Process and method for protecting components in plateau plant extraction process

Abstract

The invention relates to the technical field of plateau plant extraction processes and methods, in particular to a process and method for protecting components in the plateau plant extraction process. S2, extraction treatment; s3, carrying out solid-liquid separation treatment; s4, purification treatment; s5, drying; vacuum freeze drying or low-temperature hot air circulation drying is adopted, damage of high temperature to heat-sensitive components is avoided, the heat-sensitive components comprise vitamins, enzymes, volatile oil and the like, and integrity and stability of active components are ensured; according to the polarity of a target component, 60%-70% ethanol, water or supercritical CO2 is accurately selected as a solvent, so that efficient dissolution of components with different polarities is ensured; the two modes of spray drying and vacuum freeze drying can be selected according to product characteristics, so that the finished product is low in water content, good in stability and high in overall process compatibility, and the production requirements of different scales are met.

Description

Technical Field

[0001] The present invention relates to the technical field of extraction processes and methods for plateau plants, and particularly to a process and method for protecting components during the extraction of plateau plants. Background Art

[0002] During the extraction of plateau plants, in order to protect the active ingredients, users need to take targeted measures in combination with the growth environment, characteristics, and traditional process experience of plateau plants, and generally carry out protection treatments through drying, filtration, or centrifugation.

[0003] Traditional extraction processes and methods for plateau plants use ordinary drying methods. Improper temperature control is likely to cause damage to heat-sensitive components. During extraction, only simple soaking or heating reflux is relied on, resulting in long extraction time and low efficiency, and easy degradation of heat-sensitive substances. The traditional solid-liquid separation part only uses simple filtration or centrifugation methods, without combining multiple means such as microfiltration membrane filtration and high-speed centrifugation, making it difficult to effectively remove fine particles and impurities, and affecting the purity of the product.

[0004] Therefore, in view of the problems that the traditional extraction process and method for plateau plants are prone to damage components during the drying process, the extraction solvent selection is single, resulting in low extraction efficiency and poor overall separation effect, a process and method for protecting components during the extraction of plateau plants can be designed. Summary of the Invention

[0005] In order to overcome the problems that the traditional extraction process and method for plateau plants are prone to damage components during the drying process, the extraction solvent selection is single, resulting in low extraction efficiency and poor overall separation effect.

[0006] The technical solution of the present invention is as follows: A process and method for protecting components during the extraction of plateau plants, the steps are as follows:

[0007] SI: Raw material pretreatment

[0008] SI1: Cleaning

[0009] Rinse the raw materials with running water to remove sediment and surface contaminants;

[0010] SI2: Drying

[0011] Use a vacuum freeze dryer or a hot air circulation oven for drying treatment to avoid damage to heat-sensitive components by high temperature;

[0012] S13: Crushing

[0013] Use an ultrafine crusher to crush the raw materials to 80 - 120 meshes;

[0014] S2: Extraction treatment

[0015] Select 60%-70% ethanol, water or supercritical CO according to the component polarity 2 as the solvent. For the extraction equipment, a multi-functional extraction tank with a condensation reflux device or a supercritical extraction device is specifically used, and ultrasonic or microwave-assisted technology is used to efficiently extract the target components and reduce the degradation of thermosensitive substances;

[0016] S3: Solid-liquid separation treatment

[0017] Use a 0.45μm microporous membrane filter or a plate and frame filter press for filtration treatment, with a pressure ≤ 0.3 MPa. After filtration, start a high-speed centrifuge for separation, with a rotation speed of 4000-8000 r / min, a time of 10-20 minutes, and a temperature ≤ 25°C;

[0018] S4: Purification treatment

[0019] S41: Concentrate or dilute the extract to a concentration of 0.5-2 mg / mL, filter or centrifuge to remove solid impurities, pass through the adsorption column at a flow rate of 1-3 BV / h, collect the effluent for standby, elute successively with 30%, 40%, 50%, 60%, 70% ethanol solutions, with a flow rate of 1-2 BV / h. The eluate of each ethanol concentration segment is collected separately, the content of the target component is detected, and the eluate corresponding to the target component peak is combined;

[0020] S42: Concentrate the combined eluate to 1 / 5-1 / 10 of the original volume with a rotary evaporator, with a temperature ≤ 50°C and a vacuum degree ≥ 0.09 MPa. Prepare a solvent according to the ethanol-water volume ratio of 1:1-1:5, slowly add the concentrated solution to the solvent, stir and dissolve it, transfer the solution to an ice-water bath or a low-temperature refrigerator at -5°C to 10°C, and let it stand for several hours to several days until crystals precipitate;

[0021] S5: Drying

[0022] Use a spray dryer or a vacuum freeze dryer for drying operations;

[0023] S6: Finished product packaging and storage.

