Method for extracting and separating effective components of traditional Chinese medicine polygonum multiflorum

Abstract

The invention discloses a method for extracting and separating effective components of traditional Chinese medicine polygonum multiflorum, which comprises the following steps of: firstly, crushing the polygonum multiflorum into powder by using a crusher, and sufficiently drying the polygonum multiflorum powder; adding the dried polygonum multiflorum powder into a solution formed by mixing benzene and sulfuric acid, thoroughly stirring, and standing for a period of time for later use; filtering the polygonum multiflorum solution after standing so as to obtain polygonum multiflorum mother liquor and polygonum multiflorum filter residues; the method comprises the following steps: adding a mixed solution of benzene and benzene-ethyl acetate into polygonum multiflorum filter residues, and stirring at the same time; according to the method for extracting and separating the effective components of the traditional Chinese medicine polygonum multiflorum, the requirement on equipment required for extracting the effective components in the polygonum multiflorum is reduced by adopting a multi-time extraction mode, so that the cost required for extracting the effective components in the polygonum multiflorum is reduced, and the technical requirement required for extraction is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of drug extraction, and in particular to a method for extracting and separating effective components of Polygonum multiflorum Thunb., a traditional Chinese medicine. Background Art

[0002] Polygonum multiflorum Thunb. is a traditional Chinese medicine, which has the effects of detoxification, malaria interception, and laxative. Clinically, it can be mainly used to treat diseases such as malaria, intestinal dryness and constipation, and eczema. After steaming Polygonum multiflorum Thunb. with black beans, it will become red Polygonum multiflorum Thunb., and it can also play the effects of tonifying the liver and kidney, strengthening the muscles and bones, blackening the hair, and nourishing essence and blood. The extract of Polygonum multiflorum Thunb. is the dried tuberous root of the plant Polygonum multiflorum Thunb. of the Polygonaceae family. The main functional components are lecithin, emodin, rhein, and other components. The main effects include anti-aging, effects on the immune system, reducing blood lipid and anti-atherosclerosis, myocardial protection, liver protection, nerve protection, and antibacterial.

[0003] Modern medical research has also found that the extract of Polygonum multiflorum Thunb. contains substances that can inhibit the increase of oxidized lipids and transaminases in the liver, can fundamentally reduce the content of fatty acids, and has a certain repair effect on liver function damage caused by fatty liver, hepatitis B, etc. Polygonum multiflorum Thunb. can indirectly improve the phagocytosis ability of macrophages, activate T lymphocytes, and increase the lymphocyte transformation rate, thereby enhancing the body's immunity. Therefore, the extract of Polygonum multiflorum Thunb. has significant effects in many aspects. The traditional methods of traditional Chinese medicine extraction include maceration method, percolation method, decoction method, and heat reflux extraction method. However, these methods generally have the disadvantages of low extraction rate of effective components, low impurity clearance rate, high energy consumption, and long production cycle, which directly affect the development of the traditional Chinese medicine pharmaceutical industry. Summary of the Invention

[0004] The technical problem to be solved by the present invention is: aiming at the deficiencies of the prior art, the present invention provides a method for extracting and separating effective components of Polygonum multiflorum Thunb., a traditional Chinese medicine, and solves the common disadvantages of the traditional methods of traditional Chinese medicine extraction in the above background art, such as low extraction rate of effective components, low impurity clearance rate, high energy consumption, and long production cycle.

[0005] The technical solution adopted by the present invention to solve its technical problems is: a method for extracting and separating effective components of Polygonum multiflorum Thunb., a traditional Chinese medicine, includes the following steps:

[0006] First step, use a crusher to break Polygonum multiflorum Thunb. into powder, and fully dry the Polygonum multiflorum Thunb. powder;

[0007] Second step, add the dried Polygonum multiflorum Thunb. powder into a solution formed by mixing benzene and sulfuric acid, and let it stand for a period of time after thorough stirring for standby;

[0008] Third step, filter the standing Polygonum multiflorum Thunb. solution to obtain the mother liquor of Polygonum multiflorum Thunb. and the filter residue of Polygonum multiflorum Thunb.;

[0009] Step 4: Add benzene and a mixed solution of benzene and ethyl acetate to the Polygonum multiflorum Thunb. filter residue, stir the mixture, and after standing for a period of time, perform recrystallization on this solution to obtain emodin crystals;

[0010] Step 5: Add sodium hydroxide solution to the solution remaining after Step 4 and stir it thoroughly. After standing for a period of time, the staff adjust its pH value to 2 - 3, then extract it with chloroform and concentrate it. After standing for a period of time, emodin-6-methyl ether crystals are obtained;

[0011] Step 6: Prepare a sodium bicarbonate solution and extract the Polygonum multiflorum Thunb. mother liquor obtained in Step 3 to obtain Solution A;

[0012] Step 7: Adjust the pH value of Solution A to 2 - 3, then add chloroform for extraction and concentration. After standing for a period of time, emodin crystals are obtained.

