Polygonatum sibiricum extract as well as preparation method and application thereof

Abstract

The invention discloses a preparation method and application of a rhizoma polygonati extract, and belongs to the technical field of plant extraction. According to the preparation method, a plurality of processes such as wet ultrafine grinding, high-pressure homogenization, supramolecular inclusion, solid-liquid separation, reverse osmosis concentration and spray drying are cooperatively utilized, the process flow is novel and mild, and full-process intelligent production of online continuous feeding, instantaneous wall-breaking extraction and drying and full-component extraction and utilization can be realized; furthermore, the resource utilization maximization and environment-friendly green production of the polygonatum kingianum are realized. The process problems that an existing plant extraction technology is long in extraction time, high in energy consumption, low in efficiency and incapable of achieving full-ingredient extraction and utilization are solved, and the prepared rhizoma polygonati extract has unique application value in the aspects of nutrition nourishing, dietary therapy health care, skin care and the like and has good application prospects in the fields of food, health care products and cosmetics. The method is high in market competitiveness and suitable for large-scale popularization and application.

Description

Technical Field

[0001] The invention relates to a plant extraction method, in particular to a polygonatum sibiricum extract and a preparation method thereof, and belongs to the technical field of plant extraction. Background Art

[0002] Polygonatum sibiricum is the dried rhizome of Polygonatum kingianum Coll.et Hemsl., Polygonatum sibiricum Red. or Polygonatum cyrtonema Hua, plants of the Liliaceae family. It tastes sweet, is neutral in nature, and enters the spleen, lung, and kidney meridians. It has the effects of tonifying qi and nourishing yin, strengthening the spleen, moistening the lungs, and benefiting the kidneys. It is often used for symptoms such as spleen and stomach qi deficiency, fatigue, insufficient stomach yin, dry mouth and poor appetite, lung deficiency and dry cough, cough with blood due to fatigue, insufficient essence and blood, and soreness of the waist and knees.

[0003] Polygonatum sibiricum is a dual-purpose resource for medicine and food, and has high medicinal and therapeutic health value. Modern pharmaceutical research has shown that Polygonatum sibiricum contains a variety of chemical components, mainly including polysaccharides, steroidal saponins, triterpenes, alkaloids, lignans, flavonoids, phytosterols and volatile oils, among which polysaccharides and steroidal saponins are the main active ingredients in Polygonatum sibiricum. Modern pharmacological research has shown that Polygonatum sibiricum has a variety of pharmacological activities, such as anti-oxidation, anti-aging, immune regulation, anti-tumor, hypoglycemic, lipid regulation and other functions.

[0004] Polygonatum contains a variety of natural beauty active ingredients, which have beauty functions such as anti-aging, radiation protection, anti-inflammatory, antibacterial, hair growth and black hair. Polygonatum has been called "the medicine of the immortals" in history. Practice has also proved that long-term consumption of this product has the effect of prolonging life, preserving essence and nourishing the face, and has the effect of making the skin smooth, the complexion ruddy, and the hair black and shiny. The application of Polygonatum in cosmetics has a good market application prospect. In recent years, a series of products such as Polygonatum formula granules, Polygonatum tea, Polygonatum pollen tea, Polygonatum oral liquid, Polygonatum polysaccharide konjac glucoside capsules, Hericium edodes Polygonatum capsules, Polygonatum glutinous rice wine, etc. have continuously emerged in the market and have also won the love of consumers and market recognition.

[0005] Therefore, in recent years, the development and utilization of active ingredients in polygonatum have received extensive attention, but the research on active ingredients in polygonatum in the prior art is mostly focused on polygonatum polysaccharides, alkaloids and steroidal saponins, etc. Common extraction methods include hot water extraction, subcritical water extraction, microwave extraction, ultrasonic-assisted hot water extraction, ultrasonic-synergistic complex enzyme method, enzymatic extraction, supercritical fluid extraction technology, etc. However, no matter which of the above extraction technologies is used, only the water-soluble components in polygonatum (such as polygonatum polysaccharides, alkaloids, etc.) can be extracted, and the extraction and utilization of all components of polygonatum cannot be achieved, resulting in the fact that the value of polygonatum resources has not been fully utilized, and the application value of polygonatum extracts has not been fully reflected.

[0006] Chinese invention patent CN102351960A discloses a method for extracting polygonatum polysaccharide, which adopts ultrasonic extraction. The steps involved are relatively complicated, and the extracted polygonatum polysaccharide has low purity and contains more impurities.

[0007] Chinese invention patent CN101255199A discloses a method for extracting polygonatum polysaccharide from polygonatum, first, dissolving coarse powder of polygonatum medicinal material in water, heating, boiling and filtering, and obtaining a water extract of polygonatum; then, concentrating the water extract to a density of 1.05-1.18, adding 95% ethanol to a solution with an ethanol concentration of 75-85%, settling for 12-36 hours, filtering, obtaining a light yellow precipitate, and drying to obtain a polygonatum polysaccharide extract. The ethanol precipitation of polygonatum polysaccharide after boiling has the problems of low extraction rate, complicated steps and long time consumption, and relies on high concentration ethanol (75%-85%) precipitation, resulting in high cost and limited industrial efficiency.