[0024] Preferably, the temperature of vacuum freeze drying in SI2 is between -40°C and -60°C, and the vacuum degree ≤ 50 Pa; the temperature of hot air drying ≤ 45°C.

[0025] Preferably, for raw materials with more oil, including pine needles, n-hexane is used for degreasing treatment in SI to reduce the interference of fat-soluble impurities; activated carbon adsorption is selected for decolorization treatment to remove chlorophyll pigments.

[0026] Preferably, in S2, when ethanol reflux extraction is carried out, the temperature is 40-60°C, the time is 1-3 hours, and it is in dynamic circulation; supercritical CO 2During extraction, the pressure is 25 MPa, the temperature is 40 °C, and the time is 2 - 4 hours.

[0027] Preferably, during ultrasonic assistance in S2, the frequency is 20 - 40 kHz, the power density is 0.1 - 0.5 W / cm 2 , the time is 20 - 40 minutes. During microwave assistance, the intermittent mode is adopted, the power is 500 - 800 W, and the time is 5 - 15 minutes.

[0028] Preferably, in S2:

[0029]

[0030] Wherein, C 提取液 is the concentration of the extract, V 提取液 is the volume of the extract, C 原料 is the content of the target component in the raw material, m 原料 is the mass of the raw material.

[0031] Preferably, in S41, the AB - 8 or D101 resin is soaked in ethanol for 24 hours. After swelling, it is rinsed with distilled water until there is no alcohol smell. The resin is loaded into the adsorption column and rinsed with 2 - 3 bed volumes of distilled water at a flow rate of 2 - 3 BV / h to stabilize the resin bed. The adsorption capacity formula is:

[0032]

[0033] Wherein, Q is the adsorption capacity, C 0 is the initial concentration, C e is the equilibrium concentration, V is the volume of the solution, m 树脂 is the mass of the resin.

[0034] Preferably, in S42, the filtered crystals are washed with a cold ethanol - water solvent, and the crystals are dissolved in a small amount of hot solvent, and the low - temperature crystallization step is repeated to improve the purity.

[0035] Preferably, in S5, for spray drying, the inlet air temperature is 160 - 180 °C, the outlet air temperature is 80 - 90 °C, the feeding speed is 5 - 10 mL / min. For vacuum freeze - drying, the temperature is - 40 °C to - 60 °C, the vacuum degree is ≤50 Pa, and the time is 24 - 48 hours.

[0036] A method for protecting components during the extraction of plateau plants, which is characterized by including the process for protecting components during the extraction of plateau plants as shown above, and its steps are as follows:

[0037] Step 1: Pretreatment of raw materials

[0038] 1) Place the collected plateau plant raw materials in a cleaning device and let the flowing water continuously wash the raw materials. The water flow rate needs to be controlled within a certain range, which can not only ensure that the sediment, dust, and other pollutants attached to the surface of the raw materials are thoroughly washed away, but also will not cause excessive erosion and damage to the raw materials;

[0039] 2) Quickly put the washed raw materials into a vacuum freeze dryer. First, lower the temperature inside the device to between -40°C and -60°C. At such a low temperature, the water in the raw materials quickly freezes into ice. Subsequently, evacuate the air to make the vacuum degree reach ≤50 Pa. At this time, the ice directly sublimes into water vapor and is pumped out, thus achieving drying. If a hot air circulation oven is used, the temperature needs to be strictly controlled at ≤45°C. Place the raw materials evenly on the oven tray and use the hot air circulation system to make the hot air evenly blow on the raw materials to take away the moisture and achieve drying;

[0040] 3) Put the dried raw materials into an ultrafine pulverizer, adjust the pulverizer parameters, and pulverize the raw materials to 80 - 120 meshes. After pulverization is completed, immediately transfer the powder to a sealed container for storage;

[0041] Step Two: Extraction Treatment

[0042] 1) Select a suitable solvent according to the polarity of the target component in the plateau plant. If the polarity of the target component is moderate, 60% - 70% ethanol is selected; for components with larger polarity, water is a suitable solvent; for some components that are sensitive to temperature and require efficient extraction, supercritical CO 2 is an ideal choice;