[0013] Optionally, in Step 1, when drying the Polygonum multiflorum Thunb. powder, the temperature is maintained at 40 °C for 5 days, and after drying is completed, it needs to be taken out of the drying equipment for 24 hours and then dried again.

[0014] Optionally, in Step 2, the volumes of benzene and sulfuric acid solution are 5 times that of the Polygonum multiflorum Thunb. powder, and the mixing ratio of benzene and sulfuric acid is 5:1.

[0015] Optionally, in Step 2, the stirring time is half an hour, and the rotation speed during stirring is 1000 revolutions per minute.

[0016] Optionally, in Step 3, the Polygonum multiflorum Thunb. solution needs to be filtered three times.

[0017] Optionally, in Step 4, the mixing ratio of benzene and the benzene - ethyl acetate mixture is 4:1.

[0018] Optionally, in Step 6, the mass fraction of sodium bicarbonate is 2.5%.

[0019] Optionally, in Step 6, during extraction, it needs to be stirred for two hours, and after thorough mixing and stratification, separation is carried out.

[0020] Optionally, in Steps 5 and 7, the regulators used to adjust the pH value are sulfuric acid or sodium hydroxide.

[0021] Optionally, the standing time is at least 12 hours to ensure that the corresponding change process can proceed fully.

[0022] The extraction and separation method of the active ingredients of the traditional Chinese medicine Polygonum multiflorum Thunb. of the present invention has the beneficial effects that:

[0023] The method for extracting and separating the active ingredients of the traditional Chinese medicine Polygonum multiflorum reduces the equipment requirements for extracting the active ingredients of Polygonum multiflorum by adopting the method of multiple extractions, thereby reducing the cost required for extracting the active ingredients of Polygonum multiflorum, reducing the technical requirements for extraction, making this method easier to promote. Moreover, during the extraction process, both the leaching solution and the leaching residue are comprehensively treated, thereby maximizing the extraction rate of the active ingredients in Polygonum multiflorum, reducing the waste caused by extraction equipment and technological processes, increasing the utilization rate of Polygonum multiflorum raw materials, and indirectly reducing costs. Brief Description of the Drawings

[0024] The present invention will be further described below in conjunction with the drawings and embodiments.

[0025] Figure 1 It is a schematic diagram of the extraction and separation process of the present invention. Detailed Embodiments

[0026] The present invention will now be further described in detail in conjunction with the embodiments.

[0027] Refer to Figure 1 , the present invention provides a technical solution: a method for extracting and separating the active ingredients of the traditional Chinese medicine Polygonum multiflorum.

[0028] First step: First, pulverize Polygonum multiflorum into powder by a pulverizer, and fully dry the Polygonum multiflorum powder. The temperature is maintained at 40 degrees during drying, and the duration is five days. And after drying is completed, it needs to be taken out of the drying equipment for 24 hours, and then dried again;

[0029] The heat pump dryer for Polygonum multiflorum can select an air source heat pump drying equipment, which uses a low-temperature refrigerant to absorb heat in the air for phase change, thereby completing the transfer of heat, transporting the air heat outside the main unit into a closed drying room, continuously increasing the air temperature in the drying room where the dried materials are placed, and then cooperating with the continuous rotation of the internal axial flow fan, a stable air path circulation will be formed inside the drying room, blowing the materials continuously in a left-right circular or up-down bypass manner, taking out the moisture in the materials, and discharging it outside the drying room through condensation;

[0030] Second step: Add the dried Polygonum multiflorum powder into the solution formed by mixing benzene and sulfuric acid, and let it stand for a period of time after thorough stirring. The volume of the benzene and sulfuric acid solution is five times that of the Polygonum multiflorum powder, the mixing ratio of benzene and sulfuric acid is 5:1, the stirring time is half an hour, and the stirring speed is 1000 revolutions per minute;