[0008] Chinese invention patent CN106938006A discloses a polygonatum extract and its preparation method and application, which comprises the following steps: crushing dried polygonatum to obtain polygonatum dry powder; taking the polygonatum dry powder, adding a cell crushing material and distilled water, and mixing them evenly, wherein the cell crushing material comprises cellulase, pectinase, and CTAB; placing the mixed liquid in a 60-70°C water bath for 5-6 hours, and after the water bath, heating the mixed liquid to boiling for 10-15 minutes, and then adding activated carbon, standing and cooling, and then centrifuging to collect the supernatant; adding anhydrous ethanol to the supernatant, standing for 6-8 hours, and centrifuging to obtain a precipitate, and drying the precipitate to obtain a polygonatum extract.

[0009] It can be seen that in the above-mentioned prior art, the extraction process of polygonatum only involves the extraction of water-soluble active ingredients (polygonatum polysaccharide, etc.) in polygonatum, and fails to realize the extraction and utilization of all components of polygonatum. Based on this, a preparation method that uses water as an extraction solvent to realize online continuous feeding, instantaneous wall-breaking extraction, and drying, and full-component extraction and utilization, and realizes the maximization of polygonatum resource utilization and green production has not been reported, which is a technical direction that needs to be studied urgently. Summary of the invention

[0010] In order to solve the deficiencies of the prior art, the purpose of the present invention is to provide a method for preparing a polygonatum sibiricum extract, so as to overcome the problems of the prior art such as complicated process, high cost and inability to extract all components of polygonatum sibiricum.

[0011] In order to achieve the above object, the present invention adopts the following technical solution:

[0012] The present invention first discloses a method for preparing a polygonatum extract, comprising the following steps:

[0013] S1. Prepare raw materials: Dry the polygonatum sibiricum raw materials to obtain dry polygonatum sibiricum products, and cut them to obtain polygonatum sibiricum fragments;

[0014] S2. Wet ultrafine grinding: Place the polygonatum sibiricum fragments in a wet ultrafine grinder for ultrafine grinding to obtain a polygonatum sibiricum suspension ultrafine dispersion slurry. The active ingredients of traditional Chinese medicines are usually distributed in cells and intercellular substances, mainly in cells. If conventional grinding is used, the powder particles after grinding are often composed of several or dozens of intact cells. During the extraction process, the bioactive ingredients in the cells are difficult to release, resulting in low extraction yield, high production cost, and low resource utilization rate.

[0015] S3. High-pressure homogenization for cell wall breaking: Subject the polygonatum sibiricum suspension ultrafine dispersion slurry to high-pressure homogenization to obtain a polygonatum sibiricum homogenized dispersion slurry after cell wall breaking. Through the online linkage production of "wet crushing + high-pressure homogenization", instantaneous cell wall breaking extraction can be achieved, realizing the complete release of bioactive ingredients in cells, greatly improving the dissolution effect of active ingredients in raw materials, and at the same time improving production efficiency.

[0016] S4. Supramolecular inclusion extraction: Add hydroxypropyl-β-cyclodextrin to the polygonatum sibiricum homogenized dispersion slurry after cell wall breaking for supramolecular inclusion extraction to obtain a polygonatum sibiricum supramolecular inclusion dispersion slurry. In this step, the "supramolecular inclusion technology" is innovatively used to realize the synchronous extraction of water-soluble and fat-soluble active ingredients, solving the technological limitation that the clarity of the product obtained after "high-pressure homogenization" is poor when water is used as the extraction solvent.

[0017] S5. Solid-liquid separation: Subject the polygonatum sibiricum supramolecular inclusion dispersion slurry to solid-liquid separation to obtain wet solid polygonatum sibiricum extract I and clarified liquid polygonatum sibiricum extract II.

[0018] Preferably, the moisture mass percentage content of the aforementioned dry polygonatum sibiricum products does not exceed 15%, and the thickness and size of the polygonatum sibiricum fragments do not exceed 1.0 cm.

[0019] More preferably, in the aforementioned step S2, the cut polygonatum sibiricum fragments and pure water are placed in an online wet ultrafine grinder according to a weight ratio of 1:10 - 15 for wet ultrafine grinding, and the average particle size of the solid particles after grinding is not greater than 20 microns to obtain a polygonatum sibiricum suspension ultrafine dispersion slurry.

