Eucommia ulmoides leaf instant solid beverage with homology of medicine and food and preparation process thereof

Abstract

The invention belongs to the technical field of food, and relates to a medicinal and edible eucommia ulmoides leaf instant solid beverage and a preparation method thereof. An active ingredient in the solid beverage is a folium cortex eucommiae extract, a supercritical CO2 extraction technology is adopted, and ultrasonic-microwave-assisted extraction is combined, so that the extraction efficiency and the extraction amount of the active ingredient are effectively improved; the folium cortex eucommiae active ingredient microcapsule particles are obtained by mixing the active ingredients with stevioside, then carrying out inclusion with hydroxypropyl-beta-cyclodextrin, then carrying out embedding with carboxymethylated Arabic gum and carrying out spray drying, the double-layer microcapsule structure synergistically improves the instant solubility and covers the bitterness, and the brewed beverage is clear and uniform, does not need to be stirred for a long time, and has the advantages of simple preparation process, low cost and the like. The method adapts to fast-paced life scenes, and meanwhile, oxidative degradation of active ingredients in the storage and transportation process is avoided; sucrose fatty acid ester, glyceryl monostearate, L-ascorbic acid, sodium citrate, citric acid and glucose syrup powder are used as auxiliary materials, so that the medicinal and edible eucommia ulmoides leaf instant solid beverage is obtained, the taste of the beverage is coordinated, and the palatability is improved.

Description

Technical Field

[0001] This invention relates to the field of food technology, and in particular to an instant solid beverage made from Eucommia ulmoides leaves that is both food and medicine, and its preparation process. Background Technology

[0002] The earliest concept of medicine and food sharing the same origin was proposed in the classic Chinese medicine text, "The Five Grains nourish, the Five Fruits assist, the Five Animals benefit, and the Five Vegetables replenish. When their flavors are combined and consumed, they can replenish essence and boost qi." This clearly indicates that food can not only satisfy hunger but also regulate the body and prevent disease.

[0003] Over a long period of time, ancient people had developed rudimentary techniques for transforming food into medicine. For example, they altered the physicochemical properties of ingredients through processing, such as stir-frying Eucommia ulmoides to enhance its kidney-tonifying effects and steaming yam to reduce its cold nature. They also extracted active ingredients through extraction, such as decocting herbs and soaking them in medicinal wine. Alternatively, they improved the convenience of consumption by shaping the ingredients, such as making medicinal pills and pastes.

[0004] With rising health awareness among residents, upgraded consumption patterns, and the transformation of the food industry, the traditional model of food and medicine sharing the same origin can no longer meet the demands, thus driving the development of technology towards higher efficiency, precision, safety, and convenience. In today's fast-paced lifestyle, consumers find it difficult to spend time preparing medicinal cuisine, leading to a surge in demand for ready-to-eat, portable, and easy-to-store food and medicine sharing the same origin products, such as instant powders, compressed candies, and meal replacement powders. This places high demands on the stability and palatability of active ingredients.

[0005] Chinese patent application CN109730225A discloses a compound liver-protecting solid beverage made from Eucommia ulmoides leaves and its preparation method. Its active ingredients include Eucommia ulmoides leaf extract powder, milk thistle instant powder, mulberry instant powder, maitake mushroom instant powder, and wolfberry instant powder, etc., with the addition of other adjuvants, to prepare a compound liver-protecting solid beverage made from Eucommia ulmoides leaves with health benefits such as liver protection, heat clearing and detoxification, and prevention of acute and chronic hepatitis and cirrhosis. The aforementioned technical solutions have significant flaws. In the formula, silymarin, the active ingredient of milk thistle, has extremely poor water solubility. Even with instant powder, it requires a large amount of co-solvents such as polyethylene glycol and propylene glycol to dissolve. However, the solution does not add a dedicated co-solvent, which may cause the milk thistle instant powder to separate or precipitate during actual preparation, affecting the taste. Furthermore, Eucommia ulmoides leaf extract powder has a distinctly bitter taste. The solution only adjusts sweetness and acidity with xylitol and citric acid, without adding flavor masking agents. The bitterness of the final product will severely impact palatability, failing to meet the core requirements of easy acceptance and good taste in solid beverages, resulting in low market acceptance. In addition, the addition of additives such as sodium carboxymethyl cellulose, xanthan gum, gellan gum, and sodium hexametaphosphate is problematic. Sodium carboxymethyl cellulose and xanthan gum are both high-viscosity thickeners; their combination will make the product excessively viscous after preparation. Gellan gum has extremely high gel strength, and when combined with sodium carboxymethyl cellulose and xanthan gum, it easily forms lumpy gels at low temperatures, severely affecting the drinking experience. Summary of the Invention

[0006] This invention aims to provide an instant solid beverage made from Eucommia ulmoides leaves, a material used in both medicine and food, and its preparation process. The active ingredient in this solid beverage is Eucommia ulmoides leaf extract, which is mixed with steviol glycosides and encapsulated in microcapsules. This process masks the bitterness of the Eucommia ulmoides leaf extract while ensuring that the active ingredient does not degrade during storage and processing, achieves instant dissolution upon reconstitution, and does not affect transparency.