[0043] 2) If ethanol is used, add the pulverized raw materials and the selected solvent to a multi-functional extraction tank in a certain proportion. When using ethanol reflux extraction, control the temperature at 40 - 60°C, the reflux time at 1 - 3 hours, and maintain dynamic circulation. At the same time, turn on the ultrasonic assistance technology, set the frequency at 20 - 40 kHz, the power density at 0.1 - 0.5 W / cm 2 ², and the action time at 20 - 40 minutes; or use the microwave assistance technology, operate in an intermittent mode, with a power of 500 - 800 W and an action time of 5 - 15 minutes;

[0044] 3) When using a supercritical extraction device for supercritical CO 2 extraction, set the pressure at 25 MPa, the temperature at 40°C, and the extraction time at 2 - 4 hours;

[0045] Step Three: Solid-Liquid Separation Treatment

[0046] 1) Filter the extracted mixed solution through a 0.45 μm microporous membrane filter or a plate and frame filter press. During the filtration process, control the pressure ≤ 0.3 MPa to prevent damage to the filter membrane or affect the filtration effect caused by excessive pressure, and preliminarily separate the solid impurities in the mixed solution to obtain a relatively clear liquid, preparing for subsequent centrifugal separation;

[0047] 2) Transfer the filtered liquid to a high-speed centrifuge, set the rotation speed to 4000 - 8000 r / min, the separation time to 10 - 20 minutes, and at the same time control the temperature ≤ 25 °C to further separate the fine particles and residual impurities in the liquid, and make the solid-liquid separation more thorough through centrifugal force to obtain a relatively pure extract;

[0048] Step Four: Purification Treatment

[0049] 1) Select AB-8 or D101 resin, soak it in ethanol for 24 hours to fully swell it, and then rinse the resin with distilled water until no ethanol smell can be detected in the rinsing solution. Load the treated resin into the adsorption column, and then rinse it with 2 - 3 bed volumes of distilled water at a flow rate of 2 - 3 BV / h to stabilize the resin bed layer;

[0050] 2) Concentrate or dilute the extract to a concentration of 0.5 - 2 mg / mL. First, filter or centrifuge to remove the solid impurities in it, and then pass the treated extract through the adsorption column at a flow rate of 1 - 3 BV / h, and collect the effluent for standby. Elute the adsorption column with ethanol solutions of 30%, 40%, 50%, 60%, and 70% in turn, control the elution flow rate at 1 - 2 BV / h, collect the eluate of each ethanol concentration segment separately, and by detecting the content of the target component in each segment of the eluate, merge the eluate corresponding to the target component peak, and use the adsorption and desorption characteristics of the resin for different components to further separate the target component in the extract from other impurities and improve the purity of the target component;

[0051] 3) Concentrate the combined eluate with a rotary evaporator, control the temperature ≤ 50 °C, and the vacuum degree ≥ 0.09 MPa to reduce the volume of the concentrated solution to 1 / 5 - 1 / 10 of the original volume;

[0052] 4) Prepare a solvent according to the ethanol-water volume ratio of 1:1 - 1:5, slowly add the concentrated solution to this solvent, stir it to fully dissolve it, and then transfer the solution to an ice-water bath or a low-temperature refrigerator at -5 °C to 10 °C, and let it stand for several hours to several days to wait for crystal precipitation;

[0053] 5) After filtering to obtain the crystals, wash the crystals with a cold ethanol-water solvent to remove the surface impurities, and then dissolve the crystals with a small amount of hot solvent, and repeat the low-temperature crystallization step to further improve the crystal purity;

[0054] Step Five: Drying

[0055] 3) If a spray dryer is used, set the inlet air temperature at 160 - 180 °C, the outlet air temperature at 80 - 90 °C, and the feeding speed at 5 - 10 mL / min. Spray the concentrated liquid into the drying tower through a spraying device, and it will be quickly dried into a powdery product under the action of hot air;

[0056] 4) If the concentrated liquid is placed in a vacuum freeze dryer, lower the temperature to -40 °C to -60 °C, the vacuum degree ≤ 50 Pa, and the drying time is 24 - 48 hours, so that the moisture in the solution is sublimated and removed at low temperature to obtain a dried product;

[0057] Step Six: Finished Product Packaging and Storage

[0058] Pack the dried product, select appropriate packaging materials, including moisture-proof and light-proof aluminum foil bags or glass bottles. The packaged finished product should be stored in a cool, dry, and light-proof environment to prevent the product from getting damp, oxidized, or affected by light and deteriorating, and to ensure the quality and stability of the product.

