Method for extracting aleppo avens positive extract from aleppo avens middle and middle at low temperature

Abstract

The method comprises the following steps: adding aleppo avens and a solvent into an extraction device, carrying out countercurrent ultrasonic extraction, feeding an extracting solution into a conical stainless steel precipitation tank through a stainless steel delivery pump, cooling, standing and precipitating in the precipitation tank, taking a supernatant, filtering, washing, and drying to obtain the aleppo avens extract. And feeding the concentrated solution into an ultralow-temperature rotary film evaporator for evaporation and concentration to obtain a concentrated solution and an alcohol-water recovery solution, carrying out vacuum freeze drying on the concentrated solution, and then feeding the concentrated solution into a high-energy vibration type ultrafine grinder for low-temperature grinding to obtain the aleppo avens positive extract. The extraction method disclosed by the invention is simple in steps and easy to automatically control, the whole extraction process realizes full recycling of a solvent, no extraction waste liquid or waste gas is generated, and the whole-process green intelligent production of the extraction process is realized; the method has the advantages that the effective components of the aleppo avens extracted by the method are stable, the extraction rate of the aleppo avens extract is high, the transfer rate of the effective components is high, and the powder yield of the extract is high.

Description

Technical Field

[0001] The invention belongs to the research field of green technology for plant extraction, and in particular relates to a technology for preparing a blue bud extract from blue bud by low-temperature extraction. Background Art

[0002] Blue Buzheng (Guizhou), also known as Zhuifengqi (Shaanxi), is the dried whole herb of Geum aleppicum Jacq. or Geumjaponicum Thunb.var.chinenseBolle, a plant of the Rosaceae family. It is widely distributed in temperate regions of China and is a traditional folk medicine in my country. There are about 70 species of this genus in the world, of which only four species in my country are Geum aleppicum, Geum rivale, Geum japonicum and Geum japonicum Thunb.var.chinenseF.Bolle. Blue Buzheng grows on hillside grasslands, ditch edges, bottom edges, river beaches, forest gaps and forest edges. It has the effects of invigorating qi and strengthening the spleen, nourishing blood and yin, moistening the lungs and resolving phlegm, and is used to treat headaches, dizziness, weakness, and irregular menstruation. The chemical components found in the extract of Lanbuzheng mainly include terpenes (mainly monoterpenes, sesquiterpenes and triterpenes), tannins, phenylpropanoids, etc. Modern pharmacological and pharmacodynamic studies have shown that Lanbuzheng has multiple pharmacological effects such as anticoagulation, antihypertension, anti-inflammatory, anti-tumor and treatment of ischemic diseases.

[0003] At present, only the traditional water extraction method and the alcohol-water extraction method have been reported for the extraction process of blue bud extract. The extraction rate of effective ingredients in the traditional extraction process is low. If high alcohol concentration is used for extraction, the content of liver toxic substances will increase, affecting the efficacy of the drug. At the same time, the existing extraction process does not realize the recycling of extraction solvents, and cannot achieve green production. Based on this, it is of practical significance and development prospects to develop an environmentally friendly, low-temperature extraction process for blue bud extract from blue bud, and to recycle the extraction solvent. Summary of the invention

[0004] The present invention provides an environmentally friendly process for low-temperature extraction of blue cloth extract from blue cloth in order to solve the above-mentioned technical problems. The whole extraction process of the present invention realizes the full recycling of solvent, does not produce any extraction waste liquid and waste gas, is green and environmentally friendly, realizes the full-process green and intelligent production of the extraction process, and the blue cloth extract extracted by the method, the low temperature condition ensures that its effective ingredients are stable, the extraction process of the method is stable during production, the extraction rate of the blue cloth extract is high, the transfer rate of the effective ingredients (gallic acid and ellagic acid) in blue cloth is high, and the extract powder yield is high.