[0007] To achieve the above objectives, in a first aspect, this application provides an instant solid beverage made from Eucommia ulmoides leaves, which are both food and medicine. This instant solid beverage comprises Eucommia ulmoides leaf active ingredient microcapsule particles, sucrose fatty acid esters, glyceryl monostearate, L-ascorbic acid, sodium citrate, citric acid, and glucose syrup powder. The Eucommia ulmoides leaf active ingredient microcapsule particles comprise Eucommia ulmoides leaf active ingredient extract, steviol glycosides, an inner wall material, and an outer wall material. The inner wall material is hydroxypropyl-β-cyclodextrin, and the outer wall material is carboxymethylated gum arabic and maltodextrin. The content of each component in the instant solid beverage is as follows: sucrose fatty acid ester 0.5%~1%, glyceryl monostearate 0.1%~0.2%, L-ascorbic acid 0.1%~0.3%, sodium citrate 0.5%~1%, citric acid 0.2%~0.8%, glucose syrup powder 40%~55%, and the remainder being Eucommia ulmoides leaf active ingredient microcapsule particles.

[0008] Preferably, the volume-to-mass ratio of Eucommia ulmoides leaf active ingredient extract, steviol glycoside, hydroxypropyl-β-cyclodextrin, carboxymethylated gum arabic, and maltodextrin in the Eucommia ulmoides leaf active ingredient microcapsule particles is 1L:(10~50)g:(300~500)g:100g:(200~300)g.

[0009] Secondly, this application also provides a method for preparing an instant solid beverage made from Eucommia ulmoides leaves, which are both food and medicine, comprising:

[0010] Step S1: After cleaning and drying, the Eucommia ulmoides leaves are crushed and sieved to obtain Eucommia ulmoides leaf powder. The Eucommia ulmoides leaf powder is placed in a supercritical CO2 extraction vessel for extraction. The powder is added to an ethanol aqueous solution and treated with microwave-ultrasound assisted to obtain an extract of active ingredients from Eucommia ulmoides leaves.

[0011] Step S2: Concentrate the extract of active ingredients from Eucommia ulmoides leaves under ultrasonic assistance, add steviol glycosides to obtain a concentrated extract of active ingredients from Eucommia ulmoides leaves, mix the concentrated extract of active ingredients from Eucommia ulmoides leaves with an aqueous solution of hydroxypropyl-β-cyclodextrin, stir to obtain a primary microsphere dispersion.

[0012] Step S3: Add a mixture of carboxymethylated gum arabic and maltodextrin to the primary microsphere dispersion, stir, concentrate, and cool to obtain a pre-concentrated solution;

[0013] Step S4: Set the parameters of the spray dryer, pump the pre-concentrated liquid into the atomizer, and obtain microcapsule particles of active ingredients of Eucommia ulmoides leaves through spray drying;

[0014] Step S5: Mix the microcapsule particles of active ingredients of Eucommia ulmoides leaf, sucrose fatty acid ester, glyceryl monostearate, L-ascorbic acid, sodium citrate, citric acid and glucose syrup powder to obtain a mixture. Granulate the mixture to obtain Eucommia ulmoides leaf instant beverage.

[0015] Preferably, in step S1, the mesh size of the sieve is 40-60 mesh.

[0016] Preferably, in step S1, the volume ratio of ethanol to water in the ethanol-water solution is 1:(10~20).

[0017] Preferably, in step S1, the mass-to-volume ratio of Eucommia ulmoides leaf powder to ethanol aqueous solution is 1g:(10~15)mL.

[0018] Preferably, in step S1, the specific parameters for the microwave-ultrasound assisted treatment include: microwave power of 300~500W, ultrasonic power of 100~200W, treatment temperature of 40~60℃, and treatment time of 15~30min.

[0019] Preferably, in step S1, the specific extraction process includes: loading Eucommia ulmoides leaf powder into an extraction vessel, with an extraction vessel pressure of 25~40MPa, an extraction temperature of 35~50℃, a CO2 flow rate of 10~20L / h, and an extraction time of 0.5~1h; the material is then placed into an analysis vessel, with an analysis vessel pressure of 5~10MPa, an analysis temperature of 40~60℃, and an analysis time of 20~30min.

[0020] Preferably, in step S2, the concentration temperature is 40~50℃.

[0021] Preferably, in step S2, the volume-to-mass ratio of the Eucommia ulmoides leaf active ingredient extract to steviol glycosides is 100 mL: (1~5) g.

[0022] Preferably, in step S2, the mass ratio of hydroxypropyl-β-cyclodextrin to water in the aqueous solution of hydroxypropyl-β-cyclodextrin is 1:(4~5).

[0023] Preferably, in step S2, the volume ratio of the concentrated active ingredient solution of Eucommia ulmoides leaves to the aqueous solution of hydroxypropyl-β-cyclodextrin is 1:(1~2).

