American ginseng powder and preparation method and application thereof

Abstract

The present invention provides a kind of American ginseng powder and its preparation method and application, belonging to the technical field of pharmaceutical preparations. A method for preparing American ginseng powder comprises the following steps: mixing American ginseng powder with water to form granules to obtain granules with a water content of 25% to 33wt%; subjecting the granules to ultrasonic enhanced supercritical carbon dioxide treatment to obtain treated granules; and subjecting the treated granules to microwave sterilization. The technical solution provided by the present invention solves the problems of the difficulty in sterilizing traditional Chinese medicine raw materials and the difficulty in using preparations, and greatly improves the processing performance of the raw medicine American ginseng, and can be directly applied to the production of various preparations without adding any auxiliary materials or processing aids.

Description

Technical Field

[0001] The invention belongs to the technical field of pharmaceutical preparations, and particularly relates to American ginseng powder and a preparation method and application thereof. Background Art

[0002] American ginseng refers to the dried rhizome of Panax quinquefolium L., a plant of the Araliaceae family. It is also known as American ginseng, American ginseng, etc. It is native to Canada and the central and eastern parts of America. It was later introduced to Europe and China for cultivation. The production areas of American ginseng in my country are mainly concentrated in the Northeast, Shandong and Beijing. American ginseng is cool in nature, sweet and slightly bitter in taste. It has the effects of nourishing yin and replenishing qi, clearing away heat, moistening dryness and promoting body fluid. It is mainly used to treat insufficient qi or spleen and stomach dampness and heat deficiency, and has obvious effects on internal heat, dry mouth and throat. Modern biomedical technology research has proved that American ginseng has multiple effects such as anti-oxidation, anti-fatigue, lowering blood sugar and improving immunity. It is one of the commonly used precious drugs in clinical practice, so it is often used as an important raw material for medicine and food and daily health care.

[0003] American ginseng is included in the "Chinese Pharmacopoeia" as a legal Chinese medicinal material. On January 6, 2020, the National Health Commission and the State Administration for Market Regulation jointly issued the "Notice on Piloting the Management of 9 Substances Including Codonopsis in Accordance with Traditional Management of Substances That Are Both Food and Chinese Medicinal Materials", to pilot the production and operation of 9 edible and medicinal substances including American ginseng in accordance with the traditional management of edible and medicinal substances. It can be foreseen that with the gradual relaxation of policies, American ginseng will be more widely and deeply used in the field of health products, and the market potential is huge.

[0004] The difficulty in sterilization and preparation of traditional Chinese medicinal materials for direct preparation is a long-standing problem in the health care and pharmaceutical industry. Since the initial raw medicinal materials have a large microbial base, they generally require high-intensity sterilization treatment through moist heat sterilization, irradiation sterilization and other technologies. However, moist heat sterilization can easily lead to the inactivation of heat-sensitive effective ingredients. For example, the American ginseng used in this method will suffer serious losses of saponin effective ingredients due to moist heat sterilization treatment. Irradiation sterilization has always been controversial due to issues regarding the safety of oral administration of the treated materials.

[0005] At present, the market application of traditional Chinese medicinal materials such as American ginseng mostly adopts the processing methods of combining raw decoction pieces and substitute teas with brewing, decocting, and making soup, but it is not convenient to take. Existing powder products such as ultrafine powder and broken wall powder can be eaten directly in theory, but due to the large surface area and adhesion to the oral wall when wet, it is actually difficult to chew and the taking experience is very poor. Generally, it is still used in the form of brewing. In addition, there are no microbial requirements for decoction ultrafine powder products, and the products have not been sterilized. There are certain health and safety risks when eaten directly.

[0006] In addition, as processed products of medical health products and various types of food, due to the poor processing properties of traditional crude drugs such as fluidity and plasticity, American ginseng is generally used after extraction to obtain extracts or extract powders, but after extraction, purification, concentration and other refined processing, the extracts often lose the original flavor of the original drugs, the flavor substances are greatly reduced, and the functional substances are inevitably lost to a certain extent. There are a few preparations that use crude drug raw materials directly as medicine. Due to poor processing properties, a large amount of various types of auxiliary materials with different functions are often added to improve them in order to successfully shape the preparations. The content of crude drugs in the finished products is often very small, mainly auxiliary materials. The large amount of non-functional substances introduced makes the product dosage doubled. In addition, there is also the problem of difficulty in sterilization when crude drugs are used directly as medicine. Due to the large base of microorganisms, high-intensity treatment is often required to completely sterilize, which can easily lead to the deterioration and denaturation of materials, the loss of flavor substances and the inactivation of functional ingredients. There are food products such as American ginseng candy and American ginseng preserves on the market. American ginseng is directly sliced ​​or crushed into granular powder and added to the products. However, these products still need to be mixed with syrup and then boiled at high temperature, or a high proportion of syrup is added. After the sugar and the flavor substances in the American ginseng undergo a series of reactions such as Maillard reaction under the action of water, the original flavor of the American ginseng is changed, and the products cannot fully restore the natural flavor of the American ginseng.

[0007] At present, supercritical technology modification is mostly applied to special materials, composite materials, ultrafine powders, carrier frameworks, new crystal crystallization, etc., and there are few reports on the research and application of modifying the performance of Chinese medicinal materials. The application of supercritical technology in the fields of medicine and food is mostly still in the extraction of target ingredients. Other chemical methods of modification or the use of spray drying and freeze drying technology are often used to prepare excipients with small particle size, good fluidity, and suitable for direct tableting. Summary of the invention

[0008] In view of this, the purpose of the present invention is to provide an American ginseng powder, which solves the problems of difficulty in sterilizing traditional Chinese medicine raw materials and difficulty in using them in preparations, and greatly improves the processing performance of the raw material American ginseng, and can be directly used in the production of various preparations without adding any excipients or processing aids.

