阅读说明：本技术 一种牛蒡子活性成分的工业化制备方法 (Industrial preparation method of active ingredients of burdock ) 是由 张瑜 冀瑜 王晓莹 肖红 耿道元 于 2021-01-07 设计创作，主要内容包括：本发明涉及一种牛蒡子活性成分的工业化制备方法,解决现有工艺因成本高、收率低或工艺过程复杂等原因而导致的不适于工业生产的缺陷,包括灭酶、超临界萃取、萃取物的分离纯化及萃取渣的分离纯化等步骤,本发明工艺简单,收率高,且实现原料的综合利用,从而降低单个产品的生产成本,更适于工业化生产。(The invention relates to an industrial preparation method of an active ingredient of burdock, which solves the defect that the prior art is not suitable for industrial production due to high cost, low yield or complex process, and the like.)

1. The industrial preparation method of the active ingredient of the burdock is characterized by comprising the following steps:

step 1, inactivating enzyme;

firstly, pressing the burdock raw material into a blank by using a blank pressing machine, and then cooking and inactivating enzyme for 5-10 min;

step 2, supercritical extraction;

extracting the raw materials subjected to enzyme deactivation in the step 1 by using supercritical carbon dioxide to respectively obtain an extract and extraction residues;

when supercritical carbon dioxide extraction is carried out, the carrying agent is toluene or xylene, and the using amount of the carrying agent is 3-5% of the mass of the inactivated raw material;

step 3, separating and purifying the extract;

step 3.1, dissolving the extract obtained in the step 2 by using No. six solvent naphtha, wherein the mass of the No. six solvent naphtha is 3-5 times of that of the extract, stirring, filtering, and respectively collecting a No. six solvent oil layer and insoluble substances;

step 3.2, adding 3-5 times of mixed solvent into the insoluble substance obtained in the step 3.1, wherein the mixed solvent is the mixed solvent of No. six solvent oil and ethanol; stirring, standing, layering, and collecting ethanol layer and No. six solvent oil layer respectively;

step 3.3, concentrating the ethanol layer collected in the step 3.2 to an alcohol degree of 60-70%, adding activated carbon into the concentrated solution for decolorization, then filtering, concentrating the filtrate to a specific gravity of 1.1-1.15, refrigerating for crystallization, filtering, adding isopropanol of which the wet weight is 1-1.5 times of that of the filtrate into the filtered crystals, stirring, filtering, and drying filter residues to obtain more than 98% of arctigenin;

step 3.4, combining the No. six solvent oil layers collected in the step 3.1 and the step 3.2, adding activated carbon for decolorization, filtering, and concentrating the filtrate to obtain the burdock oil;

step 4, separating and purifying the extraction residues;

crushing the extraction residue obtained in the step 2 to 60-80 meshes, stirring and extracting at normal temperature by using n-butanol with the mass of 6-8 times of that of the extraction residue, collecting the extraction solution, concentrating the extraction solution to the alcohol degree of 5-10%, adding a mixed adsorbent with the mass of 20-30% of the extraction residue, stirring, filtering, collecting filter residues, stirring and dissolving by using water saturated ethyl acetate with the mass of 5-10 times of that of the extraction residue, filtering, combining and concentrating the filtrate to the specific gravity of 1.1-1.15, refrigerating, crystallizing, filtering, rinsing the filter residues by using dichloromethane, and drying to obtain the arctiin with the concentration of more than 98%.

2. The industrial preparation method of the burdock active ingredient according to claim 1, which is characterized by comprising the following steps: in the mixed solvent in the step 3.2, the ethanol is 80% by mass, and the volume ratio of the No. six solvent oil to the 80% by mass is 1: 1-3.

3. The industrial preparation method of the burdock active ingredient according to claim 2, which is characterized in that: the volume ratio of the No. six solvent oil to the ethanol with the mass fraction of 80 percent is 1: 2.