[0024] Preferably, in step S2, the stirring temperature is 40~45℃ and the stirring time is 15~20min.

[0025] Preferably, in step S3, the volume ratio of the primary microsphere dispersion to the mixture is 1:(1~1.5).

[0026] Preferably, in step S3, the mass-to-volume ratio of carboxymethylated gum arabic, maltodextrin, and water in the mixture is 1 g: (2~3) g: (20~40) mL.

[0027] Preferably, in step S3, the stirring time is 20-30 minutes.

[0028] Preferably, in step S3, the concentration temperature is 50~60℃.

[0029] This invention also provides a method for preparing the carboxymethylated gum arabic described in step S3, comprising:

[0030] Step A1: Disperse gum arabic in isopropanol to obtain gum arabic dispersion, add sodium hydroxide aqueous solution to it, react to obtain gum arabic alkalization solution;

[0031] Step A2: Add chloroacetic acid solution to the gum arabic alkalization solution and react. After the reaction is complete, cool and add hydrochloric acid while stirring to adjust the pH to 6.5-7.0. Filter and collect the filtrate.

[0032] Step A3: Add the filtrate to anhydrous ethanol with stirring, let stand until the product precipitates, centrifuge, wash, dry, pulverize, and sieve to obtain carboxymethylated gum arabic powder.

[0033] Preferably, in step A1, the mass-to-volume ratio of gum arabic, isopropanol, and sodium hydroxide aqueous solution is 1g:(8~10)mL:(1.2~1.35)mL.

[0034] Preferably, in step A1, the mass-to-volume ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is (4~6) g: (10~15) mL.

[0035] Preferably, in step A1, the reaction temperature is 30~40℃ and the reaction time is 1~2h.

[0036] Preferably, in step A2, the solvent in the chloroacetic acid solution is isopropanol, and the mass-volume ratio of chloroacetic acid to solvent is (8~12) g: (20~30) mL.

[0037] Preferably, in step A2, the volume ratio of the gum arabic alkalization solution to the chloroacetic acid solution is 1:(0.25~0.32).

[0038] Preferably, in step A2, the reaction temperature is 50~60℃ and the reaction time is 2~4h.

[0039] Preferably, in step A2, the concentration of hydrochloric acid is 0.1~0.5 mol / L.

[0040] Preferably, in step A3, the volume of anhydrous ethanol is 3 to 5 times the volume of the filtrate in step A2.

[0041] Preferably, in step A3, the settling time is 30-60 minutes.

[0042] Preferably, in step A3, the solvent used for washing is anhydrous ethanol.

[0043] Preferably, in step A3, the drying temperature is 60~70℃ and the drying time is 8~12h.

[0044] Preferably, in step S4, the parameters of the spray dryer include: an inlet air temperature of 100~120℃, a pre-concentrated liquid pumping speed into the atomizer of 5~10mL / min, and a pre-concentrated liquid atomized into tiny droplets with a diameter of 40~50μm.

[0045] Preferably, in step S5, the granulation process includes: spraying a 10% to 15% polyvinylpyrrolidone aqueous solution into the mixture under stirring at 80 to 100 rpm, stirring for 5 to 8 minutes, using a 16 to 20 mesh nylon screen, turning on the equipment to granulate, collecting the initial granules, and drying at 50 to 55°C for 2 to 3 hours.

[0046] Compared with the prior art, the beneficial effects of the present invention are reflected in:

[0047] (1) This invention employs supercritical CO2 extraction as the primary extraction process to extract the active ingredients from Eucommia ulmoides leaves, combined with microwave-ultrasound assisted treatment, to achieve low-temperature and efficient extraction and enrichment of the active ingredients from Eucommia ulmoides leaves. Utilizing the high permeability and solubility of supercritical CO2 extraction technology under supercritical conditions, the weakly polar active ingredients in Eucommia ulmoides leaves are rapidly dissolved, while simultaneously disrupting the cell wall structure of the leaves, opening channels for subsequent solvent penetration. Microwave-ultrasound assistance accelerates the penetration of polar solvents into the cells, ultimately achieving comprehensive extraction of both weakly polar and polar components in a relatively short time.