[0059] Advantages of the Present Invention:

[0060] The extraction process and method of plateau plants of the present invention adopt vacuum freeze drying or low-temperature hot air circulation drying, avoiding the destruction of heat-sensitive components by high temperature. Heat-sensitive components include vitamins, enzymes, volatile oils, etc., ensuring the integrity and stability of active components; according to the polarity of the target components, 60% - 70% ethanol, water, or supercritical CO 2 is accurately selected as the solvent, ensuring the efficient dissolution of different polar components, improving the pertinence and effectiveness of extraction; through ultrasonic or microwave-assisted technology, the dissolution of active components is accelerated, significantly improving the extraction efficiency, while reducing the solvent consumption and extraction time; through microfiltration membrane filtration, plate and frame filtration, and high-speed centrifugal separation, impurities are gradually removed to obtain a pure extraction solution; using resin adsorption technology, appropriate resins are selected according to the polarity of the target components, and eluted with ethanol solutions of different concentrations to achieve the efficient separation and purification of the target components: two methods of spray drying and vacuum freeze drying can be selected according to the product characteristics to ensure that the finished product has low water content and good stability, and the overall process has strong compatibility, meeting the production requirements of different scales. Description of the Drawings

[0061] Figure 1 Shown is a flow chart of the process and method for protecting components during the extraction of plateau plants of the present invention. Detailed Embodiments

[0062] The present invention will be further described below in conjunction with the drawings and embodiments.

[0063] Example 1

[0064] When using the process of this technical solution, the steps are as follows:

[0065] SI: Raw material pretreatment

[0066] SI1: Cleaning

[0067] Rinse the raw materials with running water to remove sediment and surface contaminants;

[0068] SI2: Drying

[0069] Use a vacuum freeze dryer or a hot air circulation oven for drying treatment to avoid destroying heat-sensitive components at high temperatures. The temperature of vacuum freeze drying is between -40°C and -60°C, and the vacuum degree ≤ 50 Pa; the temperature of hot air drying ≤ 45°C;

[0070] S13: Crushing

[0071] Use an ultrafine crusher to crush the raw materials to 80 - 120 mesh;

[0072] For raw materials with more oil, including pine needles, use n-hexane for degreasing treatment to reduce the interference of fat-soluble impurities; select activated carbon adsorption for decolorization treatment to remove chlorophyll pigments;

[0073] S2: Extraction treatment

[0074] Select 60% - 70% ethanol, water or supercritical CO 2 as the solvent. The extraction equipment specifically uses a multi-functional extraction tank with a condensation reflux device or a supercritical extraction device, and uses ultrasonic or microwave-assisted technology to efficiently extract the target components, reducing the degradation of heat-sensitive substances. When ethanol reflux extraction is carried out, the temperature is 40 - 60°C, the time is 1 - 3 hours, and it is dynamically circulated; supercritical CO 2 During extraction, the pressure is 25 MPa, the temperature is 40°C, the time is 2 - 4 hours. When ultrasonic assistance is used, the frequency is 20 - 40 kHz, the power density is 0.1 - 0.5 W / cm 2 , the time is 20 - 40 minutes. When microwave assistance is used, the intermittent mode is adopted, the power is 500 - 800 W, and the time is 5 - 15 minutes;

[0075]

[0076] Among them, C 提取液 is the concentration of the extract, V 提取液 is the volume of the extract, C 原料 is the content of the target component in the raw material, m 原料 is the mass of the raw material;

[0077] S3: Solid-liquid separation treatment

[0078] Filtering treatment is carried out using a 0.45 μm microporous membrane filter or a plate and frame filter press, with a pressure ≤ 0.3 MPa. After filtration, start a high-speed centrifuge for separation, with a rotation speed of 4000 - 8000 r / min, a time of 10 - 20 minutes, and a temperature ≤ 25°C;

[0079] S4: Purification treatment

[0080] S41: Concentrate or dilute the extract to a concentration of 0.5 - 2 mg / mL, filter or centrifuge to remove solid impurities, pass through the adsorption column at a flow rate of 1 - 3 BV / h, collect the effluent for standby, elute successively with ethanol solutions of 30%, 40%, 50%, 60%, and 70% at a flow rate of 1 - 2 BV / h. The eluate of each ethanol concentration is collected separately, the content of the target component is detected, and the eluate corresponding to the target component peak is combined; Soak the AB-8 or D101 resin in ethanol for 24 hours, after swelling, rinse with distilled water until there is no alcohol smell, load the resin into the adsorption column, and rinse with 2 - 3 bed volumes of distilled water at a flow rate of 2 - 3 BV / h to stabilize the resin bed layer. The adsorption capacity formula is:

[0081]

[0082] Among them, Q is the adsorption capacity, C 0 is the initial concentration, C e is the equilibrium concentration, V is the solution volume, m 树脂 is the resin mass;

[0083] S42: Concentrate the combined eluate to 1 / 5 - 1 / 10 of the original volume using a rotary evaporator, with a temperature ≤ 50°C and a vacuum degree ≥ 0.09 MPa. Prepare a solvent according to the ethanol-water volume ratio of 1:1 - 1:5, slowly add the concentrated solution to the solvent, stir to dissolve, transfer the solution to an ice-water bath or a low-temperature refrigerator at -5°C to 10°C, let it stand for several hours to several days until crystals precipitate, filter the crystals, wash them with a cold ethanol-water solvent, and dissolve the crystals with a small amount of hot solvent, repeat the low-temperature crystallization step to improve the purity;

[0084] S5: Drying

[0085] Carry out drying operation using a spray dryer or a vacuum freeze dryer. The inlet air temperature for spray drying is 160 - 180°C, the outlet air temperature is 80 - 90°C, the feed rate is 5 - 10 mL / min, the temperature for vacuum freeze drying is -40°C to -60°C, the vacuum degree ≤ 50 Pa, and the time is 24 - 48 hours;

[0086] S6: Finished product packaging and storage.

[0087] A method for protecting components during the extraction of plateau plants, characterized by including the process for protecting components during the extraction of plateau plants as shown above, and its steps are as follows:

[0088] Step 1: Raw material pretreatment

[0089] 1) Place the collected plateau plant raw materials in a cleaning device, and let the flowing water continuously wash the raw materials. The water flow rate needs to be controlled within a certain range, which can not only ensure that the sediment, dust and other pollutants attached to the surface of the raw materials are thoroughly washed, but also will not cause excessive erosion and damage to the raw materials;

[0090] 2) Quickly put the washed raw materials into a vacuum freeze dryer. First, lower the temperature inside the device to between -40°C and -60°C. At such a low temperature, the water in the raw materials quickly freezes into ice. Subsequently, evacuate to make the vacuum degree reach ≤50 Pa. At this time, the ice directly sublimes into water vapor and is pumped out, thus realizing drying; if a hot air circulation oven is used, the temperature needs to be strictly controlled at ≤45°C. Place the raw materials evenly on the oven tray, and use the hot air circulation system to make the hot air evenly blow on the raw materials to take away the moisture and realize drying;

[0091] 3) Put the dried raw materials into an ultrafine pulverizer, adjust the pulverizer parameters, pulverize the raw materials to 80 - 120 mesh. After pulverization is completed, immediately transfer the powder to a sealed container for storage;

[0092] Step 2: Extraction treatment

[0093] 1) Select a suitable solvent according to the polarity of the target component in the plateau plant. If the polarity of the target component is moderate, 60% - 70% ethanol is selected; for components with larger polarity, water is a suitable solvent; for some components that are sensitive to temperature and require efficient extraction, supercritical CO 2 is an ideal choice;

[0094] 2) If ethanol is used, add the pulverized raw materials and the selected solvent to a multi-functional extraction tank in a certain proportion. When using ethanol reflux extraction, control the temperature at 40 - 60°C, the reflux time at 1 - 3 hours, and maintain dynamic circulation. At the same time, turn on the ultrasonic assistance technology, set the frequency at 20 - 40 kHz, the power density at 0.1 - 0.5 W / cm 2 ², and the action time at 20 - 40 minutes; or use the microwave assistance technology, operate in an intermittent mode, with a power of 500 - 800 W and an action time of 5 - 15 minutes;

[0095] 3) When using a supercritical extraction device for supercritical CO 2 extraction, set the pressure at 25 MPa, the temperature at 40°C, and the extraction time at 2 - 4 hours;

[0096] Step 3: Solid-liquid separation treatment

[0097] 1) Filter the extracted mixture through a 0.45 μm microporous membrane filter or a plate and frame filter press. During the filtration process, control the pressure ≤ 0.3 MPa to prevent damage to the filter membrane or affect the filtration effect caused by excessive pressure, and preliminarily separate the solid impurities in the mixture to obtain a relatively clear liquid, preparing for subsequent centrifugal separation;