[0020] Still more preferably, in the aforementioned step S3, the polygonatum sibiricum suspension ultrafine dispersion slurry is subjected to high-pressure homogenization, wherein the continuous working pressure of the high-pressure homogenizer is 30 Mpa - 50 Mpa, and the average particle size of the solid particles after high-pressure homogenization is not greater than 1.0 micron to obtain a polygonatum sibiricum homogenized dispersion slurry after cell wall breaking.

[0021] More preferably, in the aforementioned step S4, hydroxypropyl beta-cyclodextrin is added to the homogenized and dispersed yellow-fleshed polygonatum sibiricum slurry; the addition amount of the hydroxypropyl beta-cyclodextrin is 5% to 15% of the weight of the yellow-fleshed polygonatum sibiricum raw material, the inclusion extraction of the hydroxypropyl beta-cyclodextrin is carried out at room temperature, and the time of the inclusion extraction is 30 minutes to 1.5 hours, to obtain a yellow-fleshed polygonatum sibiricum supramolecular inclusion dispersed slurry.

[0022] Even more preferably, in the aforementioned step S5, the solid-liquid separation method is: using a clarifying type automatic slag-discharging disc centrifuge for solid-liquid separation, and yellow-fleshed polygonatum sibiricum extract I (wet solid) and yellow-fleshed polygonatum sibiricum extract II (basically clarified liquid) can be obtained simultaneously.

[0023] Further preferably, the aforementioned preparation method further includes step S6: drying the yellow-fleshed polygonatum sibiricum extract I, and then performing post-treatment processing to obtain fine powder of yellow-fleshed polygonatum sibiricum extract I.

[0024] Even further preferably, the aforementioned post-treatment processing is: drying and pulverizing the yellow-fleshed polygonatum sibiricum extract I, the drying method is hot air circulation drying or vacuum drying, and the drying temperature is 60°C to 80°C; the moisture content of the yellow-fleshed polygonatum sibiricum extract I after drying does not exceed 10 wt.%, and the yellow-fleshed polygonatum sibiricum extract I is pulverized into fine powder.

[0025] Further preferably, the aforementioned preparation method further includes step S7: sequentially performing precision filtration, RO reverse osmosis membrane concentration, sterilization and drying on the yellow-fleshed polygonatum sibiricum extract II to obtain fine powder of yellow-fleshed polygonatum sibiricum extract II.

[0026] Even further preferably, the precision filtration method of the aforementioned yellow-fleshed polygonatum sibiricum extract II is: filtering with a 0.2-micron to 1.0-micron filter element and / or filter membrane; the concentration method is: using an RO reverse osmosis membrane with a 90% salt rejection rate; the sterilization method is: using UHT instant sterilization; the drying method is: spray drying; the moisture content of the yellow-fleshed polygonatum sibiricum extract II after drying does not exceed 10 wt.%, and the yellow-fleshed polygonatum sibiricum extract II is pulverized into fine powder. Concentrating the yellow-fleshed polygonatum sibiricum extraction solution with an RO reverse osmosis membrane can, on the one hand, achieve room temperature concentration, avoid the destruction and degradation of the active ingredients in the yellow-fleshed polygonatum sibiricum extraction solution during concentration under high temperature conditions, and on the other hand, the permeate generated during the concentration process can be used as the extraction solvent for yellow-fleshed polygonatum sibiricum, realizing the recycling of the extraction solvent during the yellow-fleshed polygonatum sibiricum extraction process, thereby achieving resource conservation and green production.

[0027] The present invention also discloses a yellow-fleshed polygonatum sibiricum extract prepared by the aforementioned method.

[0028] In addition, the present invention also discloses the application of the yellow-fleshed polygonatum sibiricum extract prepared by the aforementioned method in food, health products, cosmetics and medicine.

[0029] The beneficial effects of the present invention are as follows:

[0030] (1) The preparation method of the polygonatum sibiricum extract of the present invention comprises the coordinated application of multiple processes such as wet ultrafine grinding, high-pressure homogenization wall-breaking extraction, supramolecular inclusion technology, online solid-liquid separation, reverse osmosis membrane concentration, etc. The process is unique, novel and mild. Water is used as the extraction solvent to realize online continuous feeding, instantaneous wall-breaking extraction, drying, and full-process intelligent production and full-component extraction and utilization, thereby realizing the maximum utilization of polygonatum sibiricum resources and green production, and solving the process problems of the existing polygonatum sibiricum extraction technology, such as long extraction time, high energy consumption, low efficiency and inability to realize full-component extraction and utilization.

[0031] (2) Because Polygonatum sibiricum contains a lot of colloid components, it is difficult to grind Polygonatum sibiricum into ultrafine powder (powder particle size ≤ 20 μm) by conventional or low-temperature grinding methods, and it is also impossible to meet the requirements of high-pressure homogenization for the feed solid particle size. Therefore, the present invention uses a unique "wet grinding" technology to achieve online continuous ultrafine grinding of Polygonatum sibiricum, while meeting the requirements of subsequent high-pressure homogenization equipment for the feed solid particle size. Furthermore, a combined extraction process of "wet crushing + high-pressure homogenization wall breaking" is also adopted to achieve the process implementation effect of instantaneous wall breaking extraction, completely release the biologically active components in the cells, greatly improve the dissolution effect of the active components in the raw materials, and at the same time achieve an increase in production efficiency.