[0005] In order to achieve the above-mentioned purpose, the present invention adopts the following technical solutions:

[0006] A method for low-temperature extraction of a blue sedge extract from blue sedge, comprising the following steps:

[0007] The indigofera hay and solvent are added into an extraction tank for countercurrent ultrasonic extraction, and the extract is sent into a conical stainless steel precipitation tank through a stainless steel delivery pump. The precipitation tank is cooled and allowed to stand for precipitation, and the supernatant is sent into an ultra-low temperature rotary thin film evaporator for evaporation and concentration to obtain a concentrated solution and an alcohol-water recovery solution. The concentrated solution is vacuum freeze-dried and then sent into a high-energy vibration ultrafine pulverizer for low-temperature pulverization to obtain the indigofera extract.

[0008] Further, the process of extracting the blue cloth extract from the blue cloth at low temperature in the whole process specifically comprises the following steps:

[0009] (1) Low-temperature countercurrent ultrasonic extraction: first, the blue cloth hay is placed in a medicine washing machine for cleaning to remove the dirt and debris remaining on the stems, then placed in a dehydrator for dehydration and drainage, and then sent to a CNC medicine cutting machine for cutting into sections with a length of 1 to 2 cm. Then, it is placed in a vacuum extraction tank of a traditional Chinese medicine countercurrent ultrasonic extraction and concentration unit, and the solvent required for extraction is added to perform countercurrent ultrasonic extraction to obtain an extract;

[0010] (2) Cooling and settling: The concentrated solution obtained in step (1) is pumped into a settling tank via a stainless steel delivery pump. After being sealed and settling in the settling tank, the precipitate in the settling tank is removed to obtain an extraction supernatant.

[0011] (3) Ultra-low temperature rotary thin film evaporation: the supernatant obtained in step (2) is sent to an ultra-low temperature rotary thin film evaporator for ultra-low temperature rotary thin film evaporation to obtain a concentrated solution, and the obtained alcohol-water recovery solution is used for the next batch of extraction;

[0012] (4) Drying and pulverizing: The concentrated solution obtained in step (3) is subjected to vacuum freeze drying, and then sent to an ultrafine pulverizer for pulverization. The concentrated solution is packaged in composite film bags using a composite film packaging machine. After passing the inspection, the concentrated solution is packed into large boxes and sent to an intermediate warehouse to obtain the blue cloth extract.

[0013] Furthermore, in step (1), the ultrasonic power of the countercurrent ultrasonic extraction is 200W to 350W, the temperature is 25°C to 60°C, and the time is 15min to 150min; the solvent is an ethanol solution with a mass concentration of 10% to 70%, and the mass ratio of the solvent to the blue cloth positive film is 6 to 10:1. The mass concentration of the ethanol aqueous solution is preferably 10% to 40%, and more preferably 10%, 20%, 30%, and 40%.

[0014] Furthermore, the solvent in step (1) is the alcohol-water recovery liquid obtained in step (3); the mass concentration of the alcohol-water recovery liquid is 10% to 70%, which is the same as the mass concentration of the solvent added in step 1.

[0015] Furthermore, in step (2), the precipitation time is 12 hours to 36 hours, and the temperature in the precipitation tank is controlled at 0°C to 35°C.

[0016] Furthermore, in step (3), the concentration temperature is 5°C to 35°C, the pressure is 50Pa to 800Pa, and the time is 10min to 60min.

[0017] Furthermore, in step (4), the drying is vacuum freeze drying, the drying temperature is -50°C to 25°C, the vacuum degree is 20Pa-200Pa, and the time is 60min to 300min.

[0018] The high-energy vibration type ultrafine grinding has a grinding temperature of -5°C to 25°C and a grinding time of 10 minutes to 100 minutes.

[0019] Furthermore, the blue cloth extract obtained by the present invention includes the following components and contents: gallic acid content is 0.41%-0.44%, tannin content is 11.3%-11.6%, and total flavonoids content is 13.1%-14.8%.