[0098] 2) Transfer the filtered liquid to a high-speed centrifuge, set the rotation speed to 4000 - 8000 r / min, the separation time to 10 - 20 minutes, and at the same time control the temperature ≤ 25 °C to further separate the fine particles and residual impurities in the liquid, and make the solid-liquid separation more thorough through centrifugal force to obtain a relatively pure extract;

[0099] Step Four: Purification Treatment

[0100] 1) Select AB-8 or D101 resin, soak it in ethanol for 24 hours to fully swell it, and then rinse the resin with distilled water until no ethanol smell is detected in the rinsing liquid. Load the treated resin into the adsorption column, and then rinse it with 2 - 3 bed volumes of distilled water at a flow rate of 2 - 3 BV / h to stabilize the resin bed layer;

[0101] 2) Concentrate or dilute the extract to a concentration of 0.5 - 2 mg / mL. First, filter or centrifuge to remove the solid impurities in it, and then pass the treated extract through the adsorption column at a flow rate of 1 - 3 BV / h, and collect the effluent for standby. Elute the adsorption column with 30%, 40%, 50%, 60%, and 70% ethanol solutions in turn, control the elution flow rate at 1 - 2 BV / h, collect the eluate of each ethanol concentration segment separately, and by detecting the content of the target component in each segment of the eluate, merge the eluate corresponding to the target component peak, and use the adsorption and desorption characteristics of the resin for different components to further separate the target component from other impurities in the extract and improve the purity of the target component;

[0102] 3) Concentrate the combined eluate with a rotary evaporator, control the temperature ≤ 50 °C, and the vacuum degree ≥ 0.09 MPa to reduce the volume of the concentrated liquid to 1 / 5 - 1 / 10 of the original volume;

[0103] 4) Prepare a solvent according to the ethanol-water volume ratio of 1:1 - 1:5, slowly add the concentrated liquid to this solvent, and stir it to fully dissolve it. Then transfer the solution to an ice-water bath or a low-temperature refrigerator at -5 °C to 10 °C, and let it stand for several hours to several days to wait for crystal precipitation;

[0104] 5) After filtering to obtain the crystals, wash the crystals with a cold ethanol-water solvent to remove the surface impurities, and then dissolve the crystals with a small amount of hot solvent, and repeat the low-temperature crystallization step to further improve the purity of the crystals;

[0105] Step Five: Drying

[0106] 5) If a spray dryer is used, set the inlet air temperature at 160 - 180°C, the outlet air temperature at 80 - 90°C, and the feeding speed at 5 - 10 mL / min. Spray the concentrated solution into the drying tower through a spraying device and quickly dry it into a powdery product under the action of hot air;

[0107] 6) If the concentrated solution is placed in a vacuum freeze dryer, lower the temperature to -40°C to -60°C, the vacuum degree ≤ 50 Pa, and the drying time is 24 - 48 hours to sublime and remove the moisture in the solution at low temperature to obtain a dried product;

[0108] Step Six: Finished product packaging and storage

[0109] Pack the dried product, select appropriate packaging materials, including moisture-proof and light-proof aluminum foil bags or glass bottles. The packaged finished product should be stored in a cool, dry, and light-proof environment to prevent the product from getting damp, oxidized, or affected by light and deteriorating, and to ensure the quality and stability of the product.

[0110] Experimental example

[0111] Select the same plateau plant, such as saffron. There are two groups in total for the method of Example 1 and the traditional process as Example 2. The traditional process is carried out by means of normal temperature drying, hot reflux extraction, filtration separation, and normal temperature crystallization, and is detected by detection equipment. The data results are as follows;

[0112]