[0009] The present invention provides a method for preparing American ginseng powder, comprising the following steps:

[0010] Mixing American ginseng powder with water to form granules to obtain granules with a water content of 25% to 33% by weight;

[0011] The particles having a water content of 25% to 33wt% are subjected to ultrasonic enhanced supercritical carbon dioxide treatment to obtain treated particles;

[0012] The treated particles are sterilized by microwave.

[0013] Preferably, the conditions for the ultrasonic enhanced supercritical carbon dioxide treatment are: pressure: 30-35 MPa, temperature: 50-55° C., ultrasonic frequency: 20-25 KHz, and treatment time: 45-90 min.

[0014] Preferably, the microwave frequency during microwave sterilization is 2440-2500 MHz, and the sterilization time is 4-7 minutes;

[0015] Or the microwave frequency is 902-928 MHz, and the sterilization time is 12-20 minutes.

[0016] Preferably, the American ginseng powder is a fine powder of 80 to 120 meshes.

[0017] Preferably, the particle size of the particles having a water content of 25% to 33 wt% is 4 to 6 mm.

[0018] Preferably, the loose particles obtained after microwave sterilization are crushed and passed through a 60-mesh sieve, and the sieved material is collected to obtain American ginseng powder.

[0019] The invention provides American ginseng powder obtained by the preparation method.

[0020] The invention provides application of the American ginseng powder in preparing American ginseng products.

[0021] Preferably, the American ginseng product includes at least one of the following products: American ginseng traditional Chinese medicine preparations, American ginseng health products and American ginseng food.

[0022] Preferably, the dosage form of the American ginseng product includes at least one of the following: granules, powders, powders, capsules, teas and tablets.

[0023] The invention provides a method for preparing American ginseng powder, comprising the following steps: mixing American ginseng powder with water to form granules to obtain granules with a water content of 25% to 33wt%; subjecting the granules with a water content of 25% to 33wt% to ultrasonically enhanced supercritical carbon dioxide treatment to obtain treated granules; and subjecting the treated granules to microwave sterilization. The present invention mixes American ginseng powder and water to form granules, so that the material can be treated evenly during the ultrasonic enhanced supercritical treatment process, and the material can be prevented from being bonded during the treatment process, which causes the ultrasonic wave or supercritical carbon dioxide fluid to be unable to penetrate and act on the internal material, so that the treatment cannot achieve the expected effect. At the same time, the granules contain a certain amount of water, which is conducive to the dissolution and diffusion of water-soluble components such as plant colloids, sticky polysaccharides, and sticky proteins existing inside the cells to the outside under the ultrasonic supercritical action. After stopping the ultrasound and unloading the pressure, these substances are precipitated and adhered to the granules. After drying, these substances can be used as natural adhesives in a humidity-controlled environment. In addition, more importantly, the supercritical carbon dioxide treatment can modify the material, especially the ultrasonic enhanced supercritical carbon dioxide treatment of the present method can further enhance the penetration of carbon dioxide, and can act more fully and evenly on the inside of the material. In the rapid pressure relief process, carbon dioxide is rapidly converted from the original high-compression supercritical fluid state to a gas state, and rapidly flows out of the material. It expands and overflows, playing a similar role to puffing, which is similar to a deeper, more complete, more uniform, and more delicate microscopic puffing. The result of the action makes a profound change in the structure of the material. After the action, the interior of the material is filled with the gaps left after the expansion and overflow of carbon dioxide, and the interior presents a loose and porous structure. The spatial volume of the material particles becomes larger, thereby enhancing the compressibility and plasticity of the material. After the action, the material particles are also puffed into a spherical shape tending to regularity, which enhances the fluidity and filling properties of the particles. These changes can greatly enhance the preparation processing performance of American ginseng powder, so that it can be used alone without adding other auxiliary materials. Preparations such as granules, powders, capsules, and tablets have been produced, subverting the traditional preparation technology route that crude drug raw material preparations must add a large amount of auxiliary materials that impart different types of processing properties to complete the plastic preparation. It is an innovative technical solution for crude drug preparations. In addition, the particles contain a certain amount of water, which improves the sterilization effect to a certain extent during microwave sterilization. At the same time, the present invention utilizes ultrasound to strengthen supercritical carbon dioxide treatment and microwave sterilization to achieve the dual sterilization purpose. Most microorganisms are killed in advance by ultrasonic supercritical treatment, which can greatly reduce the intensity requirements of subsequent microwave treatment. The relatively low-intensity microwave treatment can achieve both sterilization effect and material denaturation caused by high-intensity microwave treatment, thereby causing the loss of flavor components and functional components, thereby causing material degradation and reducing the quality of the finished product. The method provided by the present invention has a strong correlation between the processing steps, and can achieve multiple effects at the same time. The specific method is developed for the material properties of American ginseng crude drugs, has strong pertinence, and provides a guarantee for the preparation of American ginseng pharmaceutical products.