[0020] The beneficial effects of the present invention are: (1) the entire extraction process realizes full recovery and utilization of the solvent without generating any extraction waste liquid or waste gas; (2) the extraction method has simple steps and is easy to automate, thus realizing green and intelligent production of the entire extraction process with high extraction rate of effective ingredients, high transfer rate, and high extract yield; (3) the use of low-temperature extraction ensures that the effective ingredients of Lanbuzheng are stable and of good quality. DETAILED DESCRIPTION

[0021] The specific embodiments of the present invention are further described in detail below, but the present invention is not limited to these embodiments, and any improvement or substitution based on the basic spirit of the present embodiment still falls within the scope of protection required by the claims of the present invention.

[0022] Embodiment 1-5:

[0023] In this embodiment, 1-3 is implemented by adopting the technical solution of the present invention, including the following steps:

[0024] (1) Low-temperature countercurrent ultrasonic extraction: The blue cloth hay is put into a medicine washing machine for cleaning to remove the dirt and debris remaining on the stems, and then put into a dehydrator for dehydration and drainage, and then sent to a CNC medicine cutting machine for cutting into segments with a length of about 1 cm. Then, it is placed in a vacuum extraction tank of a traditional Chinese medicine countercurrent ultrasonic extraction and concentration unit, and a solvent is added to perform countercurrent ultrasonic extraction. The specific parameters are shown in Table 1 to obtain an extract;

[0025] (2) Cooling and settling: The concentrated solution obtained in step (1) is sent into a settling tank by a stainless steel delivery pump, sealed in the settling tank and settling, and then the precipitate in the settling tank is removed. The specific parameters are shown in Table 1, and the extraction supernatant is obtained;

[0026] (3) Ultra-low temperature rotary thin film evaporator evaporation and concentration: The extraction supernatant obtained in step (2) is sent to an ultra-low temperature rotary thin film evaporator for ultra-low temperature rotary thin film evaporation. The specific parameters are shown in Table 1 to obtain a concentrated solution, and the obtained alcohol-water recovery solution is all used for the next batch of extraction; in this step, the overall solvent recovery rate is 96%, and the remaining 4% of the solvent is recovered in the freeze-drying step.

[0027] (4) Drying and pulverizing: The concentrated solution obtained in step (3) is subjected to vacuum freeze-drying. The specific parameters are shown in Table 1. The product obtained after freeze-drying is sent to a low-temperature ultrafine pulverizer for pulverization. The specific parameters are shown in Table 1. The obtained powder is packaged in a composite film bag by a composite film packaging machine. After passing the inspection, it is packed into large boxes and sent to the intermediate warehouse to obtain the blue cloth extract.

[0028] In Examples 4-5, Example 4 used a water decoction method, and Example 5 used a solvent extraction method. The two examples were compared with Examples 1-3 using different process parameters and the results obtained.

[0029] Table 1 Process parameters of the preparation example of blue bud extract

[0030]

[0031]

[0032] The above-mentioned blue cloth extract was evaluated, and the specific results are shown in Table 2:

[0033] Table 2 Evaluation results of indigo extract

[0034]

[0035]

[0036] It can be seen from the above Examples 1-3 that an ethanol aqueous solution with a mass concentration of 30% is used as the extraction solvent in the examples, wherein the mass ratio of the solvent to the blue cloth is 6-10:1, and the working temperature after freeze drying is -5°C-25°C. Under other conditions, the mass ratio of the solvent to the blue cloth in Example 1 is 6:1, the extraction rate (by powder weight) is 15.8%, the effective component transfer rate is 92.1%, and the extract yield (component yield) is 99.8%. In the extract component content of Example 1, the gallic acid content is 0.41%, the tannin content is 11.3%, and the total flavonoid content is 13.1%.

[0037] In Example 2, the mass ratio of solvent to blue cloth is 8:1, the extraction rate (based on the weight of powder) is 17.1%, the effective component transfer rate is 94.4%, and the extract yield (component yield) is 99.5%. In the extract component content of Example 1, the gallic acid content is 0.43%, the tannin content is 11.5%, and the total flavonoid content is 13.8%.