[0048] (2) The present invention uses an inner layer of hydroxypropyl-β-cyclodextrin to encapsulate the active ingredients and steviol glycosides, and an outer layer of carboxymethylated gum arabic to embed them. The resulting solid particles can be rapidly dissolved in water at room temperature to form a uniform, stable and highly transparent liquid system, and have no bitter taste when ingested. Hydroxypropyl-β-cyclodextrin encapsulates the bitter components and steviol glycosides from Eucommia ulmoides leaves within a cavity, allowing for simultaneous release during reconstitution. This avoids the unpleasant sensation of bitterness followed by sweetness or sweet-bitter stratification caused by differences in dissolution rates during simple physical mixing, and also prevents flavor degradation due to sweetener oxidation. However, hydroxypropyl-β-cyclodextrin is prone to agglomeration during product preparation due to hydrogen bonding between its intermolecular hydroxyl groups. Therefore, it needs to be further encapsulated with a layer of carboxymethylated gum arabic. This layer forms strong hydrogen bonds with the hydroxyl groups of hydroxypropyl-β-cyclodextrin through intermolecular forces, breaking the agglomeration tendency of hydroxypropyl-β-cyclodextrin and preventing the hydroxypropyl-β-cyclodextrin inclusion complex particles from sticking and agglomerating during drying. This results in primary particles with good flowability and easy dispersion. The carboxyl groups in the carboxymethylated gum arabic structure are much more polar than the hydroxyl groups in gum arabic, allowing them to form denser hydrogen bonds with water molecules, significantly reducing the interfacial tension between the encapsulation material and water. Simultaneously, the carboxyl groups readily dissociate into -COO in water. - By breaking the aggregation between molecules through charge repulsion, carboxymethylated gum arabic can quickly disperse and dissolve upon contact with water, avoiding particle floating or delayed dissolution caused by the slow dissolution of the outer shell material. Attached Figure Description

[0049] Figure 1 This is a flowchart illustrating the preparation process of an instant solid beverage made from Eucommia ulmoides leaves, which are both food and medicine.

[0050] Figure 2 This is a flowchart illustrating the preparation process of carboxymethylated gum arabic.

[0051] Figure 3 This is a picture of the instant solid beverage made from Eucommia ulmoides leaves prepared in Example 6 after brewing. Detailed Implementation

[0052] The following embodiments are only used to illustrate the technical solutions of the present invention more clearly, and should not be used to limit the scope of protection of the present invention.

[0053] The main compounds used in the examples and comparative examples were all commercially available products and were not subjected to any further purification treatment.

[0054] Example 1

[0055] like Figure 2 As shown, a carboxymethylated gum arabic is prepared by means of:

[0056] Step A1: Disperse 10g of gum arabic in 80mL of isopropanol to obtain gum arabic dispersion. Add 12mL of sodium hydroxide aqueous solution to the dispersion. The mass-volume ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 6g:10mL. React at 30℃ for 2h to obtain gum arabic alkalization solution.

[0057] Step A2: Add 25 mL of chloroacetic acid solution to 100 mL of gum arabic alkalization solution obtained in step A1. The mass-to-volume ratio of chloroacetic acid to isopropanol in the chloroacetic acid solution is 8 g: 20 mL. React at 50 °C for 4 h. After the reaction is complete, allow it to cool naturally to room temperature. Add 0.1 mol / L hydrochloric acid while stirring to adjust the pH to 6.5. Filter and collect the filtrate.

[0058] Step A3: Add the filtrate to anhydrous ethanol at 3 times the volume of the filtrate while stirring, let stand for 30 minutes until the product precipitates, centrifuge, wash the solid 5 times with anhydrous ethanol, dry at 60℃ for 12 hours, pulverize, and sieve through 100 mesh to obtain carboxymethylated gum arabic powder.

[0059] Example 2

[0060] like Figure 2 As shown, a carboxymethylated gum arabic is prepared by means of:

[0061] Step A1: Disperse 10g of gum arabic in 90mL of isopropanol to obtain gum arabic dispersion. Add 13mL of sodium hydroxide aqueous solution to the dispersion. The mass-volume ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 5g:12mL. React at 35℃ for 1.5h to obtain gum arabic alkalization solution.

[0062] Step A2: Add 32.4 mL of chloroacetic acid solution to the 108 mL alkalization solution of gum arabic obtained in step A1. The mass-to-volume ratio of chloroacetic acid and isopropanol in the chloroacetic acid solution is 10 g: 25 mL. React at 55 °C for 3 h. After the reaction is completed, allow it to cool naturally to room temperature. Add 0.3 mol / L hydrochloric acid while stirring to adjust the pH to 7. Filter and collect the filtrate.

[0063] Step A3: Add the filtrate to anhydrous ethanol at 4 times the volume of the filtrate while stirring, let stand for 45 minutes until the product precipitates, centrifuge, wash the solid 4 times with anhydrous ethanol, dry at 65℃ for 10 hours, pulverize, and sieve through 100 mesh to obtain carboxymethylated gum arabic powder.

[0064] Example 3

[0065] like Figure 2 As shown, a carboxymethylated gum arabic is prepared by means of:

[0066] Step A1: Disperse 10g of gum arabic in 100mL of isopropanol to obtain gum arabic dispersion. Add 13.5mL of sodium hydroxide aqueous solution to the dispersion. The mass-volume ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 4g:15mL. React at 40℃ for 1h to obtain gum arabic alkalization solution.

[0067] Step A2: Add 36.8 mL of chloroacetic acid solution to 115 mL of gum arabic alkalization solution obtained in step A1. The mass-to-volume ratio of chloroacetic acid to isopropanol in the chloroacetic acid solution is 12 g: 30 mL. React at 60 °C for 2 h. After the reaction is complete, allow it to cool naturally to room temperature. Add 0.5 mol / L hydrochloric acid while stirring to adjust the pH to 6.5. Filter and collect the filtrate.

