A green preparation method of a functional powder of a medicinal and edible traditional Chinese medicinal material

Abstract

This invention discloses a green preparation method for functional powders made from medicinal and edible herbs, belonging to the field of traditional Chinese medicine pharmaceutical technology. Using polysaccharide-based medicinal and edible herbs as raw materials, this invention efficiently couples low-temperature plasma pretreatment, enzymatic hydrolysis, ultra-low temperature gradient ball milling, airflow pulverization, food-grade compound coating, ultrasonic modification, and negative pressure low-temperature microcapsule spray fluidized bed granulation. The process route is simple, highly controllable, and environmentally friendly. This method can significantly reduce powder particle size, improve powder processing characteristics, and enhance powder hydrophilicity and flowability, effectively solving problems such as large particle size, poor solubility, easy loss of activity, and easy agglomeration and wall adhesion in traditional processes. The resulting functional powder has advantages such as uniform particle size, excellent processing characteristics, good filling properties, good solubility, excellent flowability, retention rate of active ingredients exceeding 90%, low moisture absorption, low water activity, and high antioxidant activity.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine pharmaceutical technology, and more specifically, relates to a green preparation method for functional powders of medicinal and edible Chinese medicinal materials. Background Technology

[0002] Traditional Chinese medicinal herbs that are also used in food (such as astragalus, wolfberry, and yam) possess both medicinal value and food safety. Their active ingredients (such as astragalus polysaccharides, wolfberry polysaccharides, and yam saponins) have various effects, including enhancing immunity and regulating bodily functions, and have broad application prospects in health products, functional foods, and pharmaceuticals. Functional powders, as a form of application for traditional Chinese medicine derived from these herbs, directly affect the absorption and functional performance of the products due to their particle size, solubility, and retention rate of active ingredients.

[0003] Currently, the preparation of powders from medicinal and edible herbs mostly employs traditional pulverization techniques, such as ordinary ball mills and universal pulverizers. These methods suffer from problems such as large particle size, easy agglomeration, difficulty in releasing active ingredients, and poor solubility, resulting in low absorption and utilization efficiency by the human body and limiting the full realization of their functional value. To improve powder performance, some preparation methods use organic solvents for surface modification or extraction. This not only increases production costs but may also leave residual organic solvents, posing safety hazards and failing to meet the production standards for green food and pharmaceutical preparations.

[0004] Existing ultrafine pulverization technologies mostly rely on a single pulverization method, resulting in low pulverization efficiency, uneven particle size distribution, and easy degradation of active ingredients due to high temperatures. Furthermore, commonly used surface modifiers are often non-food grade or have poor modification effects, failing to achieve rapid cold water dissolution of the powder. Simultaneously, existing preparation methods struggle to simultaneously meet requirements such as ultrafine pulverization, high solubility, high retention rate of active ingredients, and absence of organic solvent residues. Therefore, developing a green, environmentally friendly method for preparing functional powders from medicinal and edible herbs with superior overall performance is of great significance. Summary of the Invention

[0005] To address the aforementioned problems in existing technologies, the present invention aims to provide a green preparation method for functional powders of medicinal and edible herbs. This method synergistically couples multiple technologies, including ultra-low temperature ball milling and air jet milling, food-grade compound surface hydrophilic modification, and negative pressure low temperature microcapsule spray fluidized bed granulation, to achieve ultra-micronization, high solubility, and high retention of active ingredients in the powders of medicinal and edible herbs without the use of organic solvents.

[0006] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is as follows:

[0007] A green preparation method for functional powders of medicinal and edible herbs includes the following steps:

[0008] 1) Select medicinal and edible herbs, clean and remove impurities, then treat with low-temperature plasma, add cellulase for enzymatic hydrolysis, dry to a moisture content of no more than 8%, and pulverize and sieve to obtain coarse powder;

[0009] 2) The pretreated coarse powder is placed in an ultra-low temperature ball mill and ball milled using a gradient temperature change method to obtain primary ultrafine powder; then the primary ultrafine powder is subjected to air jet milling and classified by a low temperature air jet classifier to obtain ultrafine powder.

[0010] 3) Prepare a food-grade modifier solution, add the ultrafine powder obtained in step 2) to the modifier solution, and after ultrasonic modification, vacuum dry, pulverize and sieve to obtain modified ultrafine powder;

[0011] 4) The modified ultrafine powder obtained in step 3) is placed in a negative pressure low temperature microcapsule spray fluidized bed for granulation, cooled and sieved to obtain an instant functional powder.

[0012] Preferably, in step 1), the medicinal and edible herbs are selected from one or more of Astragalus membranaceus, Lycium barbarum, Dioscorea opposita, Polygonatum sibiricum, and Poria cocos.

[0013] Preferably, in step 1), the low-temperature plasma treatment power is 90~115W and the treatment time is 70~100s.

[0014] Preferably, in step 1), the amount of cellulase added is 0.1% to 0.3% of the dry basis weight of the medicinal and edible herbs, the enzymatic hydrolysis temperature is 40 to 44°C, and the enzymatic hydrolysis time is 25 to 35 minutes.

[0015] Preferably, in step 1), the crushing and sieving process involves crushing the material and then passing it through a 30-50 mesh sieve.

[0016] Preferably, in step 2), the specific process of gradient temperature ball milling is as follows: first, ball milling at -120℃ for 0.4~0.7h, then at -80℃ for 0.5~0.6h, and finally at -50℃ for 0.4~0.6h, with a total ball milling time of 1.2~1.8h; the airflow pressure of the air jet mill is 0.6~0.8MPa.