Claims

1. A process for protecting components in the process of plateau plant extraction, characterized in that: The steps are as follows: SI: Raw material pretreatment SI1: Cleaning Use running water to wash the raw materials to remove sediment and surface pollutants; SI2: Drying Use a vacuum freeze dryer or hot air circulation oven for drying to avoid high temperature damage to heat-sensitive components; S13: Smash Use an ultra-fine grinder to grind the raw materials into 80-120 mesh; S2: Extraction treatment According to the polarity of the components, 60%-70% ethanol, water or supercritical CO2 is selected as the solvent. The extraction equipment specifically uses a multifunctional extraction tank with a condensation reflux device or a supercritical extraction device, and uses ultrasonic or microwave-assisted technology to efficiently extract the target components and reduce the degradation of heat-sensitive substances; S3: Solid-liquid separation treatment Use a 0.45μm microporous membrane filter or a plate-and-frame filter press for filtration, with a pressure of ≤0.3MPa. After filtration, start a high-speed centrifuge for separation at a speed of 4000-8000r / min, for 10-20 minutes, and a temperature of ≤25°C; S4: Purification S41: Concentrate or dilute the extract to a concentration of 0.5-2 mg / mL, filter or centrifuge to remove solid impurities, pass the extract through an adsorption column at a flow rate of 1-3 BV / h, collect the effluent for later use, and elute with 30%, 40%, 50%, 60%, and 70% ethanol solutions in sequence at a flow rate of 1-2 BV / h. Collect the eluates of each ethanol concentration separately, detect the content of the target component, and combine the eluates corresponding to the peak of the target component; S42: Concentrate the combined eluate to 1 / 5-1 / 10 of the original volume using a rotary evaporator, the temperature is ≤50°C, the vacuum degree is ≥0.09MPa, prepare a solvent according to the ethanol-water volume ratio of 1:1-1:5, slowly add the concentrate to the solvent, stir to dissolve, transfer the solution to an ice water bath or a low-temperature refrigerator at -5°C to 10°C, and let it stand for several hours to several days until crystals precipitate; S5: Dry Use a spray dryer or vacuum freeze dryer for drying; S6: Finished product packaging and storage.

2. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: The temperature of vacuum freeze drying in SI2 is between -40℃ and -60℃, and the vacuum degree is ≤50Pa; the temperature of hot air drying is ≤45℃.

3. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In SI, for raw materials containing more oil, including pine needles, n-hexane degreasing is used for degreasing to reduce the interference of fat-soluble impurities; activated carbon adsorption is used for decolorization to remove chlorophyll pigments.

4. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In S2, the ethanol reflux extraction is carried out at a temperature of 40-60°C, for 1-3 hours, with dynamic circulation; in supercritical CO2 extraction, the pressure is 25MPa, the temperature is 40°C, and the time is 2-4 hours.

5. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: The frequency of ultrasound-assisted S2 is 20-40kHz, and the power density is 0.1-0.5W / cm 2 , time 20-40 minutes, use intermittent mode for microwave assistance, power 500-800W, time 5-15 minutes.

6. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In S2: Among them, C 提取液 is the concentration of the extract, V 提取液 is the volume of the extract, C 原料 is the target component content in the raw material, m 原料 For the quality of raw materials.

7. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In S41, AB-8 or D101 resin is soaked in ethanol for 24 hours, and after swelling, it is rinsed with distilled water until there is no alcohol smell. The resin is loaded into the adsorption column and rinsed with 2-3 times the bed volume of distilled water at a flow rate of 2-3BV / h to stabilize the resin bed. The adsorption capacity formula is: Where Q is the adsorption capacity, C0 is the initial concentration, and C e is the equilibrium concentration, V is the volume of the solution, m 树脂 For the resin quality.

8. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In S42, the crystals are filtered, washed with a cold ethanol-water solvent, and dissolved with a small amount of hot solvent, and the low-temperature crystallization step is repeated to improve the purity.

9. The process for protecting components in the process of plateau plant extraction according to claim 1, characterized in that: In S5, the inlet air temperature of the spray drying is 160-180°C, the outlet air temperature is 80-90°C, the feed rate is 5-10mL / min, the vacuum freeze drying temperature is -40°C to -60°C, the vacuum degree is ≤50Pa, and the time is 24-48 hours.