[0024] At the same time, the present invention is based on the comprehensive effects of treatment conditions such as water, ultrasound, supercritical carbon dioxide and microwave sterilization, which can greatly enhance the processing performance of American ginseng materials. It belongs to physical method modification, specifically the comprehensive effects of treatment conditions such as water, ultrasound, supercritical carbon dioxide, etc., which is different from chemical method modification or other comprehensive modification measures that require the participation of chemical solvents, catalysts, etc. The introduction of chemical substances may cause material contamination or the production of some toxic by-products in the reaction, affecting food safety. This method does not need to introduce other chemical substances and has no hidden dangers in this regard. The water and carbon dioxide used in production are non-toxic and clean substances. It is a green and safe technical solution suitable for the processing of human internal products.

[0025] The present invention provides American ginseng powder obtained by the preparation method. The American ginseng powder prepared by the present invention not only ensures that the crude drug meets the sterilization requirements but also completely retains the natural flavor substances and functional substances of American ginseng. The American ginseng powder can be directly processed for preparation production without adding other auxiliary materials. Especially when used in tablet production, the finished product can obtain more beneficial effects in terms of food / taking experience than other dosage forms: because the tablet contains only a single ingredient of American ginseng, it can be directly swallowed or chewed and eaten. The modification and compression molding of the raw materials also improve the loose, rough, sticky and medicinal residue-like bad taste of the original raw material powder, and replace it with a neat, hard and crisp chewing taste. The refreshing and non-sticky chewing experience and the refreshing and sweet natural flavor of American ginseng meet the modern consumers' demand for the ultimate experience of healthy internal products, especially functional foods and health foods, with natural ingredients, clean labels (that is, as few non-functional ingredients as possible, excipients, additives, etc.), highly restored natural flavors, complete retention of functional ingredients, good taste, convenient snack-like and even lazy eating. It is an innovative product that meets the development trend of healthy products. It has both technological content and returns to nature, unifying the seemingly contradictory product experience needs of the new era. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The process flow chart of American ginseng powder and its preparation;

[0027] Figure 2 American ginseng slices prepared by the present invention;

[0028] Figure 3 To process the first 80 mesh American ginseng powder;

[0029] Figure 4 It is 80 mesh American ginseng powder after processing. DETAILED DESCRIPTION

[0030] The present invention provides a method for preparing American ginseng powder, comprising the following steps:

[0031] Mixing American ginseng powder with water to form granules to obtain granules with a water content of 25% to 33% by weight;

[0032] The particles having a water content of 25% to 33% by weight are subjected to ultrasonic enhanced supercritical carbon dioxide treatment to obtain treated particles;

[0033] The treated particles were sterilized by microwave.

[0034] The invention mixes American ginseng powder with water to form granules, so as to obtain granules with a water content of 25% to 33wt%.

[0035] In the present invention, the preparation method of American ginseng powder is preferably obtained by sieving after crushing the American ginseng raw material. The American ginseng raw material preferably includes dried whole American ginseng, broken American ginseng, American ginseng slices or American ginseng coarse particles. The present invention has no special restrictions on the crushing method, and the crushing method well known in the art can be used. After the crushing, it is preferably passed through a sieve of 80 to 120 mesh, and the sieve is collected to obtain fine powder. The American ginseng powder is preferably a fine powder of 80 to 120 mesh, and more preferably a fine powder of 100 mesh.

[0036] In the present invention, the amount of water added is preferably 30% to 40% by mass of the American ginseng powder, and more preferably 35%. The present invention has no special restrictions on the granulation method, and the granulation method known in the art can be used. In an embodiment of the present invention, the granulation is completed by a granulator, and the screen plate of the granulator is preferably 4 to 6 mm, and more preferably 5 mm. The particle size and water content of the particles and the hardness of the raw materials are factors that affect the subsequent ultrasonic enhanced supercritical carbon dioxide treatment effect. The material is too hard, dense, and the crushing particle size is too large, which is easy to act incompletely, that is, carbon dioxide cannot penetrate the center of the particles, affecting the modification and sterilization effect; and when the particle size is too small, it is easy to form "channel flow", that is, due to the small particle size, a large amount of viscous soluble substances are precipitated under the action of ultrasonic supercritical CO2, resulting in local adhesion of the material, forming some thick lumps, thereby affecting the supercritical fluid acting on the inside of the lumps. The present invention ensures that the particles obtained after granulation have a certain looseness and support by controlling the water content and particle size of the particles, and also ensures the ultrasonic enhanced supercritical carbon dioxide treatment effect.

[0037] After obtaining particles with a water content of 25% to 33wt%, the present invention performs ultrasonic enhanced supercritical carbon dioxide treatment on the particles with a water content of 25% to 33wt% to obtain treated particles.

[0038] In the present invention, the conditions for the ultrasonic enhanced supercritical carbon dioxide treatment are preferably: pressure: 30-35MPa, temperature: 50-55°C, ultrasonic frequency: 20-25KHz, and treatment time: 45-90min; more preferably, pressure: 32-34MPa, temperature: 51-54°C, ultrasonic frequency: 21-24KHz, and treatment time: 50-85min, and most preferably, pressure: 33MPa, temperature: 52°C, ultrasonic frequency: 23KHz, and treatment time: 65min. The ultrasonic enhanced supercritical carbon dioxide treatment plays two roles. One is that a portion of microorganisms are killed by treating in an ultrasonic, osmotic high pressure, anaerobic environment for a period of time, and then the pressure is quickly released. The rapid change in air pressure causes the microorganisms to swell, rupture and inactivate, thereby further reducing the base number of microorganisms in the material. The other role is that under the action of ultrasonic supercritical, the moisture in the particles is conducive to the mixed dissolution and diffusion of water-soluble components such as plant gum, sticky polysaccharides, and sticky proteins existing inside the cells to the outside of the particles. After stopping the ultrasound and releasing the pressure, these substances precipitate and adhere to the particles. After drying, these substances can be used as natural adhesives in a humidity-controlled environment. At the same time, the microstructure of the material particles is changed after the ultrasonic supercritical action, and the plasticity, compressibility, fluidity, filling property, etc. are enhanced, thereby enhancing the preparation effects such as granulation and tableting.