[0017] Preferably, in step 2), the ball-to-material ratio of the cryogenic ball mill is 10:1 to 15:1, the ball milling speed is 300 to 400 r / min, and the feed rate of the air jet mill is 10 to 20 g / min.

[0018] Preferably, in step 3), the food-grade modifier is a compound system of sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester; the mass concentration of the modifier solution is 5%~10%.

[0019] Preferably, in step 3), the mass ratio of sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide, and polyglycerol fatty acid ester is 3:5:1:0.3:0.05.

[0020] Preferably, in step 3), the total amount of modifier added is 8% to 9% of the mass of the ultrafine powder; the ultrasonic treatment power is 220 to 270 W, the frequency is 20 to 22 kHz, and the time is 18 to 25 min.

[0021] Preferably, in step 3), the vacuum drying temperature is 45°C, the drying time is 1.5 hours, and the material is pulverized through a 100-mesh sieve.

[0022] Preferably, in step 4), the negative pressure low-temperature microcapsule spray fluidized bed granulation conditions are: negative pressure -0.025~-0.035MPa, inlet air temperature 75~88℃, outlet air temperature 38~42℃, and granulation time 35~40min.

[0023] Preferably, in step 4), the cooled product is passed through a 110-130 mesh sieve.

[0024] Beneficial effects: Compared with the prior art, the present invention has the following advantages:

[0025] 1) This invention uses a combination of ultra-low temperature ball milling and air jet milling technology to achieve ultra-fine pulverization of medicinal and edible Chinese medicinal materials; the ultra-low temperature environment can effectively avoid the degradation of active ingredients caused by the heat generated during the pulverization process; compared with a single pulverization method, the combined pulverization technology is more efficient, produces smaller powder particles, and has a more uniform distribution, which is conducive to the rapid release of active ingredients and their absorption and utilization by the human body.

[0026] 2) This invention uses a food-grade compound modifier to hydrophilize the surface of ultrafine powder. The modifier used is safe and non-toxic, and can significantly improve the problems of high viscosity, difficulty in dispersion and difficulty in dissolving of high polysaccharide Chinese medicinal powder. It makes the cold water solubility of the finished powder >85% and the dissolution time <33s, realizing the instant dissolution of the powder in cold water and greatly expanding the application scenarios of the product.

[0027] 3) The present invention adopts a preparation process without organic solvents throughout. From raw material pretreatment, ultrafine grinding, surface modification to spray granulation, water is used as the medium, eliminating the risk of solvent residue and meeting the green food production standards.

[0028] 4) This invention utilizes the synergistic coupling of multiple technologies, including low-temperature plasma activation, enzymatic hydrolysis, ultrasonic-assisted modification, and negative pressure microencapsulation granulation, to maximize the protection of the active ingredients of Chinese medicinal materials under mild conditions, with an active ingredient retention rate of ≥90%. At the same time, it significantly improves the flowability, moisture resistance, and storage stability of the powder, solving problems such as easy agglomeration, easy adhesion to the wall, and poor processing suitability of the powder.

[0029] 5) The process route of this invention is simple, the parameters are controllable, and the adaptability is strong. It can be applied to one or more high-viscosity, difficult-to-crush medicinal and edible materials such as Astragalus membranaceus, Lycium barbarum, Dioscorea opposita, Polygonatum sibiricum, and Poria cocos. It has strong versatility and is easy to scale up for industrial production. The functional powder produced can be directly used in solid beverages, functional foods, health foods and traditional Chinese medicine preparations, and has significant economic value and application prospects. Attached Figure Description

[0030] Figure 1 This is a process flow diagram for preparing functional powders of medicinal and edible herbs according to the present invention. Detailed Implementation

[0031] To make the objectives, technical solutions, and advantages of this invention clearer, the invention is further described below with reference to specific embodiments. Unless otherwise specified, the technical means used in the following embodiments are all conventional means well known to those skilled in the art. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer are followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0032] This application provides a green preparation method for functional powders of medicinal and edible herbs, such as... Figure 1 As shown, using medicinal and edible herbs such as Astragalus membranaceus, Lycium barbarum, Dioscorea opposita, Polygonatum sibiricum, and Poria cocos as raw materials, the process involves four core steps: raw material pretreatment, ultra-micronization, surface hydrophilic modification, and negative pressure low-temperature microencapsulation spray fluidized bed granulation. After cleaning and impurity removal, the medicinal and edible herbs undergo low-temperature plasma activation and food-grade cellulase hydrolysis, followed by vacuum freeze-drying and coarse pulverization to obtain qualified coarse powder. The coarse powder is then fed into a combined ultra-low temperature gradient ball mill and airflow milling system, achieving efficient ultra-micronization under low-temperature conditions to avoid thermal degradation of active ingredients and obtain ultra-fine powder with uniform particle size distribution. The ultra-fine powder is then ultrasonically coated with a food-grade compound modifier to significantly improve the surface hydrophilicity of the powder, addressing the problems of high viscosity, poor solubility, and easy agglomeration of polysaccharide materials. The modified powder is then granulated, cooled, and sieved using a negative pressure low-temperature microencapsulation spray fluidized bed to finally obtain an instant functional powder that is rapidly soluble in cold water, has good flowability, high stability, and an active ingredient retention rate of ≥90%.

[0033] Example 1

[0034] A green preparation method for Astragalus functional powder includes the following steps:

[0035] 1) Take Astragalus membranaceus slices, clean them and remove impurities, then process them with a 100W low-temperature plasma processor for 90 seconds. Add food-grade cellulase to the processed Astragalus membranaceus slices at a dosage of 0.2% of the dry weight of Astragalus membranaceus, and add an appropriate amount of purified water. Incubate at 42℃ for 30 minutes. After the enzymatic hydrolysis is completed, freeze-dry the material under vacuum at -40℃ until the moisture content is 4.5%. Crush the dried Astragalus membranaceus blocks using a universal pulverizer and pass them through a 30-mesh sieve to obtain Astragalus membranaceus coarse powder.