[0032] (3) Since Polygonatum sibiricum also contains fat components, it is easy to form a translucent emulsion after "high-pressure homogenization". The present invention innovatively uses "supramolecular inclusion technology" to significantly increase the water solubility of fat-soluble components by utilizing the unique hollow molecular structure and good water solubility of hydroxypropyl beta-cyclodextrin, as well as the molecular characteristics of external hydrophilicity and internal hydrophobicity, and improve the solubility of effective components of Polygonatum sibiricum in water by molecular absorption and inclusion, thereby improving the extraction efficiency. Moreover, supramolecular inclusion is a physical inclusion and does not change the chemical structure. Therefore, the present invention uses water as the extraction solvent, and by adding hydroxypropyl beta-cyclodextrin to the homogenized liquid after "high-pressure homogenization", the water solubility of fat-soluble components in the homogenized liquid is significantly increased. On the one hand, the simultaneous extraction of water-soluble components and fat-soluble components of Polygonatum sibiricum is achieved, and on the other hand, a Polygonatum sibiricum extract II with good water solubility can be obtained.

[0033] (4) The polygonatum sibiricum extract prepared by the method of the present invention has more comprehensive nutritional components, realizes the extraction and utilization of all components of polygonatum sibiricum, has unique application value in nutrition and nourishment, diet therapy and health care, skin care, medicine, etc., has good application prospects in the fields of food, health care products, cosmetics and medicine, has strong market competitiveness, and is suitable for large-scale industrial promotion and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 The invention discloses a process flow chart of a method for preparing a polygonatum sibiricum extract. DETAILED DESCRIPTION

[0035] The present invention will be specifically introduced below in conjunction with the accompanying drawings and specific embodiments.

[0036] Example 1

[0037] The preparation process of this example is as Figure 1 shown and includes the following steps:

[0038] S1. Prepare raw materials: Purchase polygonatum odoratum (dry product) that meets the requirements under polygonatum odoratum in Part I of the Chinese Pharmacopoeia (2020 Edition), take samples, test that the moisture content of the polygonatum odoratum (dry product) is 11.7%, and use a traditional Chinese medicine slicing machine to cut the above-mentioned polygonatum odoratum (dry product) into polygonatum odoratum fragments with a thickness and size between 0.3 and 1.0 cm, sieve out ash and fine powder to obtain polygonatum odoratum fragments.

[0039] S2. Wet ultrafine grinding: Weigh 150 kg of polygonatum odoratum fragments and 1500 kg of pure water. Add polygonatum odoratum fragments and pure water to an on-line wet ultrafine grinder at the same time for wet ultrafine grinding, control the feeding speed of wet grinding, and grind the polygonatum odoratum into a solid-liquid suspension with an average particle size of less than 20 microns to obtain a superfine dispersed slurry of polygonatum odoratum suspension.

[0040] S3. High-pressure homogenization for cell wall breaking: Subject the superfine dispersed slurry of polygonatum odoratum suspension to high-pressure homogenization. Among them, the continuous working pressure of the high-pressure homogenizer is set to 30 Mpa, and control the high-pressure homogenization to break it into a solid-liquid suspension with an average particle size of less than 1.0 micron to obtain a homogenized and dispersed slurry of cell wall-broken polygonatum odoratum.

[0041] S4. Supramolecular inclusion extraction: Add 7.5 kg of hydroxypropyl beta-cyclodextrin to the homogenized and dispersed slurry of cell wall-broken polygonatum odoratum, and perform inclusion extraction at room temperature for 30 minutes to obtain a supramolecular inclusion dispersed slurry of polygonatum odoratum.

[0042] S5. Solid-liquid separation: Use a clarifying type automatic slag-discharging disc centrifuge to perform solid-liquid separation on the supramolecular inclusion dispersed slurry of polygonatum odoratum to obtain polygonatum odoratum extract I (wet solid) and polygonatum odoratum extract II (clarified liquid).

[0043] S6. Further process polygonatum odoratum extract I:

[0044] (1) Drying: Dry the polygonatum odoratum extract I (wet solid) in a hot air circulation oven. Drying temperature: 80 °C, drying time 4 hours. The moisture content of the polygonatum odoratum extract I (dry product) is 4.27%, and the weight of the obtained polygonatum odoratum extract I (dry product) is: 51.54 kg.

[0045] (2) Grinding: Use a universal grinder to grind the polygonatum odoratum extract I (dry product) into fine powder, and the weight of the obtained fine powder of polygonatum odoratum extract I is: 50.97 kg.

