Puerarin extracting solution purifying device

Abstract

The utility model discloses a puerarin extracting solution purification device, which comprises an extraction kettle (1), an extraction kettle (2), a purification kettle (3) and a purification kettle (4), and is characterized in that the extraction kettle (1) is used for extracting puerarin and obtaining an extracting solution; the micro-filtration membrane (2) is connected to the extraction kettle (1) and is used for performing micro-filtration treatment on the extracting solution; the ultrafiltration membrane (3) is connected to the permeation side of the microfiltration membrane (2) and is used for carrying out ultrafiltration treatment on the penetrating fluid; the first nanofiltration membrane (4) is connected to the permeation side of the ultrafiltration membrane (3) and is used for concentrating the penetrating fluid; the spray dryer (8) is connected to the interception side of the first nanofiltration membrane (4) and is used for carrying out spray drying on the concentrated solution. The device disclosed by the utility model has the advantages that a membrane method or a'membrane and resin 'method purification process is used, the process is short, the consumed time is short, the production efficiency can be effectively improved, the labor cost is reduced, and the quality and the yield of products are also improved.

Description

Technical Field

[0001] The utility model relates to a puerarin separation and purification production process, belonging to the technical field of extraction and separation of effective components of natural products. Background Art

[0002] Pueraria root was first recorded in the Han Dynasty's Shennong's Herbal Classic, where it was listed as a medium-grade herb. It is a commonly used herb in Traditional Chinese Medicine for relieving wind and relieving exterior symptoms. Modern pharmacological experiments have shown that Pueraria root also has antioxidant, circulatory, and blood pressure regulation, blood sugar lowering, tumor suppression, immune enhancement, and memory improvement properties. It also has special therapeutic effects on cardiovascular and cerebrovascular diseases, sudden deafness, eye diseases, alcoholism, and diabetes.

[0003] Puerarin, one of the main active ingredients in Pueraria root, belongs to the isoflavone class of compounds and is a safe and effective drug with extremely low toxicity. It has high clinical and healthcare applications, with benefits such as lowering blood pressure, slowing heart rate, reducing myocardial oxygen consumption, and improving learning and memory. Clinically, it has protective effects on opposite motor neurons, promotes lymphocyte transformation in both healthy individuals and cancer patients, and has a significant stimulating and inducing effect on the interferon system. Consequently, China approved puerarin injection as a new drug for the clinical treatment of cardiovascular and cerebrovascular diseases in the 1990s. Furthermore, the development of Pueraria root as a health food and functional food has become a major global trend, and puerarin-based foods have become recognized health supplements worldwide. Research on puerarin is currently increasing.

[0004] The traditional extraction method for puerarin involves extraction with organic solvents, followed by separation and purification techniques such as chromatography and recrystallization to increase the purity of the active ingredient before clinical application. Existing puerarin purification methods primarily include n-butanol extraction, macroporous resins, column chromatography, low-pressure countercurrent chromatography, supercritical extraction, and liquid chromatography. These traditional separation and purification methods utilize large amounts of organic solvents, increasing costs and causing environmental pollution. Furthermore, the organic solvents used, such as methanol, n-butanol, and ethyl acetate, are highly neurotoxic, making their complete removal from the finished product difficult to meet the demands of domestic and international markets. Furthermore, the production process is complex, the crystallization and recrystallization procedures are cumbersome, energy consumption is high, and the production cycle is long. While separation and purification of puerarin using supercritical extraction and chromatography can significantly increase its purity, their high cost makes them unsuitable for large-scale production. Therefore, a new method for purifying puerarin remains to be discovered. Utility Model Content

[0005] This utility model addresses the shortcomings of current production and provides a "membrane method" or "membrane + resin" purification process. This process has short steps and time consumption, can effectively improve production efficiency, reduce labor costs, and improve product quality and yield. In addition, compared with traditional processes, this process occupies a small area, has a high degree of automation, low operating costs, can reduce evaporation energy consumption, and has good regeneration performance and a long service life, achieving efficient, high-quality, and energy-saving production of puerarin.