[0068] Step A3: Add the filtrate to 5 times the volume of anhydrous ethanol while stirring, let stand for 60 minutes until the product precipitates, centrifuge, wash the solid 6 times with anhydrous ethanol, dry at 70℃ for 8 hours, pulverize, and sieve through 100 mesh to obtain carboxymethylated gum arabic powder.

[0069] Example 4

[0070] like Figure 1 As shown, a method for preparing an instant solid beverage made from Eucommia ulmoides leaves (which are both food and medicine) includes:

[0071] Step S1: After cleaning and drying, pulverize the Eucommia ulmoides leaves and pass them through a 40-mesh sieve to obtain Eucommia ulmoides leaf powder. Put 100g of Eucommia ulmoides leaf powder into a supercritical CO2 extraction vessel. Set the pressure of the extraction vessel to 25MPa, the temperature to 35℃, and the CO2 flow rate to 10L / h. Extract for 1h. Then, put all the material in the extraction vessel into the desorption vessel and desorb for 30min at 40℃ and 5MPa pressure. Add 1L of ethanol aqueous solution, in which the volume ratio of ethanol to water is 1:10. Set the microwave power to 300W and the ultrasonic power to 100W. Treat for 30min at 40℃ with microwave and ultrasonic assistance. Filter to obtain the extract of active ingredients of Eucommia ulmoides leaves.

[0072] Step S2: Concentrate the extract of active ingredients from Eucommia ulmoides leaves to 1L at 40°C under ultrasonic assistance, add 10g of steviol glycosides to obtain a concentrated extract of active ingredients from Eucommia ulmoides leaves, mix the concentrated extract of active ingredients from Eucommia ulmoides leaves with 1L of hydroxypropyl-β-cyclodextrin aqueous solution, wherein the mass ratio of hydroxypropyl-β-cyclodextrin to water in the hydroxypropyl-β-cyclodextrin aqueous solution is 1:4, stir at 40°C for 20min to obtain a primary microsphere dispersion.

[0073] Step S3: Add 2L of the mixture of carboxymethylated gum arabic and maltodextrin prepared in Example 1 to 2L of primary microsphere dispersion. The mass-volume ratio of carboxymethylated gum arabic, maltodextrin and water in the mixture is 100g:200g:2000mL. Stir for 30min, concentrate to 1L at 50℃, and cool naturally to room temperature to obtain a pre-concentrated solution.

[0074] Step S4: Set the inlet air temperature of the spray dryer to 100℃, pump the pre-concentrated liquid into the atomizer at a rate of 5mL / min, atomize it into tiny droplets with a diameter of 40μm, and obtain microcapsule particles of active ingredients of Eucommia ulmoides leaves by spray drying.

[0075] Step S5: Mix 58.6g of Eucommia ulmoides leaf active ingredient microcapsule particles with 0.5g of sucrose fatty acid ester, 0.1g of glyceryl monostearate, 0.1g of L-ascorbic acid, 0.5g of sodium citrate, 0.2g of citric acid and 40g of glucose syrup powder. Spray with a 10% polyvinylpyrrolidone aqueous solution while stirring at 80rpm. Stir for 5min, granulate using a 16-mesh nylon sieve to obtain preliminary granules, and dry at 50℃ for 3h to obtain 100g of Eucommia ulmoides leaf instant solid beverage.

[0076] Example 5

[0077] like Figure 1 As shown, a method for preparing an instant solid beverage made from Eucommia ulmoides leaves (which are both food and medicine) includes:

[0078] Step S1: After cleaning and drying, pulverize the Eucommia ulmoides leaves and pass them through a 50-mesh sieve to obtain Eucommia ulmoides leaf powder. Put 100g of Eucommia ulmoides leaf powder into a supercritical CO2 extraction vessel. Set the pressure of the extraction vessel to 30MPa, the temperature to 40℃, and adjust the CO2 flow rate to 15L / h. Extract for 0.5h. Then, put all the material in the extraction vessel into the desorption vessel and desorb for 25min at 50℃ and 10MPa pressure. Add 1.5L of ethanol aqueous solution, in which the volume ratio of ethanol to water is 1:15. Set the microwave power to 400W and the ultrasonic power to 150W. Treat for 20min at 50℃ with microwave and ultrasonic assistance. Filter to obtain the extract of active ingredients of Eucommia ulmoides leaves.

[0079] Step S2: The extract of active ingredients from Eucommia ulmoides leaves is concentrated to 1L at 45°C under ultrasonic assistance. 30g of steviol glycosides is added to obtain a concentrated extract of active ingredients from Eucommia ulmoides leaves. The concentrated extract of active ingredients from Eucommia ulmoides leaves is mixed with 1.5L of hydroxypropyl-β-cyclodextrin aqueous solution, wherein the mass ratio of hydroxypropyl-β-cyclodextrin to water in the hydroxypropyl-β-cyclodextrin aqueous solution is 1:4.5. The mixture is stirred at 45°C for 15min to obtain a primary microsphere dispersion.