[0046] S7. Further process polygonatum odoratum extract II:

[0047] (1) Precision filtration: The polygonatum sibiricum extract II (liquid) is precisely filtered using a 1.0-micron mixed cellulose filter membrane to obtain a clear and transparent refined filtrate of polygonatum sibiricum extract II.

[0048] (2) Concentration: The refined filtrate of polygonatum sibiricum extract II is concentrated at room temperature using an RO reverse osmosis membrane with a 90% desalination rate to obtain 461.8 kg of concentrated polygonatum sibiricum extract II.

[0049] (3) Sterilization: The 461.8 kg of concentrated polygonatum sibiricum extract II is instantaneously sterilized online using the UHT instantaneous sterilization method.

[0050] (4) Drying: The sterilized and concentrated polygonatum sibiricum extract II is spray-dried to obtain fine powder of polygonatum sibiricum extract II (dry product). The moisture content of the spray-dried fine powder of polygonatum sibiricum extract II is 6.04%, and the weight of the obtained fine powder of polygonatum sibiricum extract II is 89.15 kg.

[0051] Example 2

[0052] The preparation method of this example includes the following steps:

[0053] S1. Prepare raw materials: Purchase polygonatum sibiricum medicinal materials (dry product) that meet the requirements of polygonatum sibiricum in Part I of the Chinese Pharmacopoeia (2020 Edition), take samples, and test that the moisture content of the polygonatum sibiricum (dry product) is 11.7%. Use a traditional Chinese medicine slicer to cut the above-mentioned polygonatum sibiricum (dry product) into polygonatum sibiricum fragments with a thickness and size between 0.3 and 1.0 cm, sieve out ash and fine powder to obtain polygonatum sibiricum fragments.

[0054] S2. Wet ultrafine grinding: Weigh 150 kg of polygonatum sibiricum fragments and 1875 kg of pure water. Add the polygonatum sibiricum fragments and pure water to an online wet ultrafine grinder simultaneously for wet ultrafine grinding. Control the feeding speed of the wet grinding to grind the polygonatum sibiricum into a solid-liquid suspension with an average particle size less than 20 microns to obtain a superfine dispersed slurry of polygonatum sibiricum suspension.

[0055] S3. High-pressure homogenization for cell wall breaking: The superfine dispersed slurry of polygonatum sibiricum suspension is subjected to high-pressure homogenization. Among them, the continuous working pressure of the high-pressure homogenizer is set to 40 Mpa, and control the high-pressure homogenization to break it into a solid-liquid suspension with an average particle size less than 1.0 micron to obtain a homogenized and dispersed slurry of polygonatum sibiricum with broken cell walls.

[0056] S4. Supramolecular inclusion extraction: Add 15 kg of hydroxypropyl beta-cyclodextrin to the homogenized and dispersed slurry of polygonatum sibiricum with broken cell walls, and perform inclusion extraction at room temperature for 1 hour to obtain a supramolecular inclusion dispersed slurry of polygonatum sibiricum.

[0057] S5. Solid-liquid separation: Use a clarifying type automatic slag-discharging disc centrifuge to perform solid-liquid separation on the polygonatum sibiricum supermolecular inclusion dispersion slurry to obtain polygonatum sibiricum extract I (wet solid) and polygonatum sibiricum extract II (clarified liquid).

[0058] S6. Further processing of polygonatum sibiricum extract I:

[0059] (3) Drying: Dry the polygonatum sibiricum extract I (wet solid) in a hot air circulation oven. Drying temperature: 60 °C, drying time: 6 hours. The moisture content of the polygonatum sibiricum extract I (dry product) is 5.81%. The weight of the prepared polygonatum sibiricum extract I (dry product) is: 49.28 kg.

[0060] (4) Crushing: Use a universal crusher to crush the polygonatum sibiricum extract I (dry product) into fine powder. The weight of the obtained fine powder of polygonatum sibiricum extract I is: 48.64 kg.

[0061] S7. Further processing of polygonatum sibiricum extract II:

[0062] (1) Precision filtration: Use a 0.1 μm mixed cellulose filter membrane to perform precision filtration on the polygonatum sibiricum extract II (liquid) to obtain a clarified and transparent refined filtrate of polygonatum sibiricum extract II.

[0063] (2) Concentration: Use an RO reverse osmosis membrane with a desalination rate of 90% to concentrate the refined filtrate of polygonatum sibiricum extract II at room temperature to obtain 618.5 kg of concentrated solution of polygonatum sibiricum extract II.

[0064] (3) Sterilization: Use UHT instantaneous sterilization method to perform on-line instantaneous sterilization on 618.5 kg of concentrated solution of polygonatum sibiricum extract II.