4. The industrial preparation method of the burdock active ingredient according to claim 1, which is characterized by comprising the following steps: the mass of the mixed adsorbent in the step 4 is 25% of that of the extraction slag; the mass ratio of the activated carbon to the neutral alumina in the mixed adsorbent is 1: 2-5.

5. The industrial preparation method of the burdock active ingredient according to claim 4, which is characterized by comprising the following steps: the mass ratio of the activated carbon to the neutral alumina in the mixed adsorbent is 1: 3.

6. The industrial preparation method of the burdock active ingredient according to claim 1, which is characterized by comprising the following steps: and 3.3, adding activated carbon into the concentrated solution for decoloring, wherein the mass of the activated carbon is 5% of that of the extract obtained in the step 2, and the decoloring time is 2 h.

7. The industrial preparation method of the burdock active ingredient according to claim 1, which is characterized by comprising the following steps: in step 3.4, the mass of the activated carbon is 10% of the mass of the combined solution of the solvent oil layer six collected in step 3.1 and step 3.2, and the decoloring time is 1 h.

8. The industrial preparation method of the burdock active ingredient according to any one of claims 1 to 7, characterized by comprising the following steps: in the step 2, when supercritical carbon dioxide extraction is carried out, the extraction pressure is 30-35MPa, the extraction temperature is 40-45 ℃, the extraction time is 2-5h, and the carbon dioxide flow is 10-12 Kg/h.

Technical Field

The invention relates to a method for separating and purifying burdock oil, arctiin and aglycon with high yield and low cost, which realizes the comprehensive utilization of raw materials and is suitable for industrial production.

Background

The fructus arctii is dry mature fruit of arctium lappa which is a biennial herb of the family Compositae, has the effects of dispelling wind and heat, promoting eruption and detoxifying, and is a common medicine of traditional Chinese medicines. The main active ingredients in fructus Arctii include fructus Arctii oil, arctiin and arctigenin. The fructus Arctii has a content of 18%, and has effects of preventing cancer, relieving respiratory condition, improving renal function, and resisting oxidation; arctiin and arctigenin have multiple physiological activities of resisting tumor, reducing blood sugar, resisting bacteria, resisting virus, regulating immunity and the like, and are a traditional Chinese medicine with great development significance.

In patent CN 105669797 a, a method for separating burdock oil, arctiin, arctigenin E and arctigenin H from burdock is involved, which comprises steps of firstly performing supercritical degreasing to obtain burdock oil and degreased powder, then performing ethanol extraction, dichloromethane extraction, silica gel column chromatography, and dichloromethane-methanol gradient elution to respectively obtain the above components. Although the patent adopts supercritical extraction, arctiin and aglycon are not separated, but only have the degreasing effect, so that the subsequent separation is difficult, the production period of silica gel column chromatography is too long, the cost is too high, and the industrial production is not facilitated.

Patent CN 1021101876A mentions that 98% arctiin is obtained by adopting supercritical extraction raw material, ethanol as entrainer, countercurrent extraction residue by adopting ethyl acetate, macroporous resin separation and acetone crystallization. Because ethanol is used as an entrainer during supercritical, part of arctiin is lost, the yield is low and is only 0.5%, the production cost is too high, and the method is not suitable for industrial production.

Patent CN 109053829B mentions a method for separating and purifying arctiin by reduced pressure method, which comprises extracting raw materials with ethanol, removing impurities with resin, concentrating the adsorption effluent, and precipitating with water to obtain arctiin 94% with yield of 4.2%. The patent needs to adopt a specific method to prepare the resin, the process is too complex, the cost is high, the construction period is long, and the obtained product has low yield and content and is not suitable for industrial production.