[0039] After obtaining the treated particles, the present invention performs microwave sterilization on the treated particles.

[0040] In the present invention, the microwave frequency during microwave sterilization is preferably 2440-2500MHz, and the sterilization time is preferably 4-7min, or the microwave frequency is preferably 902-928MHz, and the sterilization time is preferably 12-20min. The present invention first kills most microorganisms in advance through ultrasonic supercritical treatment, which can greatly reduce the intensity requirements of subsequent microwave treatment. The sterilization effect can be achieved through relatively low-intensity microwave treatment, thereby avoiding the material denaturation caused by high-intensity microwave treatment, and then causing the loss of flavor components and functional components, thereby causing the deterioration of the material and reducing the quality of the finished product. At the same time, in addition to the sterilization effect, the microwave sterilization also plays a drying role, removing excess water in the particles, and finally making the material moisture meet the standard requirements. Keeping a certain amount of moisture in the particles can also enhance the sterilization effect of the material during the microwave treatment process, so that the method can achieve the purpose of setting a lower microwave intensity to achieve the terminal sterilization effect. Compared with the traditional process, it avoids the loss of material flavor substances and functional substances caused by high-intensity and long-term heat treatment, so it improves the product quality, and at the same time can shorten the process flow, save processing time and energy consumption, and reduce production costs; at the same time, short-term microwave sterilization can also achieve the beneficial effect of not destroying the material performance and avoiding the denaturation loss of flavor substances and functional substances in high-intensity and long-term microwave treatment. Therefore, the process flow and parameter settings of this method are closely linked, and the overall method process is ingenious.

[0041] In the present invention, after the microwave sterilization, the obtained loose particles are preferably crushed and passed through a 60-mesh sieve, and the sieve residues are collected to obtain American ginseng powder.

[0042] The invention provides American ginseng powder obtained by the preparation method.

[0043] In the present invention, the American ginseng powder prepared by the above method of the present invention not only meets the sterilization requirements of crude drugs, but also retains the active ingredients of American ginseng to the maximum extent, and has good preparation properties. It can directly prepare various types of preparations without adding any auxiliary materials or processing adjuvants, which subverts the traditional preparation technology route that crude drug raw material preparations must add a large amount of auxiliary materials that impart different types of processing properties to complete the shaping preparation. It is an innovative technical solution for crude drug preparations.

[0044] The invention provides application of the American ginseng powder in preparing American ginseng products.

[0045] In the present invention, the American ginseng product preferably includes at least one of the following products: American ginseng traditional Chinese medicine preparations, American ginseng health products and American ginseng food.

[0046] The dosage form of the American ginseng product preferably includes at least one of the following: granules, powders, powders, capsules, teas and tablets. The preparation method of the American ginseng product preferably uses conventional preparation processes to prepare American ginseng products of different dosage forms without adding auxiliary materials or other additives to American ginseng powder.

[0047] The American ginseng powder provided by the present invention and its preparation method and application are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0048] Example 1

[0049] Take the dried whole American ginseng slices, crush them through a 120-mesh sieve, take a part of the powder and add 40% water by mass to mix evenly, use an extrusion granulator to pass through a 6mm sieve plate for granulation, and obtain relatively loose particles. Since the raw material itself contains a certain amount of moisture, and the material loses some moisture after extrusion granulation, the average moisture content of the material after granulation is about 31%. Take a part of the obtained particles and put them into the ultrasonic enhanced supercritical carbon dioxide treatment device. The process parameters are set and controlled as follows: pressure: 35MPa, temperature: 55℃, ultrasonic frequency: 25KHz, treatment time: 50min. After the time is up, the system is depressurized and carbon dioxide is recovered. Take out the treated particles, and it can be seen that the particle volume is significantly increased and the state becomes looser. The particles are flattened and placed in a box-type microwave sterilization equipment, and treated for 6min under the condition of a microwave frequency of 2450MHz to obtain materials with moisture and microorganisms that meet the standards (moisture ≤9%, microbial standards refer to the requirements of domestic health food regulations). The materials are discharged under a controlled clean environment, and the subsequent processes are carried out in a 100,000-level clean workshop. The loose particles after microwave treatment were taken and crushed through a 60-mesh sieve to obtain American ginseng powder with good preparation processing performance.

[0050] Comparative Example 1

[0051] Take a portion of the particles obtained by crushing and sieving the whole American ginseng and adding water in Example 1, and load it into a supercritical carbon dioxide extraction system without an ultrasonic enhancement device. Set and control the process parameters: pressure: 35 MPa, temperature: 55°C, maintain the pressure for 50 minutes after boosting, and after the time is up, release the pressure and recover the carbon dioxide, take out the treated particles, and perform subsequent treatment as in Example 1.

[0052] Comparative Example 2

[0053] A portion of the particles obtained by crushing and sieving the whole American ginseng and adding water in Example 1 were taken and loaded into an ultrasonic enhanced supercritical carbon dioxide treatment device. Except for setting the ultrasonic frequency to 35KHz, the other ultrasonic supercritical treatment conditions and subsequent treatment were the same as in Example 1.