[0038] In Example 3, the mass ratio of solvent to blue cloth is 10:1, the extraction rate (based on the weight of powder) is 17.9%, the effective component transfer rate is 95.6%, and the extract yield (component yield) is 99.5%. In the extract component content of Example 1, the gallic acid content is 0.44%, the tannin content is 11.6%, and the total flavonoid content is 14.8%.

[0039] Examples 4-5 respectively use water decoction and solvent extraction to compare the extraction effect of the blue cloth extract with the present invention. The extraction step does not include an ultrasonic extraction process, the concentration step adopts a single-effect condensation concentration method, and the drying step does not use freeze drying, but a spray drying method. Among them, in the water decoction method of Example 4, pure water is used as a solvent, the mass ratio of the solvent to the blue cloth is 10:1, the high temperature extraction is 90°C, and the temperature is 70°C. The results are: the extraction rate (by powder weight) is 10.5%, the effective ingredient transfer rate is 72.5%, and the extract yield (component yield) is 97.7%. In the extract component content of Example 1, the gallic acid content is 0.31%, the tannin content is 4.6%, and the total flavonoid content is 7.7%.

[0040] In the solvent extraction method of Example 5, an ethanol aqueous solution with a mass concentration of 40% was used as the extraction solvent, the mass ratio of the solvent to the blue cloth was 10:1, the extraction was carried out at a high temperature of 80°C, and the concentration was carried out at a temperature of 70°C. The results were as follows: the extraction rate (by weight of the powder) was 12.1%, the effective component transfer rate was 84.9%, and the extract yield (component yield) was 98.1%. In the extract component content of Example 1, the gallic acid content was 0.38%, the tannin content was 8.9%, and the total flavonoid content was 13.2%.

[0041] It should be further explained that in the above embodiments, after the evaporation and concentration step using the ultra-low temperature rotary thin film evaporator of embodiments 1-3 of the method of the present invention, the solvent recovery rate reached 96%, and in the freeze-drying step, the remaining 4% of the solvent was recovered, so that the solvent recovery rate reached 100%, and the full-process green and intelligent production of the extraction process was realized. In the two extraction processes of embodiments 4 and 5, the solvent recovery rate was only 90%.

[0042] It can be seen from the above table that the extracts prepared under various parameters of the present invention have stable physical and chemical properties and uniform quality.

[0043] Embodiment 6-8:

[0044] This embodiment 6-8 includes the following steps:

[0045] (1) Low-temperature countercurrent ultrasonic extraction: The blue cloth hay is put into a medicine washing machine for cleaning to remove the dirt and debris remaining on the stems, and then put into a dehydrator for dehydration and drainage, and then sent to a CNC medicine cutting machine for cutting into sections with a length of about 2 cm. Then, it is placed in a vacuum extraction tank of a traditional Chinese medicine countercurrent ultrasonic extraction and concentration unit, and a solvent is added to perform countercurrent ultrasonic extraction to obtain an extract;

[0046] (2) Cooling and settling: The concentrated solution obtained in step (1) is pumped into a settling tank via a stainless steel delivery pump. After being sealed and settling in the settling tank, the precipitate in the settling tank is removed to obtain an extraction supernatant.

[0047] (3) Evaporation and concentration using an ultra-low temperature rotary thin film evaporator: sending the extracted supernatant obtained in step (2) into an ultra-low temperature rotary thin film evaporator for ultra-low temperature rotary thin film evaporation to obtain a concentrated solution;

[0048] (4) Drying and pulverizing: The concentrated solution obtained in step (3) is subjected to vacuum freeze-drying, and the product obtained after freeze-drying is sent to a low-temperature ultrafine pulverizer for pulverization. The obtained powder is packaged in a composite film bag using a composite film packaging machine to obtain the indigo extract.

[0049] The solvent in step (1) is the alcohol-water recovery liquid obtained in step (3). The alcohol-water recovery liquid obtained in step (3) of the present invention can be fully used for the next batch of extraction, thus realizing the recycling of the solvent.