[0080] Step S3: Add 2.5L of the mixture of carboxymethylated gum arabic and maltodextrin prepared in Example 2 to 2L of primary microsphere dispersion. The mass-volume ratio of carboxymethylated gum arabic, maltodextrin and water in the mixture is 100g:250g:3000mL. Stir for 25min, concentrate at 55℃ to 1L, and cool to obtain a pre-concentrated solution.

[0081] Step S4: Set the inlet air temperature of the spray dryer to 110℃, pump the pre-concentrated liquid into the atomizer at a rate of 7.5mL / min, atomize it into tiny droplets with a diameter of 45μm, and then dry them to obtain microcapsule particles of active ingredients from Eucommia ulmoides leaves.

[0082] Step S5: Mix 47.1g of Eucommia ulmoides leaf active ingredient microcapsule particles with 1g of sucrose fatty acid ester, 0.2g of glyceryl monostearate, 0.2g of L-ascorbic acid, 1g of sodium citrate, 0.5g of citric acid and 50g of glucose syrup powder. Spray with a 15% polyvinylpyrrolidone aqueous solution while stirring at 90rpm. Stir for 8min. Granulate using an 18-mesh nylon sieve to obtain preliminary granules. Dry at 55℃ for 2h to obtain 100g of Eucommia ulmoides leaf instant solid beverage.

[0083] Example 6

[0084] like Figure 1 As shown, a method for preparing an instant solid beverage made from Eucommia ulmoides leaves (which are both food and medicine) includes:

[0085] Step S1: After cleaning and drying, pulverize the Eucommia ulmoides leaves and pass them through a 60-mesh sieve to obtain Eucommia ulmoides leaf powder. Put 100g of Eucommia ulmoides leaf powder into a supercritical CO2 extraction vessel. Set the pressure of the extraction vessel to 40MPa, the temperature to 50℃, and the CO2 flow rate to 20L / h. Extract for 1h. Then, put all the material in the extraction vessel into the desorption vessel and desorb for 20min at 60℃ and 10MPa pressure. Add 1L of ethanol aqueous solution, in which the volume ratio of ethanol to water is 1:20. Set the microwave power to 500W and the ultrasonic power to 200W. Treat for 15min at 60℃ with microwave and ultrasonic assistance. Filter to obtain the extract of active ingredients of Eucommia ulmoides leaves.

[0086] Step S2: Concentrate the extract of active ingredients from Eucommia ulmoides leaves to 1L at 50°C under ultrasonic assistance, add 50g of steviol glycosides to obtain a concentrated extract of active ingredients from Eucommia ulmoides leaves, mix the concentrated extract of active ingredients from Eucommia ulmoides leaves with 2L of hydroxypropyl-β-cyclodextrin aqueous solution, wherein the mass ratio of hydroxypropyl-β-cyclodextrin to water in the hydroxypropyl-β-cyclodextrin aqueous solution is 1:5, stir at 40°C for 15min to obtain a primary microsphere dispersion.

[0087] Step S3: Add 3L of the mixture of carboxymethylated gum arabic and maltodextrin prepared in Example 3 to 2L of primary microsphere dispersion. The mass-volume ratio of carboxymethylated gum arabic, maltodextrin and water in the mixture is 100g:300g:4000mL. Stir for 20min, concentrate to 1L at 60℃, and cool naturally to room temperature to obtain a pre-concentrated solution.

[0088] Step S4: Set the inlet air temperature of the spray dryer to 120℃, pump the pre-concentrated liquid into the atomizer at a rate of 10mL / min, atomize it into tiny droplets with a diameter of 50μm, and obtain microcapsule particles of active ingredients of Eucommia ulmoides leaves by spray drying.

[0089] Step S5: Mix 42.8g of Eucommia ulmoides leaf active ingredient microcapsule granules with 0.5g of sucrose fatty acid ester, 0.1g of glyceryl monostearate, 0.3g of L-ascorbic acid, 0.5g of sodium citrate, 0.8g of citric acid, and 55g of glucose syrup powder. Spray with a 10% polyvinylpyrrolidone aqueous solution while stirring at 100rpm for 8 minutes. Granulate using a 20-mesh nylon sieve to obtain preliminary granules. Dry at 50℃ for 2 hours to obtain 100g of Eucommia ulmoides leaf instant solid beverage. After brewing, as shown... Figure 3 As shown.

[0090] Comparative Example 1

[0091] A kind of instant solid beverage made from Eucommia ulmoides leaves that is both food and medicine is prepared in a way that differs from that in Example 6. In step S2, hydroxypropyl-β-cyclodextrin is not used to encapsulate and prepare microspheres. Instead, the extract of active ingredients of Eucommia ulmoides leaves is directly encapsulated with carboxymethylated gum arabic.