Patent CN 102351926B mentions that 90% -95% of arctiin is obtained by water extraction, no concentration, direct macroporous adsorption resin separation, ethanol elution, activated carbon or polyamide decoloration and acetone crystallization. The arctiin is a lignan compound and is unstable, so that the extraction with water can cause a great amount of degradation of the components, so that the yield is only about 2.9%; and the macroporous adsorption resin has long production period and large solution consumption, so that the production cost is high, and the macroporous adsorption resin is not suitable for industrial production.

Patent CN 103936803A mentions that ethanol extraction, concentration, stirring and impurity removal of a petroleum ether-ethyl acetate mixed solvent, dichloromethane extraction, concentration, and crystallization of methanol and isopropyl ether are adopted to obtain 98% arctiin. Although the process is simple, the isopropyl ether is adopted for crystallization, so that the process is too dangerous, has too high requirements on operators and equipment, and is not practical for industrial production.

Disclosure of Invention

In order to solve the defect that the process is not suitable for industrial production due to high cost, low yield, complex process and the like, the invention provides the industrial preparation method of the burdock active ingredient.

The technical scheme of the invention is to provide an industrial preparation method of an active component of burdock, which is characterized by comprising the following steps:

step 1, inactivating enzyme;

firstly, pressing the burdock raw material into a blank by using a blank pressing machine, and then cooking and inactivating enzyme for 5-10 min;

step 2, supercritical extraction;

extracting the raw materials subjected to enzyme deactivation in the step 1 by using supercritical carbon dioxide to respectively obtain an extract and extraction residues;

when supercritical carbon dioxide extraction is carried out, the carrying agent is toluene or xylene, and the using amount of the carrying agent is 3-5% of the mass of the inactivated raw material;

step 3, separating and purifying the extract;

step 3.1, dissolving the extract obtained in the step 2 by using No. six solvent naphtha, wherein the mass of the No. six solvent naphtha is 3-5 times of that of the extract, stirring, filtering, and respectively collecting a No. six solvent oil layer and insoluble substances;

step 3.2, adding 3-5 times of mixed solvent into the insoluble substance obtained in the step 3.1, wherein the mixed solvent is the mixed solvent of No. six solvent oil and ethanol; stirring, standing, layering, and collecting ethanol layer and No. six solvent oil layer;

step 3.3, concentrating the ethanol layer collected in the step 3.2 to an alcohol degree of 60-70%, adding activated carbon into the concentrated solution for decolorization, then filtering, concentrating the filtrate to a specific gravity of 1.1-1.15, refrigerating for crystallization, filtering, adding isopropanol of which the wet weight is 1-1.5 times of that of the filtrate into the filtered crystals, stirring, filtering, and drying filter residues to obtain more than 98% of arctigenin;

step 3.4, combining the No. six solvent oil layers collected in the step 3.1 and the step 3.2, adding activated carbon for decolorization, filtering, and concentrating the filtrate to obtain the burdock oil;

step 4, separating and purifying the extraction residues;

crushing the extraction residue obtained in the step 2 to 60-80 meshes, stirring and extracting at normal temperature by using n-butanol with the mass of 6-8 times of that of the extraction residue, collecting the extraction solution, concentrating the extraction solution to the alcohol degree of 5-10%, adding a mixed adsorbent with the mass of 20-30% of the extraction residue, stirring, filtering, collecting filter residues, stirring and dissolving by using water saturated ethyl acetate with the mass of 5-10 times of that of the extraction residue, filtering, combining and concentrating the filtrate to the specific gravity of 1.1-1.15, refrigerating, crystallizing, filtering, rinsing the filter residues by using dichloromethane, and drying to obtain the arctiin with the concentration of more than 98%.

Further, in order to realize good separation of the arctigenin and the burdock oil, in the mixed solvent of the step 3.2, the ethanol is 80% by mass, and the volume ratio of the No. six solvent oil to the 80% by mass is 1: 1-3.

Further, in order to satisfy the purity and recovery rate of arctigenin, the volume ratio of the solvent oil No. six to 80% by mass of ethanol is 1: 2.