[0031] Third step: Filter the standing Polygonum multiflorum solution to obtain the Polygonum multiflorum mother liquor and the Polygonum multiflorum filter residue. The Polygonum multiflorum powder needs to be filtered three times;

[0032] Step 4: Add benzene and a mixed solution of benzene and ethyl acetate to the filtered residue of Polygonum multiflorum. The mixing ratio of benzene to benzene-ethyl acetate is 4:1, and stir here. After standing for a period of time, recrystallize this solution to obtain emodin crystals;

[0033] Step 5: Add sodium hydroxide solution to the solution remaining in Step 4 and stir thoroughly. After standing for a period of time, the staff adjust its pH value to 2-3, then extract with chloroform and concentrate. After standing for a period of time, emodin-6-methyl ether crystals are obtained;

[0034] Step 6: Prepare a sodium bicarbonate solution and extract the mother liquor of Polygonum multiflorum obtained in Step 3 to obtain Solution A. The mass fraction of sodium bicarbonate is 2.5%;

[0035] Stirring is required for two hours during extraction. After thorough mixing and stratification, separation is carried out;

[0036] Step 7: Adjust the pH value of Solution A to 2-3, then extract with chloroform and concentrate. After standing for a period of time, emodin crystals are obtained.

[0037] Unless otherwise specified, the standing time needs to be at least twelve hours to ensure that the corresponding change process can be fully carried out. When the Polygonum multiflorum powder is first extracted, the temperature is 25 degrees, and the regulators for adjusting the pH value are sulfuric acid or sodium hydroxide.

[0038] During stirring, a constant temperature magnetic stirrer can be selected for stirring. The magnetic stirrer utilizes the principles of magnetic field and vortex. Place the container of the liquid to be stirred with the stirring bar sunk on the base of the magnetic stirrer. When the magnetic stirrer is powered on, a rotating magnetic field is generated near the base to drive the stirring bar to move in a circular cycle, and then a vortex is formed in the liquid of the container, thereby achieving the purpose of stirring the liquid. Moreover, the stirrer can set the temperature and display the temperature, can be used for long-term heating, the digital display is intuitive and accurate, and the shell is injection-molded from special flame-retardant reinforced plastic. The magnetic stirrer has very high resistance to heat, acids, alkalis and organic solvents. The stirring speed and heating temperature of the magnetic stirrer can be continuously adjusted, and it is widely applicable to the stirring of solvents with different viscosities.

[0039] Example 1:

[0040] Step 1: First, crush Polygonum multiflorum into powder by a pulverizer, and thoroughly dry the Polygonum multiflorum powder;

[0041] Step 2: Add the dried Polygonum multiflorum powder to the solution formed by mixing benzene and sulfuric acid, and stand for a period of time after thorough stirring for standby;

[0042] Step 3: Filter the standing Polygonum multiflorum solution to obtain the mother liquor of Polygonum multiflorum and the Polygonum multiflorum filter residue;

[0043] Step 4: Add benzene and a mixed solution of benzene-ethyl acetate to the Polygonum multiflorum filter residue, stir for 10 minutes, let it stand for a period of time, and then perform recrystallization on this solution to obtain emodin crystals;

[0044] Step 5: Add sodium hydroxide solution to the remaining solution from the previous step and stir well. After standing for a period of time, adjust its pH value to 2, then extract with chloroform and concentrate. After standing for a period of time, emodin-6-methyl ether crystals are obtained;

[0045] Step 6: Prepare a sodium bicarbonate solution and extract the mother liquor to obtain Solution A;

[0046] Step 7: Adjust the pH value of Solution A to 2, then extract with chloroform and concentrate. After standing for a period of time, emodin crystals are obtained.

[0047] Example 2:

[0048] Step 1: First, use a pulverizer to break Polygonum multiflorum into powder form and thoroughly dry the Polygonum multiflorum powder;

[0049] Step 2: Add the dried Polygonum multiflorum powder to a solution made of benzene and sulfuric acid, stir thoroughly, and let it stand for a period of time for later use;

[0050] Step 3: Filter the standing Polygonum multiflorum solution to obtain the mother liquor of Polygonum multiflorum and the Polygonum multiflorum filter residue;

[0051] Step 4: Add benzene and a mixed solution of benzene-ethyl acetate to the Polygonum multiflorum filter residue, stir for 10 minutes, let it stand for a period of time, and then perform recrystallization on this solution to obtain emodin crystals;

[0052] Step 5: Add sodium carbonate solution to the remaining solution and stir well. After standing for a period of time, the staff adjust its pH value to 3, then extract with chloroform and concentrate. After standing for a period of time, emodin-6-methyl ether crystals are obtained;

[0053] Step 6: Prepare a mixed solution of sodium carbonate and 1% sodium bicarbonate and extract the mother liquor to obtain Solution A;

[0054] Step 7: Adjust the pH value of Solution A to 3, then extract with chloroform and concentrate. After standing for a period of time, emodin crystals are obtained.