10. The method for protecting components in the process of plateau plant extraction according to claim 1, characterized in that The process comprises the following steps: Step 1: Raw material pretreatment 1) Place the collected plateau plant materials in the cleaning equipment and let the flowing water continuously wash the materials. The water flow rate must be controlled within a certain range to ensure that the sand, dust and other pollutants attached to the surface of the materials are thoroughly washed away without causing excessive washing and damage to the materials; 2) The cleaned raw materials are quickly placed in a vacuum freeze dryer, and the temperature inside the equipment is first reduced to between -40°C and -60°C. At such a low temperature, the moisture in the raw materials is quickly frozen into ice. Subsequently, the vacuum is evacuated to a vacuum degree of ≤50Pa, at which time the ice is directly sublimated into water vapor and extracted, thereby achieving drying. If a hot air circulation oven is used, the temperature must be strictly controlled to ≤45°C, and the raw materials are evenly placed on the oven tray. The hot air circulation system is used to evenly blow hot air over the raw materials to remove moisture and achieve drying. 3) Put the dried raw materials into the ultrafine pulverizer, adjust the parameters of the pulverizer, and pulverize the raw materials into 80-120 mesh. After the pulverization is completed, immediately transfer the powder to a sealed container for storage; Step 2: Extraction 1) Select the appropriate solvent according to the polarity of the target component in the plateau plants. If the target component has moderate polarity, use 60%-70% ethanol; for components with greater polarity, water is a suitable solvent; for some components that are sensitive to temperature and require efficient extraction, supercritical CO2 is an ideal choice; 2) If ethanol is used, add the crushed raw materials and the selected solvent into the multifunctional extraction tank in a certain proportion. When ethanol reflux extraction is used, the temperature is controlled at 40-60°C, the reflux time is 1-3 hours, and the dynamic cycle is maintained. At the same time, the ultrasonic auxiliary technology is turned on, the frequency is set at 20-40kHz, and the power density is 0.1-0.5W / cm 2 , action time 20-40 minutes; or use microwave-assisted technology, run in intermittent mode, power 500-800W, action time 5-15 minutes; 3) When using a supercritical extraction device for supercritical CO2 extraction, the set pressure is 25MPa, the temperature is 40°C, and the extraction time is 2-4 hours; Step 3: Solid-liquid separation 1) The mixed solution after extraction is filtered through a 0.45 μm microporous membrane filter or a plate and frame filter press. During the filtering process, the pressure is controlled to be ≤0.3 MPa to prevent excessive pressure from damaging the filter membrane or affecting the filtering effect. Solid impurities in the mixed solution are initially separated to obtain a relatively clear liquid in preparation for subsequent centrifugal separation; 2) The filtered liquid is transferred to a high-speed centrifuge, the speed is set to 4000-8000r / min, the separation time is 10-20 minutes, and the temperature is controlled to be ≤25°C, so as to further separate the fine particles and residual impurities in the liquid, and the solid and liquid are separated more thoroughly by centrifugal force to obtain a relatively pure extract; Step 4: Purification 1) Select AB-8 or D101 resin, soak it in ethanol for 24 hours to fully swell it, then rinse the resin with distilled water until no ethanol taste is detected in the rinse solution, load the treated resin into the adsorption column, and then rinse it with 2-3 times the bed volume of distilled water at a flow rate of 2-3BV / h to stabilize the resin bed; 2) The extract is concentrated or diluted to a concentration of 0.5-2 mg / mL, first filtered or centrifuged to remove solid impurities therein, then the treated extract is passed through an adsorption column at a flow rate of 1-3 BV / h, the effluent is collected for standby use, and the adsorption column is eluted with 30%, 40%, 50%, 60%, and 70% ethanol solutions in sequence, the elution flow rate is controlled at 1-2 BV / h, and the eluates of each ethanol concentration are collected separately, and the content of the target component in each eluate is detected, and the eluates corresponding to the peak of the target component are combined, and the adsorption and desorption characteristics of the resin for different components are used to further separate the target component in the extract from other impurities, thereby improving the purity of the target component; 3) Concentrate the combined eluent using a rotary evaporator, control the temperature at ≤50°C and the vacuum degree at ≥0.09MPa, and reduce the volume of the concentrate to 1 / 5-1 / 10 of the original volume; 4) Prepare a solvent according to the volume ratio of ethanol to water of 1:1-1:5, slowly add the concentrate to the solvent, stir to fully dissolve it, then transfer the solution to an ice water bath or a low-temperature refrigerator at -5°C to 10°C, and let it stand for several hours to several days to wait for crystals to precipitate; 5) After filtering to obtain the crystals, wash the crystals with a cold ethanol-water solvent to remove surface impurities, then dissolve the crystals with a small amount of hot solvent, and repeat the low-temperature crystallization step to further improve the purity of the crystals; Step 5: Drying 1) If a spray dryer is used, set the inlet air temperature to 160-180°C, the outlet air temperature to 80-90°C, and the feed rate to 5-10mL / min. Spray the concentrated liquid into the drying tower through the spray device and quickly dry it into a powdery product under the action of hot air; 2) If the concentrated solution is placed in a vacuum freeze dryer, the temperature is reduced to -40°C to -60°C, the vacuum degree is ≤50Pa, and the drying time is 24-48 hours, so that the water in the solution is sublimated and removed at low temperature to obtain a dry product; Step 6: Finished product packaging and storage Package the dried product and choose appropriate packaging materials, including moisture-proof and light-proof aluminum foil bags or glass bottles. The packaged finished products should be stored in a cool, dry, and light-proof environment to prevent the product from being affected by moisture, oxidation, or deterioration due to light, so as to ensure the quality and stability of the product.

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