Further, in order to realize the separation of the arctiin from the high-polarity impurities, the mass of the mixed adsorbent in the step 4 is 25% of the mass of the extraction residue; the mass ratio of the activated carbon to the neutral alumina in the mixed adsorbent is 1: 2-5.

Further, in order to satisfy the purity and recovery rate of arctiin, the mass ratio of activated carbon to neutral alumina in the mixed adsorbent is 1: 3.

In order to further remove pigment impurities in the arctigenin, in the step 3.3, activated carbon is added into the concentrated solution for decolorization, the mass of the activated carbon is 5% of the mass of the extract obtained in the step 2, and the decolorization time is 2 hours.

Further, in order to improve the clarity and color of the burdock oil, in step 3.4, the mass of the activated carbon is 10% of the mass of the combined solution of the solvent oil layer six collected in step 3.1 and step 3.2, and the decoloring time is 1 h.

Further, in the step 2, when the supercritical carbon dioxide is used for extraction, the extraction pressure is 30-35MPa, the extraction temperature is 40-45 ℃, the extraction time is 2-5h, and the carbon dioxide flow is 10-12 Kg/h.

The invention has the beneficial effects that:

1. the great amount of glucosidase exists in the burdock, which causes degradation of arctiin in the production process, so that the arctiin is well protected by cooking to inactivate the enzyme before extraction, the recovery rate of active ingredients is more than 85%, and the key step of the invention is high arctiin yield.

2. The invention realizes the separation of the great burdock oil, the arctigenin and the arctiin by a supercritical extraction process and taking toluene or xylene as a carrying agent, has simple process and easy operation, and is suitable for industrial production.

3. The supercritical extract is stirred and dissolved by the solvent oil VI to realize the separation of the burdock oil and the arctigenin, so that the burdock oil can be obtained, the arctigenin can be well purified, the separation of the arctigenin and the burdock oil is realized by the gasoline and the 80% ethanol, the selectivity is good, the operation is simple, the yield is high, and the recovery rate of the active ingredients of the arctigenin can reach more than 80%.

4. The extraction residue is separated from impurities by the mixed adsorbent of activated carbon and neutral alumina, the selectivity is good, the operation is simple, and the resinification reaction in the treatment process is avoided. High yield and low cost, and is suitable for industrial production.

5. The invention adopts a plurality of technologies of enzyme deactivation, supercritical extraction, mixed solvent extraction, adsorption, analysis and the like to be used in a combined way, and develops the active ingredients in the burdock raw material to the utmost extent. Through the innovation of the process, the separation of the burdock oil, the arctigenin and the arctiin is realized, the resource utilization is maximized, the energy consumption is reduced, the production cost of a single product is greatly reduced, and the production efficiency is greatly improved.

Drawings

FIG. 1 is a liquid phase spectrum of the burdock fruit raw material in the fifth embodiment;

FIG. 2 is a liquid phase diagram of the supercritical extraction residue of the burdock fruit raw material in the fifth embodiment;

FIG. 3 is a liquid phase chromatogram of n-butanol extract of fructus Arctii in example V;

FIG. 4 is a liquid phase spectrum of the five examples after adsorption by the mixed adsorbent of fructus Arctii activated carbon and neutral alumina;

FIG. 5 is a liquid phase diagram of arctiin product of example V;

fig. 6 is a liquid phase diagram of arctigenin product in example five.

Detailed Description

The invention is further described with reference to the following figures and specific embodiments.

Example one

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and the enzyme is cooked and inactivated for 5 min. Then, toluene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 30MPa, the extraction temperature is 45 ℃, the extraction time is 2 hours, the carbon dioxide flow is 10Kg/h, and the carrying agent dosage is 3 percent of the raw material mass.

The supercritical extract is prepared by stirring 3 times of number six solvent oil for 30min, filtering, and collecting number six solvent oil layer and insoluble substance respectively.