[0036] 2) The coarse Astragalus powder obtained in step 1) was fed into an ultra-low temperature ball mill with a ball-to-material ratio of 12:1 and a ball milling speed of 350 r / min. The ball milling was carried out for 1.5 h using a gradient three-stage temperature change method: first ball milling at -120℃ for 0.5 h, then ball milling at -80℃ for 0.5 h, and finally ball milling at -50℃ for 0.5 h. The ball-milled material was then transferred to a pulse airflow pulverizer for ultra-fine pulverization. The pulse frequency was set to 0.2 s on and 0.1 s intermittent, the working pressure was 0.8 MPa, and the feed rate was 10 g / min. The pulverized powder was then classified by a low-temperature airflow classifier to obtain ultrafine powder.

[0037] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 9% modifier solution.

[0038] The Astragalus ultrafine powder obtained in step 2) was added to the modifier solution, and the total amount of modifier added was 9% of the mass of the Astragalus ultrafine powder. The mixture was stirred and dispersed evenly. The mixture was treated with ultrasonic power of 250W and frequency of 20kHz for 20min. After ultrasonic treatment, the mixture was placed in a vacuum drying oven at 45℃ and dried for 1.5h. The dried material was crushed by a pulverizer and passed through a 100-mesh sieve to obtain modified powder.

[0039] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.03MPa, air inlet temperature is 80℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 120-mesh sieve and the sieve material is collected to obtain Astragalus functional powder.

[0040] Example 2

[0041] A green preparation method for a compound functional powder of wolfberry-yam-poria cocos includes the following steps:

[0042] 1) Weigh out wolfberry, yam, and poria cocos (medicinal and edible raw materials) in a mass ratio of 1:1:1, mix them, wash them clean, and process them with a 90W low-temperature plasma processor for 100 seconds. Add food-grade cellulase to the treated mixture at a rate of 0.15% of the dry weight of the mixture, and add an appropriate amount of purified water. Incubate the mixture at 42℃ for 35 minutes. After the enzymatic hydrolysis is completed, freeze-dry the material under vacuum at -40℃ until the moisture content is ≤5%. Crush the dried material using a universal pulverizer and pass it through a 30-mesh sieve to obtain a coarse powder of the compound medicinal material.

[0043] 2) The composite coarse powder obtained in step 1) is fed into an ultra-low temperature ball mill with a ball-to-material ratio of 13:1 and a rotation speed of 360 r / min. The milling is performed for 1.8 h using a gradient three-stage temperature change method: first, ball milling at -120℃ for 0.6 h; then, ball milling at -80℃ for 0.6 h; finally, ball milling at -50℃ for 0.6 h. The milled material is then transferred to a pulse jet mill for ultra-fine grinding. The pulse frequency is set to 0.2 s on and 0.1 s off, the working pressure is 0.75 MPa, and the feed rate is 16 g / min. The pulverized powder is then classified by a low-temperature airflow classifier to obtain ultra-fine composite powder.

[0044] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a modifier solution with a mass fraction of 8%.

[0045] The ultrafine composite powder obtained in step 2) is added to the modifier solution, with the total amount of modifier added being 8% of the mass of the ultrafine composite powder. The mixture is stirred and dispersed evenly. The mixture is then treated with ultrasonic power of 220W and frequency of 20kHz for 25 minutes. After ultrasonic treatment, the mixture is placed in a vacuum drying oven at 45℃ and dried for 1.5 hours. The dried material is then pulverized using a pulverizer and passed through a 100-mesh sieve to obtain the modified composite powder.

[0046] 4) The modified composite powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.025MPa, air inlet temperature is 75℃, air outlet temperature is 38℃, and granulation time is 35min. After granulation and cooling, the granules are passed through a 130-mesh sieve and the sieve material is collected to obtain the wolfberry-yam-poria composite functional powder.

[0047] Example 3

[0048] A green preparation method for Astragalus-Lycium-Dioscorea composite functional powder includes the following steps:

[0049] 1) Weigh out three medicinal and edible raw materials, namely Astragalus membranaceus, Lycium barbarum, and Dioscorea opposita, in a mass ratio of 2:1:1. After mixing and cleaning, process the mixture with a 100W low-temperature plasma processor for 90 seconds. Add food-grade cellulase to the processed mixture at a concentration of 0.2% of the dry weight of the mixture and add an appropriate amount of purified water. Incubate the mixture at 42°C for 30 minutes. After the enzymatic hydrolysis is completed, freeze-dry the material under vacuum at -40°C until the moisture content is ≤5%. Crush the dried material using a universal pulverizer and pass it through a 30-mesh sieve to obtain a coarse powder of the compound medicinal materials.

[0050] 2) The coarse powder of the composite medicinal material obtained in step 1) is fed into an ultra-low temperature ball mill with a ball-to-material ratio of 12:1 and a rotation speed of 350 r / min. The ball milling is carried out for 1.5 h using a gradient three-stage temperature change method: first ball milling at -120℃ for 0.5 h, then ball milling at -80℃ for 0.5 h, and finally ball milling at -50℃ for 0.5 h. The ball-milled material is then transferred to a pulse airflow pulverizer for ultra-fine pulverization. The pulse frequency is set to 0.2 s on and 0.1 s off, the working pressure is 0.75 MPa, and the feed rate is 15 g / min. The pulverized powder is then classified by a low-temperature airflow classifier to obtain ultra-fine composite powder.