[0054] Comparative Example 3

[0055] Take a portion of the American ginseng powder after the whole American ginseng is crushed and sieved in Example 1, add 80% of water by weight and mix evenly, use an extrusion granulator to pass through a 6mm sieve plate for granulation, and obtain relatively solid granules. The average moisture content of the material after granulation is about 73%, and the subsequent treatment is the same as Example 1. During the treatment process, it was found that the surface of the particles discharged after ultrasonic supercritical treatment had a certain viscosity, and some local materials showed adhesion and agglomeration.

[0056] Example 2

[0057] Powder preparation performance test experiment

[0058] The American ginseng powder obtained after the whole raw material of Example 1 was crushed and sieved (American ginseng powder before treatment), and the American ginseng powder obtained after all the treatments of Example 1, Comparative Example 1, Comparative Example 2, and Comparative Example 3 were taken, and various index parameters reflecting the processing performance of the powder were measured and calculated using a powder property measuring instrument. The results are shown in Table 1:

[0059] Table 1

[0060]

[0061]

[0062] Note: Angle of repose (°), wipe angle (°), flow rate (g / s), bulk density (g / mL), tap density (g / mL) are the average values ​​of three measurements according to the standard method. Compression (%): Compression = (1-bulk density / tapped density) × 100%. Uniformity: According to the particle size distribution measurement results, uniformity = D60 / D10. Flowability index: automatically calculated by the system based on the above measurement and calculation results.

[0063] From Table 1, we can see that:

[0064] 1. The angle of repose reflects the size of the dynamic friction coefficient between powder particles. The larger the angle of repose, the larger the friction coefficient and the worse the fluidity of the powder particles. Generally, the angle of repose <40° is required for the powder fluidity to meet the production requirements. The angle of repose <35° is rated as good. The angle of repose of the American ginseng powder before treatment and in comparative example 3 is greater than 40°, and the angle of repose of the American ginseng powder in comparative examples 1 and 2 is close to 40°. The angle of repose of the American ginseng powder in Example 1 is the smallest and is less than 35°, and the fluidity is rated as good.

[0065] 2. The smoothing angle reflects the static friction coefficient between powder particles. The larger the smoothing angle, the greater the friction coefficient and the worse the fluidity of the powder particles. Among the five samples, the smoothing angle of the American ginseng powder in Example 1 is the smallest.

[0066] 3. Flow rate is also a parameter that reflects the fluidity of powder. The greater the flow rate, the better the fluidity. Among the five samples, the flow rate of American ginseng powder in Example 1 is the largest.

[0067] 4. Loose density, tap density and compression reflect the compressibility and filling performance of powder particles. The smaller the compression, the stronger the filling property. It is generally believed that when the compression is between 15% and 25%, the powder can meet the requirements of direct tableting. Among the five samples, the American ginseng powder in Example 1 has the smallest compression, and its value is in the range of 15% to 25%, showing the potential for direct tableting.

[0068] 5. Uniformity reflects the uniformity of powder particles. The uniformity is generally greater than 1. The closer to 1, the better. Powder preparations with good uniformity have small differences in loading amounts. Among the five samples, the uniformity of the American ginseng powder in the example is closest to 1.

[0069] 6. The fluidity index is a comprehensive parameter that reflects the fluidity of powder from a more comprehensive perspective. The higher the value, the better the fluidity. Among the five samples, the fluidity index of the American ginseng powder in the example is the highest.

[0070] The above index parameters all reflect that the preparation processing performance of the American ginseng powder in the embodiment of the present method is good, and the above processing performance indicators of the American ginseng powder before treatment and the American ginseng powder in comparative example 1 are significantly enhanced, that is, the processing performance of the American ginseng powder after ultrasonic supercritical treatment by the present method is better than that of the American ginseng powder treated with ordinary crushing and the American ginseng powder without ultrasonic supercritical treatment.

[0071] In addition, the above processing performance indicators of the American ginseng powder in implementation 1 of the present method are also better than those of the American ginseng powder in Examples 2 and 3 whose processing conditions exceed the limit. In Example 2, the excessive ultrasonic frequency makes the cavitation effect too strong, which weakens the permeability of the supercritical fluid, and the incomplete penetration leads to weakened effect; in Example 3, the excessive amount of water added leads to relatively solid particles, which is also not conducive to the supercritical fluid penetrating into the interior of the particles for action. In addition, too high a moisture content will also change the characteristics of the supercritical fluid, enhancing the solubility of water-soluble substances, but weakening the permeability of the fluid, which is likely to cause a large amount of sticky substances to precipitate on the surface of the particles but cannot be dissolved and diffused into the supercritical fluid outside the particles in time, forming a layer of mucous film on the surface of the particles, and making it easy for the particles to stick to each other and agglomerate, thereby further hindering the supercritical fluid from penetrating into the interior of the particles for action. Therefore, the material after treatment presents a state of uneven modification as a whole, which is specifically manifested in the poor uniformity of the American ginseng powder in Example 3.

[0072] Example 3

[0073] Tablet Compression Test

[0074] The five samples involved in Example 2 were taken separately, and no auxiliary materials were added. The powder direct tablet press was used to try to compress the tablets by debugging parameters. Among them, the American ginseng powder before treatment and the American ginseng powder of Comparative Examples 1 to 3 were not stable due to poor comprehensive properties such as fluidity, compressibility, and uniformity. After debugging, the American ginseng powder of Example 1 was compressed, and the pressed plain tablets (specification: 0.25g / tablet) were taken to measure a series of indicators according to the technical requirements of tablet products. The results are shown in Table 2.

[0075] Table 2

[0076]

[0077] It can be seen that the tablets directly pressed out of the American ginseng powder treated by this method without adding any auxiliary materials have product dosage form-related technical indicator parameters that fully meet the requirements of relevant standards.

