to ellipse, and the slope of the response surface curve is steep, indicating that there is an extremely significant interaction between the two factors of sea buckthorn fruit powder addition and drying temperature.

[0094] (4) Fig.11 When A (the amount of seabuckthorn fruit powder added) is 14.9567% and D (the drying temperature) is 35.6366°C, B (the amount of sorbitol added) and C (the dispersion time of starch) have an interactive effect on sensory evaluation. The contour lines of B (the amount of sorbitol added) and C (the dispersion time of starch) are close to ellipses, and the slope of the response surface curve is slightly steep, indicating that there is a significant interaction between the amount of sorbitol added and the dispersion time of starch.

[0095] (5) Fig.12When A (sea buckthorn fruit powder addition) is 14.9567% and C (starch dispersion time) is 31.6224min, B (sorbitol addition) and D (drying temperature) have an interactive effect on sensory evaluation. The contour lines of B (sorbitol addition) and D (drying temperature) are close to ellipses, and the slope of the response surface curve is steep, indicating that the interaction between sorbitol addition and drying temperature has a significant effect on sensory evaluation.

[0096] (6) Fig.13 When A (sea buckthorn fruit powder addition) is 14.9567% and B (sorbitol addition) is 29.5466%, C (starch dispersion time) and D (drying temperature) have an interactive effect on sensory evaluation. The contour lines of C (starch dispersion time) and D (drying temperature) are close to ellipses, and the slope of the response surface curve is steep, indicating that the interaction between the two factors of starch dispersion time and drying temperature has a significant effect on sensory evaluation.

[0097] 4. Verification test and results

[0098] According to the analysis of Design-Expert 13 software, the best process formula of sea buckthorn fruit powder oral instant film was obtained: 14.96% (w / w) sea buckthorn fruit powder, 29.55% (w / w) sorbitol, 31.62min starch dispersion time, and 35.64℃ drying temperature. Combined with the actual production situation, the drying temperature was set to an integer, and the optimal process formula was fine-tuned in combination with the convenience of experimental operation. Therefore, the formula after a series of corrections was: the addition amount of sea buckthorn fruit powder was 15% (w / w), the addition amount of sorbitol was 30% (w / w), the drying temperature was 36℃, and the starch dispersion time was 32min. The sensory score of the sea buckthorn fruit powder oral instant film after optimization reached 83.90±0.32 points. Three batches of sea buckthorn fruit powder oral instant film were prepared according to the formula, and the sensory evaluation was carried out respectively, and the water content, antioxidant activity, disintegration time and thickness were measured. According to the model prediction, the predicted value and actual value of the optimized best process formula are shown in Table 5. The final result shows that the actual value of the sensory score is 83.97±0.32 points, which is very close to the predicted value of the model, proving that the regression model has good predictive power. The optimization of the sea buckthorn fruit powder oral instant film formula by response surface methodology is stable and feasible, and has certain guiding significance.

[0099] Table 5 Predicted values ​​of the best process formula and actual values ​​of the optimized formula

[0100] Test No. Sensory score / points Thickness / mm Disintegration time / s Moisture content / % Antioxidant / % 1 83.60 0.0480 6.46 8.375 53.10 2 84.10 0.0490 6.55 8.521 55.43 3 84.20 0.0510 6.58 8.433 54.10 average value 83.97±0.32 0.0493±0.0015 6.53±0.06 8.443±0.073 54.21±0.94 Predicted value 83.90

[0101] On the basis of the single factor experiment, the present invention adopts the response surface experiment to further optimize the process formula for preparing the sea buckthorn fruit powder oral instant film, and determines the optimal process conditions for preparing the sea buckthorn fruit powder instant film: adding 15% (w / w) sea buckthorn fruit powder, adding 30% (w / w) sorbitol, the starch dispersion time is 32min, and the drying temperature is 36°C. Under this formula, the prepared sea buckthorn fruit powder oral instant film has a complete appearance, a smooth surface, an appropriate sea buckthorn fruit flavor, melts in the mouth, and has an appropriate sweet and sour taste. The experimental results verify the accuracy of the Box-Behnken design response surface experiment prediction, and the fitting model is significantly higher than the experimental model, indicating that the prediction results are more accurate. The experiment shows that the sea buckthorn fruit powder oral instant film has good reproducibility under the predicted conditions, and the deviation from the predicted results is small. Therefore, it is believed that the Box-Behnken design response surface experiment prediction conditions are suitable for optimizing the sea buckthorn fruit powder oral instant film formula.

Claims

1. A method for preparing a seabuckthorn fruit powder oral instant film, comprising the following steps: Prepare a dispersion of potato pregelatinized starch, add seabuckthorn fruit powder and sorbitol after dispersion, and continue to disperse the film-forming liquid; pour the film-forming liquid into a culture dish and dry it to obtain the film-forming liquid.

2. The preparation method according to claim 1, characterized in that: In the dispersion, the mass concentration of the potato pregelatinized starch is 1-4% (w / v).

3. The preparation method according to claim 1 or 2, characterized in that: The added amount of the seabuckthorn fruit powder is 10-20% of the mass of the potato pregelatinized starch.

4. The preparation method according to any one of claims 1 to 3, characterized in that: The added amount of the sorbitol is 25-35% of the mass of the pregelatinized potato starch.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The dispersion time of the dispersion liquid is 20 to 40 minutes.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The drying temperature is 30-40°C.

7. The preparation method according to any one of claims 1 to 6, characterized in that: The amount of seabuckthorn fruit powder added is 15% of the mass of the pregelatinized potato starch, the amount of sorbitol added is 30% of the mass of the pregelatinized potato starch, the dispersion time of the dispersion is 32 minutes, and the drying temperature is 36°C.

8. An orally-dissolving seabuckthorn fruit powder film prepared by the method according to any one of claims 1 to 7.

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