[0051] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 9% modifier solution.

[0052] The ultrafine composite powder obtained in step 2) is added to the modifier solution, with the total amount of modifier added being 8% of the mass of the ultrafine composite powder. The mixture is stirred and dispersed evenly. The mixture is then treated with ultrasonic power of 250W and frequency of 22kHz for 25 minutes. After ultrasonic treatment, the mixture is placed in a vacuum drying oven at 45℃ and dried for 1.5 hours. The dried material is then pulverized using a pulverizer and passed through a 100-mesh sieve to obtain the modified composite powder.

[0053] 4) The modified composite powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.03MPa, air inlet temperature is 85℃, air outlet temperature is 42℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 120-mesh sieve and the sieve material is collected to obtain Astragalus-Lycium barbarum-Dioscorea opposita composite functional powder.

[0054] Example 4

[0055] A green preparation method for yam functional powder includes the following steps:

[0056] 1) After washing and peeling, the yam is treated with a 110W low-temperature plasma processor for 80 seconds. Food-grade cellulase is added to the treated yam at a dosage of 0.25% of the yam mass, along with an appropriate amount of purified water. The mixture is then enzymatically hydrolyzed at 40℃ for 35 minutes. After the enzymatic hydrolysis is completed, the material is vacuum freeze-dried at -40℃ until the moisture content is 4.5%. The dried yam is then pulverized using a universal pulverizer and passed through a 40-mesh sieve to obtain coarse yam powder.

[0057] 2) The coarse yam powder obtained in step 1) is fed into an ultra-low temperature ball mill with a ball-to-material ratio of 14:1 and a rotation speed of 380 r / min. The milling is performed for 1.6 h using a gradient three-stage temperature control method: first, ball milling at -120℃ for 0.6 h; then at -80℃ for 0.5 h; and finally at -50℃ for 0.5 h. The milled material is then transferred to a pulse jet mill for ultra-fine grinding. The pulse frequency is set to 0.2 s on and 0.1 s off, the working pressure is 0.8 MPa, and the feed rate is 12 g / min. The pulverized powder is then classified by a low-temperature airflow classifier to obtain ultra-fine yam powder.

[0058] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a modifier solution with a mass fraction of 8%.

[0059] Add the yam ultrafine powder obtained in step 2) to the modifier solution. The total amount of modifier added is 9% of the mass of the yam ultrafine powder. Stir and disperse evenly. Treat the mixture with ultrasonic power of 260W and frequency of 20kHz for 20min. After ultrasonic treatment, place the mixture in a vacuum drying oven at 45℃ and dry for 1.5h. Crush the dried material with a pulverizer and pass it through a 100-mesh sieve to obtain modified powder.

[0060] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.03MPa, air inlet temperature is 80℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 110-mesh sieve and the sieve material is collected to obtain yam functional powder.

[0061] Example 5

[0062] A green preparation method for wolfberry functional powder includes the following steps:

[0063] 1) After washing, the goji berries were treated with a 90W low-temperature plasma processor for 100 seconds. Food-grade cellulase was added to the treated goji berries at a concentration of 0.1% of the goji berry mass, along with an appropriate amount of purified water. The mixture was then enzymatically hydrolyzed at 43°C for 25 minutes. After the enzymatic hydrolysis was completed, the material was vacuum freeze-dried at -40°C until the moisture content was 4%. The dried goji berries were then pulverized using a universal pulverizer and passed through a 40-mesh sieve to obtain coarse goji berry powder.

[0064] 2) The coarse wolfberry powder obtained in step 1) was fed into an ultra-low temperature ball mill with a ball-to-material ratio of 11:1 and a rotation speed of 330 r / min. The ball milling was carried out for 1.3 h using a gradient three-stage temperature change method: first ball milling at -120℃ for 0.4 h, then ball milling at -80℃ for 0.5 h, and finally ball milling at -50℃ for 0.4 h. The ball-milled material was then transferred to a pulse airflow pulverizer for ultra-fine pulverization. The pulse frequency was set to 0.2 s on and 0.1 s intermittent, the working pressure was 0.7 MPa, and the feed rate was 13 g / min. The pulverized powder was then classified by a low-temperature airflow classifier to obtain ultra-fine wolfberry powder.

[0065] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 7% modifier solution.

[0066] The wolfberry ultrafine powder obtained in step 2) was added to the modifier solution, and the total amount of modifier added was 9% of the mass of the wolfberry ultrafine powder. The mixture was stirred and dispersed evenly. The mixture was treated with ultrasonic power of 230W and frequency of 20kHz for 22 minutes. After ultrasonic treatment, the mixture was placed in a vacuum drying oven at 45℃ and dried for 1.5 hours. The dried material was crushed by a pulverizer and passed through a 100-mesh sieve to obtain modified powder.

[0067] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.025MPa, air inlet temperature is 78℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 120-mesh sieve and the sieve material is collected to obtain wolfberry functional powder.

[0068] Example 6

[0069] A green preparation method for Polygonatum functional powder includes the following steps:

[0070] 1) After washing, Polygonatum sibiricum was treated with a 105W low-temperature plasma processor for 90 seconds. Food-grade cellulase was added to the treated Polygonatum sibiricum at a dosage of 0.2% of the Polygonatum sibiricum mass, along with an appropriate amount of purified water. The mixture was then enzymatically hydrolyzed at 41℃ for 32 minutes. After the enzymatic hydrolysis was completed, the material was vacuum freeze-dried at -40℃ until the moisture content was 4.3%. The dried Polygonatum sibiricum was then pulverized using a universal pulverizer and passed through a 30-mesh sieve to obtain coarse Polygonatum sibiricum powder.