[0050] The effect of the solvent reuse recovered by the technical solution of the present invention is evaluated by Examples 6-8. In Examples 6-8, the alcohol-water recovery solution obtained in Examples 1-3 is used to re-extract the blue cloth extract; the specific implementation parameters in each example are carried out under the conditions of Example 3 of No. 3 in Table 1. Three blue cloth extracts were evaluated, and the specific results are shown in Table 3:

[0051] Table 3 Evaluation results of indigo extract

[0052] Serial number Example 6 Example 7 Example 8 Extraction rate (calculated by powder weight) 17.8％ 17.8％ 17.9％ Active ingredient transfer rate 95.4％ 95.5％ 95.4％ Extract yield (powder yield) 99.5％ 99.5％ 99.5％ Gallic acid content 0.44％ 0.44％ 0.44％ Tannin content 11.5％ 11.8％ 11.6％ Total flavonoids content 14.6％ 14.5％ 14.9％

[0053] In each embodiment, the extraction rate (based on the weight of the powder) is as low as 17.8%, the effective component transfer rate is as low as 95.4%, and the extract yield (component yield) is 99.5%. Among the extract components, the gallic acid content is 0.43%, the tannin content is as low as 11.5%, and the total flavonoid content is as low as 14.5%.

[0054] According to the results in the above table, the product quality is still qualified when the recycled alcohol aqueous solution is used for extraction, and has the same technical effect as Examples 1 to 3 of the present invention. This method achieves green environmental protection on the basis of ensuring qualified product quality.

[0055] Embodiment 9-12:

[0056] Examples 9-12 used the traditional extraction solvents: water, ethanol, methanol and the ethanol-water solution of the present method to extract blue cloth, and evaluated the blue cloth extracts with different extraction solvents. Each example used the parameters of Example 1 with sequence number 1 in Table 1 as the implementation parameters. The specific results are shown in Table 4:

[0057] Table 4 Evaluation results of indigo extract

[0058]

[0059] In each embodiment, the extraction rate (based on the weight of the powder) is up to 12.9% with methanol, the effective component transfer rate is up to 90.8%, and the extract yield (component yield) is up to 92.8%. Among the extract components, the gallic acid content is up to 0.40%, the tannin content is up to 10.5%, and the total flavonoid content is up to 14.6%.

[0060] According to the results in the table above, the above Examples 9-12 use the traditional extraction solvents: water, ethanol, methanol and the ethanol-water solution of the present method to extract blue cloth, and the product's extraction rate (calculated by powder weight), effective component transfer rate, extract yield (powder yield) and other indicators, as well as the gallic acid content, tannin content, and total flavonoid content in the product are all lower than the results obtained by the technical solution of the present invention. This shows that the method of the present invention has a high extraction rate, a high effective component transfer rate, and a high extract yield; it has achieved an ideal technical effect.

[0061] Based on the above embodiments, the present invention adds blue cloth and solvent into the extraction device for countercurrent ultrasonic extraction, and after the extract is cooled and allowed to stand for precipitation, the supernatant is sent to an ultra-low temperature rotary film evaporator for evaporation and concentration to obtain a concentrated solution and an alcohol-water recovery solution, and the concentrated solution is sent to a high-energy vibration ultrafine grinder for low-temperature pulverization after vacuum freeze drying to obtain the blue cloth extract. The present invention uses a low-temperature extraction process to extract the blue cloth extract, and the entire extraction process realizes the full recycling of the solvent, does not generate extraction waste liquid and waste gas, realizes the full-process green intelligent production of the extraction process, and the low-temperature process ensures the activity of the effective ingredients in the blue cloth extract. In addition, unlike conventional techniques, the present invention uses 10% to 70% ethanol aqueous solution as a solvent, and the lower concentration of ethanol aqueous solution has a good protective effect on the effective ingredients of the extract. According to the experimental verification of the present invention, when the concentration of the solvent ethanol aqueous solution is higher than 70%, the content of the effective ingredient in the extract is significantly reduced, and the optimal solvent concentration is 10-40%. The present invention uses 30% and 40% solvent concentrations as examples to illustrate the technical solution of the present invention, but the use of solvent concentrations within this range, although slightly different, also has the same technical effect. The method of the present invention adopts a method combining low temperature and low solvent concentration, and has the advantages of stable extraction of effective components of blue cloth, high extraction rate of blue cloth extract, high effective component transfer rate, and high extract powder yield.