[0078] Based on the results of the above-mentioned Examples 2 and 3, it is further fully demonstrated that the processing performance of the American ginseng powder after ultrasonic supercritical treatment by the present method is better than that of the American ginseng powder treated by ordinary pulverization, the American ginseng powder treated by simple supercritical treatment, and the American ginseng powder treated by ultrasonic supercritical treatment whose treatment conditions exceed the scope of the present method, and has essential differences. Only the American ginseng powder obtained by the present method finally achieves direct tableting without adding any additional auxiliary materials. The parameter range set by the present method is obtained through a large number of experimental explorations and summaries, and has its rationality and ingenuity. It can balance the effects of granulation, water content, ultrasonic cavitation, dissolution and penetration of supercritical fluids, etc., so as to achieve the effect of improving the processing performance of American ginseng powder for direct preparation. The same effect may not be obtained if the parameter setting range of the present method is exceeded.

[0079] Comparative Example 4

[0080] Take a portion of the American ginseng particles after ultrasonic supercritical treatment in Example 1, flatten them and put them into a horizontal pressure steam sterilizer, set the conditions to 121° C., 20 min for wet heat sterilization, and discharge the material under a controlled clean environment to obtain a sterilized material.

[0081] Example 4

[0082] Comparison of sensory properties, moisture content, and effective ingredient content of American ginseng powder before and after treatment

[0083] A portion of the American ginseng raw material in Example 1 was crushed through a 120-mesh sieve to obtain a powder (American ginseng powder before treatment), and the American ginseng powder after treatment in Example 1 (American ginseng powder treated with ultrasonic supercritical + microwave sterilization, American ginseng powder in Example 1) were submitted to a qualified professional organization (Qingdao Puni Testing Co., Ltd.) for sensory evaluation, and a blind evaluation was conducted among the company's employees. The evaluation results unanimously agreed that there was no obvious change in the basic flavor characteristics of the American ginseng powder before and after treatment by this method, indicating that this method is effective in maintaining the natural flavor of the American ginseng raw material. The evaluation reflected that the color of the powder after treatment was slightly lighter than that before treatment, and that there were some subtle differences in the appearance of the powder, the taste of the food, and the thickness of the front, middle and aftertaste of the taste perception. This is due to the change in the microstructure of the American ginseng powder after treatment, resulting in detailed changes in the appearance and taste.

[0084] In addition, the American ginseng material after treatment in Comparative Example 4 was taken, dried with hot air at 60°C, and then crushed through a 60-mesh sieve to obtain a powder (American ginseng powder treated with ultrasonic supercritical + moist heat sterilization, American ginseng powder in Comparative Example 4). The American ginseng powder in Comparative Example 4 and the American ginseng powder before treatment were handed over to the company's internal quality inspectors and technicians for sensory evaluation. It was unanimously agreed that the American ginseng powder in Comparative Example 4 was significantly darker in color (browning), the smell was significantly weakened, and the taste was significantly changed (the ginseng taste of the American ginseng powder in Comparative Example 4 was significantly weakened and had a characteristic less-layered and single taste after over-ripening of a food ingredient), and the taste was significantly deteriorated (the taste of the American ginseng powder in Comparative Example 4 was very rough, similar to the taste of chewing residue). Since the sensory changes were already very obvious, no large-scale and more professional sensory evaluation was arranged. The above results show that other methods of treatment (such as ultrasonic supercritical + moist heat sterilization in Example 4) may not necessarily achieve the beneficial effects of this method in maintaining the natural flavor characteristics of American ginseng raw materials.

[0085] Example 5

[0086] The American ginseng powder before and after the treatment by the above method and the American ginseng material after the treatment of comparative example 4 (without drying treatment) were tested for moisture and effective component content. The results are shown in Table 3:

[0087] Table 3

[0088]

[0089] It can be seen that the total saponin content of the American ginseng powder in Example 1 before and after treatment is basically the same (the slight difference in the result values ​​can be regarded as the deviation of the method system, the decrease in water content leads to a slight increase in the content values ​​of other substances, etc., in short, the difference between the results is negligible), indicating that the present method is effective in maintaining the content of effective components of the American ginseng raw material; while the total saponin content of American ginseng after treatment in Comparative Example 4 has decreased significantly, even lower than the standard requirement, indicating that other treatment methods (such as ultrasonic supercritical + moist heat sterilization treatment in Comparative Example 4) may not necessarily achieve the beneficial effect of the present method in maintaining the content of effective components of the American ginseng raw material.

[0090] In addition, the moisture content of the American ginseng powder after treatment in Example 1 is basically restored to the moisture content level of the raw material before treatment, and is slightly reduced, indicating that the microwave treatment step of the present method can effectively remove the moisture added in the previous granulation step, thereby eliminating other additional drying steps, which simplifies the process, reduces energy consumption, and saves production costs; the moisture content of the American ginseng material after treatment in Comparative Example 4 is still very high, much higher than the moisture content level of the American ginseng powder before treatment. Generally, the material needs to be subjected to additional drying treatment after wet heat sterilization treatment to restore the moisture content of the material to the level of conventional dry materials, indicating that other treatment methods (such as ultrasonic supercritical + wet heat sterilization treatment in Example 4) may not necessarily achieve the beneficial effects of the present method of removing the moisture added in the previous granulation step, eliminating other additional drying steps, simplifying the process, reducing energy consumption, and saving costs.