[0071] 2) The coarse powder of Polygonatum obtained in step 1) is fed into an ultra-low temperature ball mill with a ball-to-material ratio of 15:1 and a rotation speed of 400 r / min. The ball milling is carried out for 1.7 h using a gradient three-stage temperature change method: first ball milling at -120℃ for 0.7 h, then ball milling at -80℃ for 0.5 h, and finally ball milling at -50℃ for 0.5 h. The ball-milled material is then transferred to a pulse airflow pulverizer for ultra-fine pulverization. The pulse frequency is set to 0.2 s on and 0.1 s off, the working pressure is 0.8 MPa, and the feed rate is 18 g / min. The pulverized powder is then classified by a low-temperature airflow classifier to obtain Polygonatum ultrafine powder.

[0072] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 10% modifier solution.

[0073] The Polygonatum ultrafine powder obtained in step 2) was added to the modifier solution, and the total amount of modifier added was 9% of the mass of Polygonatum ultrafine powder. The mixture was stirred and dispersed evenly. The mixture was treated with ultrasonic power of 270W and frequency of 20kHz for 18 minutes. After ultrasonic treatment, the mixture was placed in a vacuum drying oven at 45℃ and dried for 1.5 hours. The dried material was crushed by a pulverizer and passed through a 100-mesh sieve to obtain modified powder.

[0074] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.035MPa, air inlet temperature is 88℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 130-mesh sieve and the sieve material is collected to obtain Polygonatum functional powder.

[0075] Example 7

[0076] A green preparation method for Poria cocos functional powder includes the following steps:

[0077] 1) After washing and peeling, Poria cocos was treated with a 115W low-temperature plasma processor for 70 seconds. Food-grade cellulase was added to the treated Poria cocos at a dosage of 0.3% of the Poria cocos mass, along with an appropriate amount of purified water. The mixture was then enzymatically hydrolyzed at 44℃ for 30 minutes. After the enzymatic hydrolysis was completed, the material was vacuum freeze-dried at -40℃ until the moisture content was 3.8%. The dried Poria cocos was then pulverized using a universal pulverizer and passed through a 50-mesh sieve to obtain coarse Poria cocos powder.

[0078] 2) The coarse Poria cocos powder obtained in step 1) was fed into an ultra-low temperature ball mill with a ball-to-material ratio of 10:1 and a rotation speed of 300 r / min. The ball milling was carried out for 1.4 h using a gradient three-stage temperature change method: first ball milling at -120℃ for 0.5 h, then ball milling at -80℃ for 0.5 h, and finally ball milling at -50℃ for 0.4 h. The ball-milled material was then transferred to a pulse airflow pulverizer for ultra-fine pulverization. The pulse frequency was set to 0.2 s on and 0.1 s off, the working pressure was 0.6 MPa, and the feed rate was 20 g / min. The pulverized powder was then classified by a low-temperature airflow classifier to obtain ultra-fine Poria cocos powder.

[0079] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 5% modifier solution.

[0080] Add the Poria cocos ultrafine powder obtained in step 2) to the modifier solution. The total amount of modifier added is 9% of the mass of the Poria cocos ultrafine powder. Stir and disperse evenly. Treat the mixture with ultrasonic power of 240W and frequency of 20kHz for 24min. After ultrasonic treatment, place the mixture in a vacuum drying oven at 45℃ and dry for 1.5h. The dried material is crushed by a pulverizer and passed through a 100-mesh sieve to obtain modified powder.

[0081] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.03MPa, air inlet temperature is 82℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 120-mesh sieve and the sieve material is collected to obtain Poria cocos functional powder.

[0082] Comparative Example 1

[0083] A conventional method for preparing Astragalus powder by pulverization includes the following steps:

[0084] 1) Take Astragalus membranaceus slices, wash and remove impurities, dry at 55℃ for 2.5h until the moisture content is 4.5%, pulverize and pass through a 30-mesh sieve to obtain Astragalus membranaceus coarse powder;

[0085] 2) The coarse Astragalus powder obtained in step 1) is directly fed into an ultra-fine pulverizer for pulverization. The pulverization speed is set to 2800 r / min, the pulverization time is 30 min, and the feeding speed is 15 g / min. No ultra-low temperature ball milling, no air jet milling, and no low temperature classification are used to obtain ordinary Astragalus ultra-fine powder.

[0086] 3) Weigh out sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester in a mass ratio of 3:5:1:0.3:0.05, mix them evenly and add purified water to prepare a 9% modifier solution.

[0087] Add the Astragalus powder obtained in step 2) to the modifier solution. The total amount of modifier added is 9% of the mass of Astragalus ultrafine powder. Stir and disperse evenly. Treat the mixture with ultrasonic power of 250W and frequency of 20kHz for 20min. After ultrasonic treatment, place the mixture in a vacuum drying oven at 45℃ and dry for 1.5h. Crush the dried material with a pulverizer and pass it through a 100-mesh sieve to obtain modified powder.

[0088] 4) The modified powder obtained in step 3) is fed into a negative pressure low temperature microcapsule spray fluidized bed granulation equipment. The granulation parameters are set as follows: negative pressure is -0.03MPa, air inlet temperature is 80℃, air outlet temperature is 40℃, and granulation time is 40min. After granulation and cooling, the granules are passed through a 120-mesh sieve and the sieve material is collected to obtain Astragalus powder.