[0092] Comparative Example 2

[0093] A kind of instant solid beverage made from Eucommia ulmoides leaves that is both food and medicine is prepared in a way that differs from that in Example 6, the microspheres prepared by encapsulation with hydroxypropyl-β-cyclodextrin in step S2 are encapsulated with unmodified gum arabic.

[0094] The contents of Escherichia coli, mold, Salmonella, and lead in the instant solid beverages made from Eucommia ulmoides leaves prepared in Examples 4-6 and Comparative Examples 1-2 were tested according to standard GB4789-2016. The results are shown in Tables 1-4.

[0095] The instant eucommia leaf solid beverages prepared in Examples 4-6 and Comparative Examples 1-2 were brewed with mineral water, and their sensory evaluation was performed. The results are shown in Table 5.

[0096] Table 1. Results of Escherichia coli detection

[0097]

[0098] Table 2. Mold Detection Results

[0099]

[0100] Table 3 Salmonella Detection Results

[0101]

[0102] Table 4 Detection results of heavy metal lead

[0103]

[0104] According to the data in Tables 1 to 4, the number of Escherichia coli, mold, and Salmonella in the Eucommia ulmoides leaf solid beverages prepared in Examples 4 to 6 and Comparative Examples 1 to 2 were all within the required range, and the content of heavy metal lead ions also met the standards.

[0105] Table 5 Sensory Evaluation

[0106]

[0107] As shown in Table 5, the instant eucommia leaf solid beverages prepared in Examples 4-6, when brewed with room temperature mineral water, produced a clear liquid with high clarity, no sediment or suspended matter, no foreign impurities, bright color, aroma, and good taste. The instant eucommia leaf solid beverage prepared in Comparative Example 1, where the active ingredient was only encapsulated with hydroxypropyl-β-cyclodextrin and not with carboxymethylated gum arabic, had a slower dissolution rate during brewing, resulting in a slightly turbid liquid. Stirring did not improve the turbidity. After standing for a period of time, no sediment was found, but suspended matter remained, resulting in a darker color, aroma, and poor taste. The instant eucommia leaf solid beverage prepared in Comparative Example 2 dissolved and stirred during brewing, forming distinct layers in the water. After stirring or shaking, the layers disappeared, forming a homogeneous liquid with high clarity, no sediment or foreign impurities, bright color, aroma, and good taste.

[0108] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A soluble solid beverage made from Eucommia ulmoides leaves, which is both a food and a medicine, characterized in that... The product comprises microcapsule particles of active ingredients from Eucommia ulmoides leaves, sucrose fatty acid esters, glyceryl monostearate, L-ascorbic acid, sodium citrate, citric acid, and glucose syrup powder. The microcapsule particles of active ingredients from Eucommia ulmoides leaves include an extract of active ingredients from Eucommia ulmoides leaves, steviol glycosides, an inner wall material, and an outer wall material. The inner wall material is hydroxypropyl-β-cyclodextrin, and the outer wall material is carboxymethylated gum arabic and maltodextrin. The content of each component in the instant solid beverage containing Eucommia ulmoides leaves is as follows: 0.5%~1% sucrose fatty acid esters, 0.1%~0.2% glyceryl monostearate, 0.1%~0.3% L-ascorbic acid, 0.5%~1% sodium citrate, 0.2%~0.8% citric acid, 40%~55% glucose syrup powder, with the remainder being microcapsule particles of active ingredients from Eucommia ulmoides leaves.

2. The instant solid beverage made from Eucommia ulmoides leaves (a medicinal and edible herb) according to claim 1, characterized in that, The volume-to-mass ratio of Eucommia ulmoides leaf active ingredient extract, stevioside, hydroxypropyl-β-cyclodextrin, carboxymethylated gum arabic, and maltodextrin in the Eucommia ulmoides leaf active ingredient microcapsule particles is 1L:(10~50)g:(300~500)g:100g:(200~300)g.

3. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 1, characterized in that, include: Step S1: After cleaning and drying, the Eucommia ulmoides leaves are crushed and sieved to obtain Eucommia ulmoides leaf powder. The Eucommia ulmoides leaf powder is placed in a supercritical CO2 extraction vessel for extraction. The powder is added to an ethanol aqueous solution and treated with microwave-ultrasound assisted to obtain an extract of active ingredients from Eucommia ulmoides leaves. Step S2: Concentrate the extract of active ingredients from Eucommia ulmoides leaves under ultrasonic assistance, add steviol glycosides to obtain a concentrated extract of active ingredients from Eucommia ulmoides leaves, mix the concentrated extract of active ingredients from Eucommia ulmoides leaves with an aqueous solution of hydroxypropyl-β-cyclodextrin, stir to obtain a primary microsphere dispersion. Step S3: Add a mixture of carboxymethylated gum arabic and maltodextrin to the primary microsphere dispersion, stir, concentrate, and cool to obtain a pre-concentrated solution; Step S4: Set the parameters of the spray dryer, pump the pre-concentrated liquid into the atomizer, and obtain microcapsule particles of active ingredients of Eucommia ulmoides leaves through spray drying; Step S5: Mix the microcapsule particles of active ingredients of Eucommia ulmoides leaf, sucrose fatty acid ester, glyceryl monostearate, L-ascorbic acid, sodium citrate, citric acid and glucose syrup powder to obtain a mixture. Granulate the mixture to obtain Eucommia ulmoides leaf instant beverage.

4. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 3, characterized in that, In step S1, the sieve mesh size is 40-60 mesh; the volume ratio of ethanol to water in the ethanol-water solution is 1:(10-20); the mass-volume ratio of Eucommia ulmoides leaf powder to ethanol-water solution is 1g:(10-15)mL; the specific parameters of the microwave-ultrasonic assisted treatment include: microwave power of 300-500W, ultrasonic power of 100-200W, treatment temperature of 40-60℃, and treatment time of 15-30min. The specific extraction process includes: loading Eucommia ulmoides leaf powder into an extraction vessel, with an extraction vessel pressure of 25~40MPa, an extraction temperature of 35~50℃, a CO2 flow rate of 10~20L / h, and an extraction time of 0.5~1h; the material is then placed into an analysis vessel, with an analysis vessel pressure of 5~10MPa, an analysis temperature of 40~60℃, and an analysis time of 20~30min.

5. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 3, characterized in that, In step S2, the concentration temperature is 40-50℃; the volume-to-mass ratio of the Eucommia ulmoides leaf active ingredient extract to steviol glycosides is 100mL:(1-5)g; in the hydroxypropyl-β-cyclodextrin aqueous solution, the mass ratio of hydroxypropyl-β-cyclodextrin to water is 1:(4-5); the volume ratio of the Eucommia ulmoides leaf active ingredient concentrate to the hydroxypropyl-β-cyclodextrin aqueous solution is 1:(1-2); the stirring temperature is 40-45℃, and the stirring time is 15-20min.

6. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 3, characterized in that, In step S3, the volume ratio of the primary microsphere dispersion to the mixture is 1:(1~1.5); in the mixture, the mass-volume ratio of carboxymethylated gum arabic, maltodextrin, and water is 1g:(2~3)g:(20~40)mL; the stirring time is 20~30min; and the concentration temperature is 50~60℃.

7. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 3, characterized in that, In step S3, the method for preparing carboxymethylated gum arabic includes: Step A1: Disperse gum arabic in isopropanol to obtain gum arabic dispersion, add sodium hydroxide aqueous solution to it, react to obtain gum arabic alkalization solution; Step A2: Add chloroacetic acid solution to the gum arabic alkalization solution and react. After the reaction is complete, cool and add hydrochloric acid while stirring to adjust the pH to 6.5-7.

0. Filter and collect the filtrate. Step A3: Add the filtrate to anhydrous ethanol with stirring, let stand until the product precipitates, centrifuge, wash, dry, pulverize, and sieve to obtain carboxymethylated gum arabic powder.

8. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a medicinal and edible herb) according to claim 7, characterized in that, In step A1, the mass-to-volume ratio of gum arabic, isopropanol, and sodium hydroxide aqueous solution is 1 g : (8~10) mL : (1.2~1.35) mL; the mass-to-volume ratio of sodium hydroxide and water in the sodium hydroxide aqueous solution is (4~6) g : (10~15) mL; the reaction temperature is 30~40℃, and the reaction time is 1~2 h. In step A2, the solvent in the chloroacetic acid solution is isopropanol, and the mass-to-volume ratio of chloroacetic acid to solvent is (8~12) g : (20~30) mL; the volume ratio of the gum arabic alkalization solution to the chloroacetic acid solution is 1 : (0.25~0.32); the reaction temperature is 50~60℃, the reaction time is 2~4 h, and the concentration of hydrochloric acid is 0.1~0.5 mol / L.

9. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 7, characterized in that, In step A3, the volume of anhydrous ethanol is 3 to 5 times the volume of the filtrate in step A2; the standing time is 30 to 60 minutes; the washing solvent is anhydrous ethanol; the drying temperature is 60 to 70°C, and the drying time is 8 to 12 hours.

10. The preparation process of an instant solid beverage made from Eucommia ulmoides leaves (a food and medicine homology) according to claim 3, characterized in that, In step S4, the parameters of the spray dryer include: an inlet air temperature of 100~120℃, a pre-concentrated liquid pumping speed of 5~10mL / min into the atomizer, and a pre-concentrated liquid atomized into tiny droplets with a diameter of 40~50μm. In step S5, the granulation process includes: spraying a 10% to 15% polyvinylpyrrolidone aqueous solution onto the mixture under stirring at 80 to 100 rpm, stirring for 5 to 8 minutes, using a 16 to 20 mesh nylon screen, turning on the equipment to granulate, collecting the initial granules, and drying at 50 to 55°C for 2 to 3 hours.

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