Adding 5 times of mixed solvent (No. six solvent oil: 80% ethanol 1:1) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to alcohol degree of 65%, adding active carbon with extract quality of 5% for decolorizing for 2h, filtering, concentrating the filtrate to specific gravity of 1.12, refrigerating for crystallization, filtering, stirring the crystal with wet isopropanol with equal mass, filtering, crystallizing, and drying to obtain 346g arctigenin, with liquid phase detection content of 98.5%.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.73Kg of burdock oil.

Pulverizing supercritical extraction residue to 60-80 mesh, extracting with 8 times of n-butanol at normal temperature under stirring for 2 times, each for 1.5 hr, concentrating the extractive solution to alcohol degree of 5%, adding 30% of mixed adsorbent (activated carbon: neutral alumina 1:5) of extraction residue, stirring for 2 hr, filtering, collecting mixed adsorbent, dissolving with 10 times of water saturated ethyl acetate under stirring for 2 times, each for 2 hr, filtering, mixing filtrates, concentrating to specific gravity of 1.134, refrigerating for crystallization, filtering, rinsing with dichloromethane, and drying to obtain arctiin 2.90Kg, with liquid phase content of 98.3%.

Example two

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and enzyme is steamed and inactivated for 10 min. The xylene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 35MPa, the extraction temperature is 40 ℃, the extraction time is 5 hours, the carbon dioxide flow is 12Kg/h, and the carrying agent dosage is 5 percent of the raw material mass.

The supercritical extract is firstly stirred for a certain time by using No. six solvent oil with the mass being 5 times that of the supercritical extract, and then filtered, and the No. six solvent oil layer and insoluble substances are respectively collected.

Adding 3 times of mixed solvent (No. six solvent oil: 80% ethanol: 1:3) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to alcohol degree of 70%, adding active carbon with extract quality of 5% for decolorizing for 2h, filtering, concentrating the filtrate to specific gravity of 1.143, refrigerating for crystallization, filtering, stirring the crystallization with isopropanol with wet weight of 1.5 times, filtering, crystallizing and drying to obtain 358g arctigenin, with liquid phase detection content of 98.1%.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.90Kg of burdock oil.

Pulverizing supercritical extraction residue to 60-80 mesh, extracting with 6 times of n-butanol at normal temperature under stirring for 2 times (1.5 hr each time), concentrating the extractive solution to alcohol degree of 10%, adding 20% of mixed adsorbent (activated carbon: neutral alumina 1:2) of extraction residue, stirring for 2 hr, filtering, collecting mixed adsorbent, dissolving with 5 times of water saturated ethyl acetate under stirring for 2 times (2 hr each time), filtering, mixing filtrates, concentrating to specific gravity 1.129, refrigerating for crystallization, filtering, rinsing with dichloromethane, and drying to obtain arctiin 2.82Kg, with liquid phase content of 98.2%.

EXAMPLE III

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and the enzyme is steamed and inactivated for 8 min. Xylene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 32MPa, the extraction temperature is 43 ℃, the extraction time is 3 hours, the carbon dioxide flow is 12Kg/h, and the carrying agent dosage is 4 percent of the raw material mass.

The supercritical extract is prepared by stirring No. six solvent oil with the mass of 4 times of the supercritical extract for 30min, filtering, and respectively collecting No. six solvent oil layer and insoluble substances.

Adding 4 times of mixed solvent (No. six solvent oil: 80% ethanol: 1:2) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to 60% of alcohol degree, adding active carbon with the extract quality of 5% for decoloring for 2h, filtering, continuously concentrating the filtrate to the specific gravity of 1.127, refrigerating for crystallization, filtering, stirring the crystals by using isopropanol with the wet weight of 1.3 times of the crystals, filtering, crystallizing and drying to obtain 344g of arctigenin, wherein the content of the arctigenin detected by a liquid phase is 98.5%.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.82Kg of burdock oil.