[0089] Comparative Example 2

[0090] A method for preparing Astragalus powder by modifying hydroxypropyl methylcellulose includes the following steps:

[0091] 1) Prepare Astragalus membranaceus crude powder using the same step 1) as in Example 1;

[0092] 2) Prepare Astragalus ultrafine powder in step 2) of Example 1;

[0093] 3) Hydroxypropyl methylcellulose was used to replace the compound modifier, and a modifier solution with a mass fraction of 9% was prepared. The remaining steps were the same as in Example 1.

[0094] 4) Perform negative pressure low temperature microcapsule spray fluidized bed granulation and sieving as in step 4) of Example 1 to obtain Astragalus powder.

[0095] Comparative Example 3

[0096] A method for preparing Astragalus powder without food-grade compound coating modification includes the following steps:

[0097] 1) Prepare Astragalus membranaceus crude powder using the same step 1) as in Example 1;

[0098] 2) Prepare Astragalus ultrafine powder in step 2) of Example 1;

[0099] 3) Without coating modification, the ultrafine powder is directly pulverized by a pulverizer and passed through a 100-mesh sieve to obtain modified powder;

[0100] 4) Perform negative pressure low temperature microcapsule spray fluidized bed granulation and sieving as in step 4) of Example 1 to obtain Astragalus powder.

[0101] Comparative Example 4

[0102] A conventional open-type spray drying method for preparing Astragalus powder includes the following steps:

[0103] 1) Prepare Astragalus membranaceus crude powder using the same step 1) as in Example 1;

[0104] 2) Prepare Astragalus ultrafine powder in step 2) of Example 1;

[0105] 3) Perform the same coating modification, drying, and pulverizing process as in step 3) of Example 1 to obtain the modified powder;

[0106] 4) The modified powder was dried using conventional open spray drying with an inlet air temperature of 160~180℃, an outlet air temperature of 80~90℃, an atomization pressure of 0.6~0.8MPa, and a feed rate of 15~20mL / min. There was no negative pressure and no microcapsule structure. After drying, it was passed through a 120-mesh sieve to obtain Astragalus powder.

[0107] The performance of the medicinal and edible herbal powders prepared in Examples 1-7 and Comparative Examples 1-4 was tested using the following methods:

[0108] 1) Particle size determination: A Mastersizer 2000 laser particle size analyzer was used to determine the particle size using a wet particle size distribution system. Before measurement, the samples were first ultrasonically dispersed in the ethanol phase. v10 D v50 D v90 D represents the particle size corresponding to a cumulative particle size distribution percentage of 10%, 50%, and 90% for the sample, respectively. [3,2] D represents the average diameter of the powder surface area. [4,3] The average diameter representing the powder volume, the span value Span, is calculated using the formula: Span = (D v90 -D v10 ) / D v50 .

[0109] 2) Water holding capacity: Accurately weigh 1g of powder into a beaker, add 20mL of deionized water, stir magnetically at 25℃ for 30min, centrifuge at 4000 r / min for 20min, remove the upper layer of water and record the sample mass.

[0110] ;

[0111] In the formula: m1 is the mass of the powder sample in g; m2 is the mass of the powder sample after absorbing water in g.

[0112] 3) Oil holding capacity: Accurately weigh 0.5g of powder into a centrifuge tube, add 10g of edible oil, let stand at 37℃ for 1 hour, centrifuge at 3000 r / min for 20 min, remove the upper layer of oil and record the sample mass.

[0113] ;

[0114] In the formula: m3 is the mass of the powder sample in g; m4 is the mass of the powder sample after standing and absorbing oil in g.

[0115] 4) Expansion force: Weigh 0.5g of powder into a 15mL graduated cylinder, gently tap the cylinder wall 5-8 times to smooth the powder surface and eliminate internal voids, and read the initial volume; transfer 10mL of deionized water to the sample, shake to mix, and let stand at room temperature for 24h, then read the volume of the sample after water absorption and expansion:

[0116] Expansion force ;

[0117] In the formula: m is the mass of the powder sample / g; V1 represents the initial volume of the powder sample / mL; V2 represents the volume of the powder sample after absorbing water and swelling / mL.

[0118] 5) Cold water solubility: Disperse 0.2g of powder in 20mL of deionized water, vortex for 5min, centrifuge at 3000 r / min for 15min, transfer the supernatant to a pre-weighed drying flask, and dry in an oven at 105℃ to constant weight. Calculate the cold water solubility:

[0119] Solubility / ;

[0120] In the formula: m0 is the mass of the powder sample (g); m1 is the mass of the drying flask (g); m2 is the total mass of the drying flask and the dried powder sample (g).

[0121] 6) Cold water dissolution time: 25℃, 100mL water, 200r / min stirring, record the time for complete dissolution.

[0122] 7) Bulk density and tapped density: Weigh 5 g of powder and add it to a 25 mL graduated cylinder, minimizing powder adhesion to the cylinder wall. Measure the volume occupied by the powder without compaction, and calculate the bulk density using the formula. Continuously tap the bottom of the graduated cylinder against the experimental platform until the powder volume inside the cylinder no longer changes.

[0123] ;

[0124] ;

[0125] In the formula: m is the mass of the powder in g; V1 is the volume of the powder in the graduated cylinder in mL; V2 is the final volume of the powder in the graduated cylinder after shaking in mL.

[0126] 8) Angle of repose: Fix the funnel vertically on an iron stand 3cm above the bottom of the funnel on a horizontal table. Place a transparent glass plate on the table. Let 3g of powder slide evenly through the funnel onto the glass plate, accumulating into a cone shape. Record the radius and height of the cone using calipers. Calculate the angle of repose using the formula:

[0127] ;

[0128] In the formula: H is the height of the cone formed by the powder in cm; R is the radius of the base circle of the cone in cm.