[0055] In the present invention, Polygonum multiflorum is first crushed and dried, then initially extracted with benzene and sulfuric acid solution in a volume ratio of 1:5, and filtered. Subsequently, the filter residue and mother liquor obtained after filtration are respectively subjected to recrystallization, extraction and other treatments, and finally an extract of the active ingredients of Polygonum multiflorum is obtained. By adopting the method of multiple extractions, the equipment requirements for extracting the active ingredients from Polygonum multiflorum are reduced, thereby reducing the cost required for extracting the active ingredients from Polygonum multiflorum, lowering the technical requirements for extraction, making this method easier to be popularized. Moreover, during the extraction process, the leaching solution and leaching residue are both comprehensively treated, so as to maximize the extraction rate of the active ingredients in Polygonum multiflorum, reduce the waste caused by the extraction equipment and technological process, improve the utilization rate of Polygonum multiflorum raw materials, and indirectly reduce the cost.

[0056] Enlightened by the ideal embodiments of the present invention described above, through the above description, relevant staff can completely make various changes and modifications without departing from the technical idea of the present invention. The technical scope of the present invention is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A method for extracting and separating effective ingredients of Chinese medicine Polygonum multiflorum, characterized in that: Includes the following step, The first step is to crush the Polygonum multiflorum into powder by a crusher, and fully dry the Polygonum multiflorum powder; The second step is to add the dried Polygonum multiflorum powder into a solution of benzene and sulfuric acid, and then stir thoroughly and let it stand for a period of time for later use; The third step is to filter the standing Polygonum multiflorum solution to obtain a Polygonum multiflorum mother liquor and a Polygonum multiflorum filter residue; The fourth step is to add a mixed solution of benzene and benzene-ethyl acetate to the Polygonum multiflorum filter residue, stir the mixture, and recrystallize the solution after standing for a period of time to obtain rhein crystals; Step 5: Add sodium hydroxide solution to the remaining solution in step 4 and stir thoroughly. After standing for a period of time, the staff adjusts the pH value to 2-3, and then extracts and concentrates it with chloroform. After standing for a period of time, the crystals of rheumatoid artemisia-6-methyl ether are obtained. Step 6, preparing a sodium bicarbonate solution and extracting the Polygonum multiflorum mother liquor obtained in the third step to obtain a solution A; The seventh step is to adjust the pH value of solution A to 2-3, then add chloroform to extract and concentrate, and after standing for a period of time, obtain rhein crystals.

2. The method for extracting and separating the effective ingredients of the Chinese medicine Polygonum multiflorum according to claim 1 is characterized in that: in the first step, the temperature of the Polygonum multiflorum powder is maintained at 40 degrees during drying, and the duration is 5 days, and after the drying is completed, it needs to be taken out from the drying equipment for 24 hours, and then dried.

3. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the second step, the volume of the benzene and sulfuric acid solution is 5 times that of the Polygonum multiflorum powder, and the mixing ratio of benzene and sulfuric acid is 5:

1.

4. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the second step, the stirring time is half an hour, and the stirring speed is 1000 revolutions per minute.

5. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the third step, the Polygonum multiflorum solution needs to be filtered three times.

6. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the fourth step, the mixing ratio of benzene and benzene-ethyl acetate is 4:

1.

7. The method for extracting and separating the effective components of the Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the sixth step, the mass fraction of sodium bicarbonate is 2.5%.

8. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the sixth step, the extraction needs to be stirred for two hours, and separation is performed after sufficient mixing and stratification.

9. The method for extracting and separating the effective ingredients of Chinese medicine Polygonum multiflorum according to claim 1, wherein: In the fifth and seventh steps, the regulator selected for adjusting the pH value is sulfuric acid or sodium hydroxide.

10. The method for extracting and separating the effective components of the Chinese medicine Polygonum multiflorum according to claim 1, characterized in that: The standing time is at least 12 hours to ensure that the corresponding change process can be fully carried out.

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