[0065] (4) Drying: Perform spray drying on the sterilized and concentrated solution of polygonatum sibiricum extract II to obtain fine powder of polygonatum sibiricum extract II (dry product). The moisture content of the spray-dried fine powder of polygonatum sibiricum extract II is 5.83%. The weight of the obtained fine powder of polygonatum sibiricum extract II is 92.52 kg.

[0066] Example 3

[0067] The preparation method of this example includes the following steps:

[0068] S1. Prepare raw materials: Purchase polygonatum sibiricum medicinal materials (dry product) that meet the requirements of polygonatum sibiricum in Part I of the Chinese Pharmacopoeia (2020 Edition). Take samples and test that the moisture content of the polygonatum sibiricum (dry product) is 11.7%. Use a traditional Chinese medicine slicer to cut the above-mentioned polygonatum sibiricum (dry product) into polygonatum sibiricum fragments with a thickness and size between 0.3 and 1.0 cm. Sieve out the ash and fine powder to obtain polygonatum sibiricum fragments.

[0069] S2. Wet ultrafine grinding: Weigh 150 kg of polygonatum sibiricum fragments and 2250 kg of pure water. Add the polygonatum sibiricum fragments and pure water to an in-line wet ultrafine grinder simultaneously for wet ultrafine grinding. Control the feeding speed of the wet grinding, and grind the polygonatum sibiricum into a solid-liquid suspension with an average particle size less than 20 microns to obtain a superfine dispersed slurry of polygonatum sibiricum suspension.

[0070] S3. High-pressure homogenization for cell wall breaking: Subject the superfine dispersed slurry of polygonatum sibiricum suspension to high-pressure homogenization. Among them, the continuous working pressure of the high-pressure homogenizer is set to 50 Mpa, and control the high-pressure homogenization to break it into a solid-liquid suspension with an average particle size less than 1.0 micron to obtain a homogenized and dispersed slurry of polygonatum sibiricum with broken cell walls.

[0071] S4. Supramolecular inclusion extraction: Add 22.5 kg of hydroxypropyl beta-cyclodextrin to the homogenized and dispersed slurry of polygonatum sibiricum with broken cell walls, and perform inclusion extraction at room temperature for 1.5 hours to obtain a supramolecular inclusion dispersed slurry of polygonatum sibiricum.

[0072] S5. Solid-liquid separation: Use a clarifying type automatic slag-discharging disc centrifuge to perform solid-liquid separation on the supramolecular inclusion dispersed slurry of polygonatum sibiricum to obtain polygonatum sibiricum extract I (wet solid) and polygonatum sibiricum extract II (clarified liquid).

[0073] S6. Further processing of polygonatum sibiricum extract I:

[0074] (5) Drying: Dry the polygonatum sibiricum extract I (wet solid) in a hot air circulation oven. Drying temperature: 70 °C, drying time 4 hours. The water content of the polygonatum sibiricum extract I (dried product) is 8.27%. The weight of the obtained polygonatum sibiricum extract I (dried product) is: 41.85 kg.

[0075] (6) Grinding: Use a universal grinder to grind the polygonatum sibiricum extract I (dried product) into fine powder. The weight of the obtained fine powder of polygonatum sibiricum extract I is: 41.38 kg.

[0076] S7. Further processing of polygonatum sibiricum extract II:

[0077] (1) Precision filtration: Use a 0.2-micron mixed cellulose ester membrane to perform precision filtration on the polygonatum sibiricum extract II (liquid) to obtain a clarified and transparent refined filtrate of polygonatum sibiricum extract II.

[0078] (2) Concentration: Use an RO reverse osmosis membrane with a salt rejection rate of 90% to concentrate the refined filtrate of polygonatum sibiricum extract II at room temperature to obtain 702.1 kg of concentrated liquid of polygonatum sibiricum extract II.

[0079] (3) Sterilization: Use UHT instantaneous sterilization method to perform on-line instantaneous sterilization on 702.1 kg of concentrated liquid of polygonatum sibiricum extract II.

[0080] (4) Drying: The sterilized and concentrated solution of Polygonatum sibiricum extract II was spray-dried to obtain fine powder of Polygonatum sibiricum extract II (dried product). The moisture content of the spray-dried fine powder of Polygonatum sibiricum extract II was 5.19%, and the weight of the obtained fine powder of Polygonatum sibiricum extract II was 98.27 kg.

[0081] Control Example

[0082] The preparation method of this control example includes the following steps:

[0083] S1. Prepare raw materials: Purchase Polygonatum sibiricum medicinal materials (dried product) that meet the requirements of Polygonatum sibiricum in Part I of the Chinese Pharmacopoeia (2020 Edition), take samples, and test that the moisture content of Polygonatum sibiricum (dried product) is 11.7%. Use a traditional Chinese medicine slicing machine to cut the above-mentioned Polygonatum sibiricum (dried product) into Polygonatum sibiricum fragments with a thickness and size between 0.3 and 1.0 cm, sieve out ash and fine powder to obtain Polygonatum sibiricum fragments.