[0091] Example 6

[0092] Detection of Microbial Content in American Ginseng Powder During Processing

[0093] A portion of the American ginseng particles treated with ultrasonic supercritical fluid in Example 1 were taken and dried with hot air at 50°C. The powder obtained by crushing the American ginseng raw material in Example 1 through a 120-mesh sieve (American ginseng before treatment) and the American ginseng particles treated with microwaves in Example 1 were tested for microbial items. The results are shown in Table 4.

[0094] Table 4

[0095]

[0096] Note: The standard requirements and test methods for each microbial item index refer to the general technical requirements for domestic health food products (GB 16740 "National Food Safety Standard Health Food").

[0097] It can be seen that before treatment, American ginseng, as a crude drug with a low degree of processing, had a high base value of various microbial index contents. After ultrasonic supercritical treatment, various microbial indexes decreased significantly. This was due to the inactivation of a large number of microorganisms after being subjected to harsh environmental treatments such as ultrasound, hypertonicity and high pressure, anaerobic treatment, and sudden drop in air pressure during pressure relief, which caused the cells to swell and rupture. However, the total colony count level was still high, and the detection values ​​of mold and yeast were still close to the upper limit of the standard. After microwave treatment by this method, all microbial indexes dropped to a safe level, and the number was far below the upper limit of the standard. Therefore, it is believed that after treatment by this method, the microbial indexes of American ginseng powder are effectively controlled, and the material has achieved a sterilization effect. As long as the subsequent processing of the preparation application is carried out in a controlled clean workshop according to the specifications, the microbial standards of the final preparation can be guaranteed.

[0098] Furthermore, even if the same method of ultrasonic supercritical + microwave sterilization is adopted, it can be simply predicted that the specific parameter setting of microwave sterilization is always closely related to the microbial base number, moisture content, material texture and particle size of the raw material. The microwave sterilization conditions of this method are suitable for American ginseng materials treated under specific conditions of this method (containing appropriate amount of moisture but not dry matter, loose texture, and the microbial content of the material is reduced to a certain extent after ultrasonic supercritical treatment. These conditions are conducive to setting a relatively low intensity and short time microwave sterilization treatment to achieve sterilization and the effect achieved by microwave sterilization of this method as discussed in Examples 4 and 5). The same microwave treatment conditions for other materials may not achieve the same effect. The microwave treatment condition setting of this method has been repeatedly verified and concluded that if the time is too short, it is impossible to ensure that the moisture and microbial content meet the standards, and if the time is too long, it is impossible to ensure that the flavor substances and functional components of the material are maintained, and the material may even be directly scorched. This part will no longer cite experimental cases for explanation.

[0099] Example 7

[0100] Take dried sliced ​​American ginseng slices, crush them through an 80-mesh sieve, add 30% water by weight to the powder and mix them evenly, use an extrusion granulator to pass through a 4mm sieve plate for granulation, and obtain relatively loose particles. Since the raw material itself contains a certain amount of moisture, and the material loses some moisture after extrusion granulation, the average moisture content of the material after granulation is about 26%. The obtained particles are loaded into an ultrasonic enhanced supercritical carbon dioxide treatment device, and the process parameters are set and controlled as follows: pressure: 30MPa, temperature: 50℃, ultrasonic frequency: 20KHz, treatment time: 60min. After the time is up, the system is depressurized and carbon dioxide is recovered. The treated particles are taken out, and it can be seen that the particle volume is significantly increased and the state becomes looser. The particles are flattened and placed in a box-type microwave sterilization device, and treated for 5min under a microwave frequency of 2450MHz to obtain materials with moisture and microorganisms that meet the standards (moisture ≤9%, microbial standards refer to domestic health food regulations). The materials are discharged under a controlled clean environment, and the subsequent processes are carried out in a 100,000-level clean workshop. The loose particles after microwave treatment are taken and crushed through a 60-mesh sieve to obtain American ginseng powder with good preparation processing performance, and the powder is prepared into powder, granules, capsules, tablets, tea and other dosage forms through corresponding preparation equipment without adding any excipients (when preparing granules and using non-direct compression equipment such as rotary tablet presses and single-punch tablet presses to prepare tablets, it is necessary to add an appropriate amount of water to prepare particles with a size that meets the performance requirements of the preparation equipment and product design requirements. After the particles are dried at a low temperature of ≤60°C, they are packaged on a machine to obtain granules with a fixed filling specification, or after the particles are granulated, they are compressed on a machine and coated or uncoated to obtain tablets with a fixed tablet weight specification).

[0101] Example 8

[0102] Microscopic observation of American ginseng powder before and after treatment

[0103] The American ginseng powder with good preparation processing performance obtained after the treatment in Example 7 was passed through an 80-mesh sieve to obtain the undersize powder (80-mesh American ginseng powder after treatment), and the undersize powder obtained by crushing the American ginseng slices before the treatment in Example 2 through an 80-mesh sieve (80-mesh American ginseng powder before treatment) were made into suspensions respectively, and the supernatant was taken after standing for 2 minutes. After obtaining glass slides, they were observed under a microscope with a magnification of 16×40.

[0104] Observe the field of view Figure 3 and Figure 4 , Figure 3 To process the first 80 mesh American ginseng powder, Figure 4 It is 80 mesh American ginseng powder after processing.