Pulverizing supercritical extraction residue to 60-80 mesh, extracting with 7 times of n-butanol at normal temperature under stirring for 2 times (1.5 hr each time), concentrating the extractive solution to alcohol degree of 8%, adding 22% of mixed adsorbent (activated carbon: neutral alumina 1:4) of extraction residue, stirring for 2 hr, filtering, collecting mixed adsorbent, dissolving with 8 times of water saturated ethyl acetate under stirring for 2 times (2 hr each time), filtering, mixing filtrates, concentrating to specific gravity of 1.148, refrigerating for crystallization, filtering, rinsing with dichloromethane, and drying to obtain arctiin 2.85Kg, with liquid phase content of 98.3%.

Example four

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and enzyme is cooked and inactivated for 6 min. Toluene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 34MPa, the extraction temperature is 42 ℃, the extraction time is 2.5h, the carbon dioxide flow is 11Kg/h, and the carrying agent dosage is 3.5 percent of the raw material mass.

The supercritical extract is prepared by stirring 3 times of number six solvent oil for 30min, filtering, and collecting number six solvent oil layer and insoluble substance respectively.

Adding 4 times of mixed solvent (No. six solvent oil: 80% ethanol: 2:3) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to alcohol degree of 68%, adding active carbon with extract quality of 5% for decolorizing for 2h, filtering, concentrating the filtrate to specific gravity of 1.142, refrigerating for crystallization, filtering, stirring the crystallization with isopropanol with wet weight of 1.2 times, filtering, crystallizing, and drying to obtain 338g arctigenin, with liquid phase detection content of 98.2%.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.77Kg of burdock oil.

Pulverizing supercritical extraction residue to 60-80 mesh, extracting with 8 times of n-butanol at normal temperature under stirring for 2 times (1.5 hr each time), concentrating the extractive solution to alcohol degree of 6%, adding 21% of mixed adsorbent (activated carbon: neutral alumina 2:7) of extraction residue, stirring for 2 hr, filtering, collecting mixed adsorbent, dissolving with 9 times of water saturated ethyl acetate under stirring for 2 hr each time, filtering, mixing filtrates, concentrating to specific gravity of 1.113, refrigerating for crystallization, filtering, rinsing with dichloromethane, and drying to obtain arctiin 2.81Kg, with liquid phase content of 98.1%.

EXAMPLE five

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and enzyme is cooked and inactivated for 9 min. The liquid phase spectrum of the burdock fruit raw material adopted in the embodiment is shown in figure 1. Toluene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 34MPa, the extraction temperature is 42 ℃, the extraction time is 2.5h, the carbon dioxide flow is 11Kg/h, and the carrying agent dosage is 4 percent of the raw material mass. The liquid phase map of the supercritical extraction residue of the burdock raw material is shown in figure 2, and compared with figure 1, the burdock raw material can be seen that the burdock takes toluene as a carrying agent, after supercritical extraction, the good separation of the arctiin from the burdock oil and the arctigenin can be realized, the content of the arctiin is increased from 5.3 percent to 7.2 percent, and the content is increased by 35 percent.

The supercritical extract is prepared by stirring 3 times of number six solvent oil for 30min, filtering, and collecting number six solvent oil layer and insoluble substance respectively.

Adding 4 times of mixed solvent (No. six solvent oil: 80% ethanol: 1:2) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to alcohol degree of 68%, adding active carbon with extract quality of 5% for decolorizing for 2h, filtering, concentrating the filtrate to specific gravity of 1.142, refrigerating for crystallization, filtering, stirring with isopropanol with wet weight of 1.2 times, filtering, crystallizing, and drying to obtain 356g arctigenin, with liquid phase content of 98.9%, and liquid phase chromatogram as shown in FIG. 6.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.70Kg of burdock oil.