[0084] S2. Extraction: Weigh 150 kg of Polygonatum sibiricum fragments and 2250 kg of pure water, put them into a 3-ton extraction tank, stir and heat up to 90 °C, and keep the temperature for extraction for 4 hours to obtain a Polygonatum sibiricum solid-liquid suspension.

[0085] S3. Solid-liquid separation: Use a rotary vibrating filter screen (80 mesh) for solid-liquid separation to obtain Polygonatum sibiricum extract I (wet solid) and Polygonatum sibiricum extract II (liquid).

[0086] S4. Further process Polygonatum sibiricum extract I:

[0087] (1) Drying: Dry the Polygonatum sibiricum extract I (wet solid) in a hot air circulation oven. Drying temperature: 80 °C, drying time 4 hours. The moisture content of Polygonatum sibiricum extract I (dried product) is 7.85%, and the weight of the obtained Polygonatum sibiricum extract I (dried product) is 62.81 kg.

[0088] (2) Crushing: Use a universal crusher to crush the Polygonatum sibiricum extract I (dried product) into fine powder. The weight of the obtained fine powder of Polygonatum sibiricum extract I is 62.05 kg.

[0089] S5. Further process Polygonatum sibiricum extract II:

[0090] (1) Graded filtration: Use a plate and frame filter press to filter the Polygonatum sibiricum extract II (liquid) with a 300-mesh filter cloth to obtain a basically clear filtrate. Then, use a 0.1-micron polypropylene filter element (PP) to conduct precision filtration on the Polygonatum sibiricum extract II (liquid) to obtain a clear and transparent refined filtrate of Polygonatum sibiricum extract II.

[0091] (2) Concentration: Use a single (double)-effect concentrator or a thin film concentrator to conduct vacuum concentration on the refined filtrate of Polygonatum sibiricum extract II, and finally concentrate to obtain 408.2 kg of concentrated solution of Polygonatum sibiricum extract II.

[0092] (3) Sterilization: The 408.2 kg of concentrated Polygonatum sibiricum extract II was sterilized by pasteurization to obtain the sterilized concentrated Polygonatum sibiricum extract II.

[0093] (4) Drying: The sterilized concentrated Polygonatum sibiricum extract II was spray-dried to obtain the fine powder of Polygonatum sibiricum extract II (dried product), and the moisture content of the spray-dried fine powder of Polygonatum sibiricum extract II was 6.07%. The weight of the fine powder of Polygonatum sibiricum extract II was 73.01 kg.

[0094] The relevant quality indexes of the products in Examples 1 to 3 and Comparative Example 1 were detected, and the results are shown in Table 1 below:

[0095]

[0096]

[0097] Table 1

[0098] It can be seen that when directly using Polygonatum sibiricum fragments (the same Polygonatum sibiricum fragments as in Examples 1, 2, and 3) for feeding and heating extraction in the comparative example, since the cell wall of the Polygonatum sibiricum raw material was not broken, the substances inside the cells (intracellular polysaccharides and other related bioactive components) were difficult to dissolve effectively. The yield of Polygonatum sibiricum extract I obtained was significantly higher, while the extraction yield of Polygonatum sibiricum extract II was significantly lower. Polygonatum sibiricum extract I is the undissolved solid residue remaining after extraction. Although it has certain utilization value, its economic benefit is relatively low; while Polygonatum sibiricum extract II is rich in various bioactive substances and has more comprehensive nutritional components, which is the key target product obtained from the extraction of Polygonatum sibiricum. Therefore, the yield of Polygonatum sibiricum extract II obtained by the extraction method in the comparative example is significantly lower, which will cause waste of Polygonatum sibiricum resources.

[0099] In summary, the preparation method of the Polygonatum sibiricum extract of the present invention uniquely and creatively synergistically utilizes several processes such as wet crushing, high-pressure homogenization for cell wall breaking extraction, supramolecular inclusion technology, online solid-liquid separation, and reverse osmosis membrane concentration, which can realize the full-process intelligent production of online continuous feeding, instantaneous cell wall breaking extraction, and drying, as well as the extraction and utilization of all components of Polygonatum sibiricum, thereby maximizing the utilization of Polygonatum sibiricum resources and achieving environmentally friendly green production. It solves the process problems of long extraction time, high energy consumption, low efficiency, and inability to achieve the extraction and utilization of all components in the existing plant extraction technology, and obtains a new preparation process for the extraction of all components of Polygonatum sibiricum. The prepared Polygonatum sibiricum extract has unique application value in aspects such as nutritional tonic, dietotherapy and health care, and skin care, and has good application prospects in the fields of food, health products and cosmetics. The extraction method is ingeniously designed, simple and convenient to operate, reasonable in process, low in cost, mild in process and easy to implement, and is suitable for large-scale industrial promotion and application.