[0105] visible, Figure 3The 80-mesh American ginseng powder particles before processing in the microscope field of view are rather irregular, with different shapes and sizes. Many particles are irregularly elongated, irregularly polygonal with jagged edges or abnormal defects, irregular shapes with abnormal bifurcations, and other irregular shapes. The background color of the particles varies in depth, indicating that the particle density, three-dimensional structure, etc. are also irregular. The powder composed of particles with obvious morphological differences often has poor fluidity, which can easily cause unstable filling quantity and is difficult to prepare directly. Other auxiliary materials with good fluidity need to be added to improve the powder properties. Figure 4 The state of the 80-mesh American ginseng powder particles after treatment by this method in the microscope field of view shows a strong regularity on the whole, specifically, the shape is relatively regular, presenting a spherical shape with rounded edges and full particles. Such particles often have good fluidity, and fluidity is the first characteristic that all dosage forms must satisfy. Furthermore, the particles show a certain size difference regularity, but the size difference is not too large overall. The appropriate combination of large and small particles can enhance the fluidity and filling performance of the material, thereby enhancing the performance of the preparation. The background color of the particles shows a light color and high permeability as a whole, indicating that the particles are in a state similar to puffing. Such particles are plastic and compressible, and can also enhance the performance of the preparation. In addition to the high permeability of the particles as a whole in the field of view, it can be seen that the background color of the edges of most particles is deepened. This is because the soluble substances such as polysaccharides, colloids, protein polypeptides, etc. adhere to the surface of the particles after special ultrasonic supercritical treatment by this method. They have strong adhesion and can play the role of "natural adhesive" during tableting or granulation, thereby further enhancing the preparation performance of the material.

[0106] Overall, through Figure 3 and Figure 4 It can be seen from the comparison that the properties of the American ginseng powder before and after the treatment have changed significantly, indicating that the processing performance of the American ginseng powder after the treatment by this method has been changed, and the tests of Example 1 and Example 7 and other series of practices have proved that this change is more conducive to the preparation, and the method is to improve the properties of the particles by physical methods, without the need to add toxic chemical catalysts or other high-risk radiation substances for treatment, and the food safety is guaranteed, so it is very suitable for the modification of American ginseng powder for internal use.

[0107] Example 9

[0108] Three batches of pilot tests and accelerated stability tests of formulation products

[0109] Take the dried broken American ginseng coarse pieces, crush them through a 100-mesh sieve, add 35% water by weight to the powder and mix them evenly, use an extrusion granulator to pass through a 4mm sieve plate for granulation, and obtain relatively loose particles. Since the raw material itself contains a certain amount of moisture, and the material loses some moisture after extrusion granulation, the average moisture content of the material after granulation is about 28%. The obtained particles are loaded into an ultrasonic enhanced supercritical carbon dioxide treatment device, and the process parameters are set and controlled as follows: pressure: 32MPa, temperature: 52℃, ultrasonic frequency: 20KHz, treatment time: 90min. After the time is up, the system is depressurized and carbon dioxide is recovered. The treated particles are taken out, and it can be seen that the particle volume is significantly increased and the state becomes looser. The particles are flattened and placed in a box-type microwave sterilization equipment, and treated for 6min under a microwave frequency of 2450MHz to obtain materials with moisture and microorganisms that meet the standards (moisture ≤9%, microbial standards refer to domestic health food regulations). The materials are discharged under a controlled clean environment, and the subsequent processes are carried out in a 100,000-level clean workshop. The loose particles after microwave treatment were crushed through a 60-mesh sieve to obtain American ginseng powder with good preparation processing performance. The powder was directly tableted using a powder tablet press without adding any excipients (specification: 0.25 g / tablet) to obtain tablet products, which were packaged in polyester bottles at 60 tablets / bottle.

[0110] The above operation was repeated three times to obtain three batches of pilot products.

[0111] Example 10

[0112] Accelerated stability test of three batches of pilot products

[0113] Three batches of pilot products of American ginseng slices prepared in Example 9 were taken for accelerated testing in accordance with the "Guidelines for Stability Testing of Health Foods". Products accelerated for 0, 1, 2, and 3 months were tested for all items in accordance with the quality standard requirements, and the results were all qualified, proving that the finished preparation prepared from American ginseng powder using this method has a quality stability that meets the relevant requirements for health foods.

[0114] The American ginseng slices accelerated for 3 months have moderate hardness when chewed, are non-sticky, and have a crisp and refreshing overall taste. The natural flavor of American ginseng is fully retained, with a natural and fresh aroma and a slightly bitter and sweet taste. Overall, the taste is improved and the flavor is restored. It is a new and simple American ginseng tonic health product eating experience. In addition, the method fully retains the effective ingredients of American ginseng. Therefore, the tablets obtained by this method are a product that meets the quality expectations and trend requirements of consumers in the new era for herbal health internal products.

[0115] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing American ginseng powder, characterized in that: The following steps are involved: Mixing American ginseng powder with water to form granules, and obtaining granules with a water content of 25% to 33 wt %; the American ginseng powder is a fine powder with a mesh size of 80 to 120; and the granules with a water content of 25% to 33 wt % have a particle size of 4 to 6 mm; The particles having a water content of 25% to 33wt% are subjected to ultrasonic enhanced supercritical carbon dioxide treatment to obtain treated particles; the conditions of the ultrasonic enhanced supercritical carbon dioxide treatment are: pressure: 30 to 35MPa, temperature: 50 to 55°C, ultrasonic frequency: 20 to 25KHz, and treatment time: 45 to 90min; subjecting the treated particles to microwave sterilization; The microwave frequency during the microwave sterilization is 2440-2500 MHz, and the sterilization time is 4-7 minutes; The loose particles obtained after microwave sterilization are crushed and passed through a 60-mesh sieve, and the sieved material is collected to obtain American ginseng powder.

2. American ginseng powder prepared by the preparation method according to claim 1.

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