[0129] 9) Slip Angle: Pour 10 g of powder onto one fixed end of a glass plate, keeping the initial position of the material constant each time. Slowly tilt the glass plate until the powder begins to slide. Use calipers to record the length of the plane and the vertical distance from the top to the table. The slip angle is calculated using the formula:

[0130] ;

[0131] In the formula: H is the vertical distance from the initial position of the powder to the tabletop / cm; L is the length of the glass plate / cm.

[0132] 10) Retention rate of active ingredients: Using the raw material as a control, the content of polysaccharides / saponins was determined and the retention rate was calculated.

[0133] 11) Moisture absorption rate: Calculate the moisture absorption rate after placing the product at 25℃ and RH75% for 24 hours.

[0134] 12) Water activity: directly measured using a water activity meter at 25℃.

[0135] 13) Antioxidant activity: Characterized by the DPPH free radical scavenging rate of the powder. The test results are shown in Table 1-3.

[0136] Table 1. Particle size test results of medicinal and edible herbal powders in Examples 1-7 and Comparative Examples 1-4

[0137] sample <![CDATA[D v10 (μm)]]> <![CDATA[D v50 (μm)]]> <![CDATA[D v90 (μm)]]> <![CDATA[D [3,2] (μm)]]> <![CDATA[D [4,3] (μm)]]> Span(μm) Example 1 5.24 9.21 36.82 11.43 19.61 1.77 Example 2 6.85 10.32 39.34 11.57 20.05 1.89 Example 3 5.38 9.72 38.64 11.49 19.88 1.90 Example 4 7.05 11.24 41.44 11.79 21.98 2.10 Example 5 6.93 10.81 40.31 11.58 20.13 2.00 Example 6 5.70 9.94 37.11 11.27 19.44 1.96 Example 7 5.27 8.96 35.33 11.06 18.72 1.68 Comparative Example 1 10.11 32.66 60.67 14.67 28.28 2.98 Comparative Example 2 7.89 11.94 43.22 12.87 22.52 2.43 Comparative Example 3 8.98 12.48 45.87 12.22 27.98 2.44 Comparative Example 4 7.77 11.86 42.98 12.01 23.01 2.41

[0138] Table 2. Test results of quality characteristics of medicinal and edible herbal powders from Examples 1-7 and Comparative Examples 1-4

[0139] sample Water holding capacity (g / g) Oil holding capacity (g / g) Expansion force (mL / g) Cold water solubility (%) Dissolution time in cold water (s) Example 1 2.94 1.74 3.92 90.5 28 Example 2 2.75 1.62 3.74 86.2 33 Example 3 2.88 1.72 3.64 90.1 26 Example 4 2.65 1.54 3.44 89.3 30 Example 5 2.50 1.41 3.31 87.5 32 Example 6 2.60 1.44 3.51 88.6 29 Example 7 2.67 1.46 3.53 89.7 27 Comparative Example 1 2.01 1.06 1.67 61.4 128 Comparative Example 2 1.89 0.94 2.22 72.5 79 Comparative Example 3 1.18 1.28 1.87 41.6 280 Comparative Example 4 1.77 1.16 2.18 43.2 210

[0140] Table 3. Test results of processing characteristics of medicinal and edible herbal powders from Examples 1-7 and Comparative Examples 1-4

[0141] sample Bulk density (g / mL) Tap density (g / mL) Angle of repose (°) Slip angle (°) Active ingredient retention rate (%) Moisture absorption rate (%) Water activity Aw DPPH removal rate (%) Example 1 0.476 0.631 36.82 26.34 93.1 4.2 0.26 82.3 Example 2 0.377 0.522 39.34 29.33 91.2 4.5 0.27 81.5 Example 3 0.461 0.593 38.64 28.45 92.9 3.9 0.25 83.1 Example 4 0.452 0.571 41.44 21.67 92.6 4.6 0.28 80.7 Example 5 0.403 0.482 40.31 20.77 91.8 4.3 0.26 81.2 Example 6 0.482 0.507 37.11 27.86 92.3 4.1 0.25 82.6 Example 7 0.497 0.666 35.33 25.36 93.2 3.7 0.24 83.5 Comparative Example 1 0.111 0.423 60.67 40.17 82.3 8.9 0.42 65.7 Comparative Example 2 0.192 0.342 43.22 32.18 76.8 7.1 0.38 68.2 Comparative Example 3 0.342 0.478 45.87 34.07 90.8 12.4 0.48 83.5 Comparative Example 4 0.271 0.419 42.98 31.89 88.7 11.8 0.46 82.8

[0142] As shown in Tables 1-3, this invention targets high-viscosity, high-polysaccharide, difficult-to-dissolve, and difficult-to-pulverize medicinal and edible herbs such as Astragalus membranaceus, Lycium barbarum, Dioscorea opposita, Polygonatum sibiricum, and Poria cocos. It employs a combined ultra-low temperature ball milling and airflow pulverization technology to achieve ultra-fine particle size reduction, significantly decreasing the particle size D. v50 All particles are less than 12 μm in size, indicating a uniform particle size distribution. The span value represents the width of the particle size distribution; the smaller the span value, the more uniform the distribution. Correspondingly, the span values ​​of Examples 1-7 are all reduced to 2.10 µm, indicating that the powder can maintain a good concentration and uniformity of particle size.