[0062] It should be further explained that the above implementation modes are only used for understanding the technical solutions of the present invention, and are not used to limit the protection scope of the present invention. Any obvious adjustments and modifications made to the technical solutions of the present invention within the technical concept of the present invention should also fall within the protection scope of the present invention.

Claims

1. A method for low-temperature extraction of indigo extract from indigo, characterized in that: The following steps are involved: (1) Low-temperature countercurrent ultrasonic extraction: first, put the blue cloth into a medicine washing machine for cleaning, remove the dirt and debris remaining on the stem, put it into a dehydrator for dehydration and draining, and then send it to a CNC medicine cutting machine for cutting into sections with a length of 1 to 2 cm. Then, put it into the vacuum extraction device of the Chinese medicine countercurrent ultrasonic extraction and concentration unit, add a solvent, and perform countercurrent ultrasonic extraction to obtain an extract; (2) Cooling and settling: The concentrated solution obtained in step (1) is pumped into a settling tank via a stainless steel delivery pump. After being sealed and cooled in the settling tank and settling, the precipitate in the settling tank is removed to obtain an extraction supernatant. (3) Ultra-low temperature rotary thin film evaporation concentration: the extraction supernatant obtained in step (2) is sent to an ultra-low temperature rotary thin film evaporator for ultra-low temperature rotary thin film evaporation concentration to obtain a concentrated solution, and the obtained alcohol-water recovery solution is used for the next batch of extraction; (4) Drying and pulverizing: The concentrated solution obtained in step (3) is subjected to vacuum freeze-drying and then fed into an ultrafine pulverizer for pulverization to obtain the blue cloth extract.

2. The method for low-temperature extraction of indigo extract from indigo according to claim 1, characterized in that: In step (1), the ultrasonic extraction has an ultrasonic power of 300W to 350W, a temperature of 25°C to 60°C, and a time of 15min to 60min; the solvent is an ethanol aqueous solution with a mass concentration of 10% to 70%, and the mass ratio of the solvent to the blue cloth positive film is 6 to 10:

1.

3. The method for low-temperature extraction of indigo extract from indigo according to claim 1, characterized in that: The solvent in step (1) is the alcohol-water recovery liquid obtained in step (3); the mass concentration of the alcohol-water recovery liquid is 10% to 70%.

4. The method for low-temperature extraction of indigo extract from indigo according to claim 1, characterized in that: In step (2), the precipitation time is 12 hours to 36 hours, and the temperature in the precipitation tank is controlled at 0°C to 35°C.

5. The method for low-temperature extraction of indigo extract from indigo according to claim 1, characterized in that: In step (3), the concentration temperature is 5°C to 35°C, the pressure is 50Pa to 800Pa, and the time is 10min to 60min.

6. The method for low-temperature extraction of indigo extract from indigo according to claim 1, characterized in that: In step (4), the drying is vacuum freeze drying, the drying temperature is -50°C to 25°C, the vacuum degree is 20Pa-200 Pa, and the time is 60min to 300min; the pulverization is high-energy vibration ultrafine pulverization, the pulverization temperature is -5°C to 25°C, and the time is 10min to 100min.

7. The method for low-temperature extraction of indigo extract from indigo according to any one of claims 1 to 6, characterized in that: The obtained blue cloth extract includes the following components and contents: gallic acid content is 0.41%-0.44%, tannin content is 11.3%-11.6%, and total flavonoids content is 13.1%-14.8%.

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