[0100] The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the art should understand that the above embodiments do not limit the present invention in any form, and all technical solutions obtained by means of equivalent replacement or equivalent transformation fall within the protection scope of the present invention.

Claims

1. A method for preparing a polygonatum extract, characterized in that: The steps include: S1. preparing raw materials: drying the raw materials of polygonatum to obtain a dried product of polygonatum, and cutting the dried product to obtain polygonatum fragments; S2, wet superfine grinding: placing the polygonatum sibiricum fragments in a wet superfine grinder for superfine grinding to obtain a polygonatum sibiricum suspension superfine dispersion slurry; S3, high-pressure homogenization and wall breaking: subjecting the polygonatum sibiricum suspension ultrafine dispersion slurry to high-pressure homogenization to obtain a wall-broken polygonatum sibiricum homogeneous dispersion slurry; S4, supramolecular inclusion extraction: adding hydroxypropyl-beta-cyclodextrin to the wall-broken polygonatum homogeneous dispersion slurry for supramolecular inclusion extraction to obtain a polygonatum supramolecular inclusion dispersion slurry; S5. Solid-liquid separation: subjecting the polygonatum sibiricum supramolecular inclusion dispersion slurry to solid-liquid separation to obtain a wet solid polygonatum sibiricum extract I and a clear liquid polygonatum sibiricum extract II.

2. The method for preparing a polygonatum sibiricum extract according to claim 1, characterized in that: The moisture content of the dried polygonatum sibiricum variety does not exceed 15% by mass, and the thickness and size of the polygonatum sibiricum fragments do not exceed 1.0 cm.

3. The method for preparing a polygonatum sibiricum extract according to claim 1, characterized in that: In the step S2, the cut polygonatum sibiricum fragments and pure water are placed in an online wet ultrafine grinder at a weight ratio of 1:10-15 for wet ultrafine grinding. The average particle size of the solid particles after grinding is not more than 20 microns, and a polygonatum sibiricum suspension ultrafine dispersion slurry is obtained.

4. The method for preparing a polygonatum sibiricum extract according to claim 1, characterized in that: In the step S3, the ultrafine dispersed slurry of the polygonatum suspension is subjected to high-pressure homogenization, wherein the continuous working pressure of the high-pressure homogenizer is 30Mpa to 50Mpa, and the average particle size of the solid particles after high-pressure homogenization is not greater than 1.0 micron, thereby obtaining a homogeneous dispersed slurry of polygonatum with broken wall.

5. The method for preparing a polygonatum sibiricum extract according to claim 1, characterized in that: In the step S4, hydroxypropyl beta-cyclodextrin is added to the wall-broken polygonatum homogeneous dispersion slurry; the amount of hydroxypropyl beta-cyclodextrin added is 5% to 15% of the weight of the polygonatum raw material, the hydroxypropyl beta-cyclodextrin inclusion extraction is carried out at room temperature, and the inclusion extraction time is 30 minutes to 1.5 hours to obtain the polygonatum supramolecular inclusion dispersion slurry.

6. The method for preparing a polygonatum sibiricum extract according to claim 1, characterized in that: In the step S5, the solid-liquid separation method is: using a clarifying automatic slag discharge disc centrifuge to perform solid-liquid separation.

7. The method for preparing a polygonatum sibiricum extract according to any one of claims 1 to 6, characterized in that: The method further comprises step S6, drying the polygonatum extract I, and then performing post-processing to obtain a fine powder of the polygonatum extract I.

8. The method for preparing a polygonatum sibiricum extract according to claim 7, characterized in that: The post-processing process is: drying and crushing the polygonatum extract I, the drying method is hot air circulation drying or vacuum drying, and the drying temperature is 60°C to 80°C; the moisture content of the polygonatum extract I after drying does not exceed 10wt.%, and the polygonatum extract I is crushed into fine powder.

9. The method for preparing a polygonatum sibiricum extract according to any one of claims 1 to 6, characterized in that: The method further comprises step S7, wherein the polygonatum sibiricum extract II is sequentially subjected to precision filtration, RO reverse osmosis membrane concentration, sterilization and drying to obtain a fine powder of the polygonatum sibiricum extract II.

10. The method for preparing a polygonatum sibiricum extract according to claim 9, characterized in that: The method for precision filtration of the polygonatum extract II is: filtration using a 0.2 micron to 1.0 micron filter element and / or filter membrane; the method for concentration is: using an RO reverse osmosis membrane with a desalination rate of 90%; the method for sterilization is: UHT instantaneous sterilization; the method for drying is: spray drying; the moisture content of the polygonatum extract II after drying does not exceed 10wt.%, and the polygonatum extract II is crushed into fine powder.

11. A polygonatum extract, characterized in that Prepared by the method according to any one of claims 1 to 10.

12. Use of the polygonatum sibiricum extract obtained by the method according to any one of claims 1 to 10 in food, health products, cosmetics and medicine.

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