[0143] Water-holding capacity and oil-holding capacity are indicators that measure the ability of powder samples to retain water and oil under external centrifugal force, and they are crucial to the processing characteristics of functional powders. Expansion force is a key indicator for measuring the quality characteristics of dietary fiber in food. The greater the expansion force, the better the stability and suspension properties of the powder after dissolving in water. As shown in Table 2, the water-holding capacity, oil-holding capacity, and expansion force of Examples 1-7 reached 2.50 g / g, 1.41 g / g, and 3.31 mL / g, respectively, all superior to those of Comparative Examples 1-4, indicating that the functional powders prepared by the process used in this invention have good processing characteristics.

[0144] Solubility typically reflects food quality and is related to the digestion and absorption of components in food. Its magnitude is mainly related to the contact area between the powder and the aqueous solution. Instantaneous functional powders were prepared by surface hydrophilic modification of powders using food-grade compound modifiers and granulation via negative pressure low-temperature microcapsule spray fluidized bed. The cold water solubility of Examples 1-7 was greater than 85%, and the dissolution time was less than 33 seconds, representing a more than twofold increase in dissolution rate compared to Comparative Examples 1-3.

[0145] Bulk density and tap density are important indicators for characterizing the filling properties of materials. Powders with higher density are more conducive to tableting and low-cost packaging and transportation. The bulk density of Examples 1-7 ranges from 0.377 g / mL to 0.497 g / mL, and the tap density ranges from 0.482 g / mL to 0.666 g / mL, indicating that the functional powder prepared by the process used in this invention has excellent filling properties, which is significantly better than the powders obtained by the single process in Comparative Examples 1-4.

[0146] The angle of repose and the slip angle are commonly used to reflect the flowability of powders; the smaller the value, the better the flowability. The angle of repose of Examples 1-7 ranges from 35.33° to 41.44°, and the slip angle ranges from 20.77° to 29.33°, indicating that the functional powders prepared by the process used in this invention have excellent flowability, significantly better than the powders obtained by a single process in Comparative Examples 1-4.

[0147] The retention rate of active ingredients is an important indicator for evaluating the quality characteristics of functional powders. This invention uses raw materials as a control to determine the polysaccharide / saponin content and calculate the retention rate. The active ingredient retention rates of Examples 1-7 are over 90%. Furthermore, the functional powders prepared by the process employed in this invention have low hygroscopicity, low water activity, and high antioxidant activity.

[0148] This invention uses water as the medium throughout the process and does not use any organic solvents, which meets the standards for green food production. It is the first to adopt the coupling of ultrasonic molecular coating and negative pressure microcapsule granulation of the sodium octenyl succinate starch composite system, which solves the technical problems of poor solubility, poor flowability, easy agglomeration and poor processing suitability of polysaccharide powders that have long existed in the industry.

[0149] 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 principle 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 green preparation method for functional powders of medicinal and edible herbs, characterized in that, Includes the following steps: 1) Select medicinal and edible herbs, clean and remove impurities, then treat with low-temperature plasma, add cellulase for enzymatic hydrolysis, dry to a moisture content of no more than 8%, and pulverize and sieve to obtain coarse powder; 2) The pretreated coarse powder is placed in an ultra-low temperature ball mill and ball milled using a gradient temperature change method to obtain primary ultrafine powder; then the primary ultrafine powder is subjected to air jet milling and classified by a low temperature air jet classifier to obtain ultrafine powder. 3) Prepare a food-grade modifier solution, add the ultrafine powder obtained in step 2) to the modifier solution, and after ultrasonic modification, vacuum dry, pulverize and sieve to obtain modified ultrafine powder; 4) The modified ultrafine powder obtained in step 3) is placed in a negative pressure low temperature microcapsule spray fluidized bed for granulation, cooled and then sieved to obtain an instant functional powder.

2. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 1), the medicinal and edible herbs are selected from one or more of the following: Astragalus membranaceus, Lycium barbarum, Dioscorea opposita, Polygonatum sibiricum, and Poria cocos.

3. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 1), the low-temperature plasma treatment power is 90~115W and the treatment time is 70~100s.

4. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 1), the amount of cellulase added is 0.1% to 0.3% of the dry basis weight of the medicinal and edible herbs, the enzymatic hydrolysis temperature is 40 to 44°C, and the enzymatic hydrolysis time is 25 to 35 minutes.

5. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 2), the specific process of gradient temperature ball milling is as follows: first, ball milling is carried out at -120℃ for 0.4~0.7h, then at -80℃ for 0.5~0.6h, and finally at -50℃ for 0.4~0.6h, with a total ball milling time of 1.2~1.8h; the airflow pressure of the airflow pulverizer is 0.6~0.8MPa.

6. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 2), the ball-to-material ratio of the cryogenic ball mill is 10:1 to 15:1, and the ball milling speed is 300 to 400 r / min; the feed rate of the air jet mill is 10 to 20 g / min.

7. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 3), the food-grade modifier is a compound system of sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide and polyglycerol fatty acid ester; the mass concentration of the modifier solution is 5%~10%.

8. The green preparation method of functional powder of medicinal and edible herbs according to claim 7, characterized in that, In step 3), the mass ratio of sodium octenyl succinate starch, maltodextrin, gum arabic, soybean polysaccharide, and polyglycerol fatty acid ester is 3:5:1:0.3:0.

05.

9. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 3), the total amount of modifier added is 8% to 9% of the mass of the ultrafine powder; the ultrasonic treatment power is 220 to 270W, the frequency is 20 to 22kHz, and the time is 18 to 25min.

10. The green preparation method of functional powder of medicinal and edible herbs according to claim 1, characterized in that, In step 4), the negative pressure low temperature microcapsule spray fluidized bed granulation conditions are: negative pressure -0.025~-0.035MPa, inlet air temperature 75~88℃, outlet air temperature 38~42℃, and granulation time 35~40min.

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