Pulverizing the supercritical extraction residue to 60-80 mesh, extracting with n-butanol with mass of 8 times at normal temperature for 1.5 hr for 2 times. The liquid phase spectrum of the n-butanol extract is shown in fig. 3, and it can be seen that some large-polarity impurities can be removed by extracting the extraction residue with n-butanol, thereby realizing the purification of arctiin. Then, the extracting solution is concentrated to the alcohol degree of 8%, a mixed adsorbent (activated carbon: neutral alumina: 1:3) with the mass of 25% of the extraction residue is added, the mixture is stirred for 2 hours, filtered and collected, and a liquid phase map of the mixed adsorbent is shown in figure 4. After the feed liquid is adsorbed, the separation of the arctiin and impurities can be well realized, the process is simple, and the operability is strong. Then the mixed adsorbent is eluted by ethyl acetate with medium polarity, so that the removal of impurities with large polarity can be further realized. Then, water saturated ethyl acetate with the amount of 8 times of the extraction residue is adopted to stir and dissolve for 2 times, each time lasts for 2 hours, the filtration is carried out, the filtrates are combined and concentrated to the specific gravity of 1.126, the cold storage crystallization, the filtration and the rinsing with dichloromethane are carried out, and then the drying is carried out, thus obtaining 2.96Kg of arctiin, the liquid phase detection content is 98.8%, and the liquid phase atlas is shown in figure 5.

EXAMPLE six

Firstly, 50Kg of burdock raw material is pressed into a compact by a briquetting machine, and the enzyme is steamed and killed for 7 min. The xylene is used as a carrying agent, supercritical carbon dioxide extraction is adopted, the extraction pressure is 33MPa, the extraction temperature is 45 ℃, the extraction time is 3.5h, the carbon dioxide flow is 10Kg/h, and the carrying agent dosage is 4.5 percent of the raw material mass.

The supercritical extract is prepared by stirring No. six solvent oil with the mass of 4 times of the supercritical extract for 30min, filtering, and respectively collecting No. six solvent oil layer and insoluble substances.

Adding 3 times of mixed solvent (No. six solvent oil: 80% ethanol: 2:5) into the insoluble substance, stirring for 30min, and collecting ethanol layer and No. six solvent oil layer.

Concentrating the ethanol layer to reach an alcohol degree of 63%, adding active carbon with the mass of 5% of the extract for decolorization for 2h, filtering, continuously concentrating the filtrate to reach a specific gravity of 1.122, refrigerating for crystallization, filtering, stirring the crystals by using isopropanol with the wet weight of 1.3 times of the crystals, filtering, crystallizing and drying to obtain 343g of arctigenin, wherein the content of the arctigenin is 98.4% by liquid phase detection.

Mixing the six solvent oil layers, decolorizing with 10% active carbon for 1 hr, filtering, and concentrating to obtain 6.68Kg of burdock oil.

Pulverizing supercritical extraction residue to 60-80 mesh, extracting with 6 times of n-butanol at normal temperature under stirring for 2 times (1.5 hr each time), concentrating the extractive solution to 7% alcohol degree, adding 28% mixed adsorbent (activated carbon: neutral alumina 1:3) of extraction residue, stirring for 2 hr, filtering, collecting mixed adsorbent, dissolving with 9 times of water saturated ethyl acetate under stirring for 2 times (2 hr each time), filtering, mixing filtrates, concentrating to specific gravity 1.144, refrigerating for crystallization, filtering, rinsing with dichloromethane, and drying to obtain arctiin 2.84Kg, with liquid phase content of 98.3%.

The invention adopts a plurality of technologies of enzyme deactivation, supercritical extraction, mixed solvent extraction, adsorption, analysis and the like to be jointly used, shortens the production period to 48 hours through 7 steps of reaction, develops the active ingredients in the burdock raw material to the maximum extent, realizes the maximization of resource utilization, reduces energy consumption, greatly reduces the production cost of a single product, greatly improves the production efficiency, and is suitable for industrial production.