[0006] A method for purifying a puerarin extract comprises the following steps:

[0007] Step 1, extracting Pueraria root to obtain an extract;

[0008] Step 2, filtering and purifying the extract obtained in step 1 through a microfiltration membrane and an ultrafiltration membrane, respectively, to obtain a filtrate;

[0009] Step 3: performing a first nanofiltration concentration treatment on the filtrate obtained in step 2, and drying the obtained first concentrated liquid to obtain a puerarin finished product.

[0010] In the step 1, the extraction process adopts water extraction or alcohol extraction.

[0011] In the step 3, the first concentrated liquid needs to be subjected to adsorption and desorption treatment by an adsorption resin, and then the desorbed liquid is subjected to a second nanofiltration concentration treatment and then dried.

[0012] The adsorption resin is D101, AB-8, DM130, HPD100, HPD600 resin, the flow rate is controlled to be 2-5 Bv / h, the temperature is 20-60 DEG C; the desorption liquid is 20%-90% ethanol solution.

[0013] The spray drying air inlet temperature is 130-150℃.

[0014] The microfiltration membrane is a ceramic membrane or an organic membrane.

[0015] The pore size of the ceramic membrane is 1-1200 nm, preferably 4-200 nm. The feed liquid temperature during the ceramic membrane filtration process is 5-80° C., the pressure is 0.1-0.5 MPa, the membrane surface flow rate is 2-5 m / s, and the concentration multiple is 1 to 20 times.

[0016] The pore size of the organic membrane is 20-500nm, the feed liquid temperature in the filtration process is 5-80℃, the pressure is 0.1-1.0Mpa, the membrane surface flow rate is 2-5m / s, and the concentration multiple is 1-20 times.

[0017] The molecular weight cut-off of the ultrafiltration membrane is 1KD-100KD, preferably 1KD-10KD. The feed liquid temperature during the filtration process is 5-45°C, the pressure is 0.3-3.0Mpa, the membrane surface flow rate is 2-5m / s, and the concentration multiple is 1-30 times.

[0018] The molecular weight cutoff of the first nanofiltration membrane and / or the second nanofiltration membrane is 100-1000Da, and the filtration pressure is 0.5-5.0Mpa. In the later stage of nanofiltration concentration, the nanofiltration concentrate needs to be washed with water. In the washing operation, the amount of water added is generally 0.1-3 times the amount of the original liquid.

[0019] A device for purifying puerarin extract, comprising:

[0020] An extraction kettle, used for extracting puerarin and obtaining an extract;

[0021] A microfiltration membrane is connected to the extraction kettle and is used to perform microfiltration treatment on the extract;

[0022] Ultrafiltration membrane, connected to the permeate side of the microfiltration membrane, used for ultrafiltration treatment of the permeate;

[0023] The first nanofiltration membrane is connected to the permeate side of the ultrafiltration membrane and is used to concentrate the permeate;

[0024] The spray dryer is connected to the retentate side of the first nanofiltration membrane and is used for spray drying the concentrated liquid.

[0025] It also includes: an adsorption resin column and a second nanofiltration membrane; and the concentration side of the first nanofiltration membrane is connected to the feed side of the second nanofiltration membrane through the adsorption resin column, and the permeation side of the second nanofiltration membrane is further connected to a spray dryer; the adsorption resin column is used to adsorb and desorb the concentrated liquid obtained from the first nanofiltration membrane, and the second nanofiltration membrane is used to concentrate the desorbed liquid obtained in the adsorption resin column.

[0026] The molecular weight cut-off of the first nanofiltration membrane is 100 to 1000 Da.

[0027] The molecular weight cut-off of the second nanofiltration membrane is 100 to 1000 Da.

[0028] The microfiltration membrane is a ceramic membrane or an organic membrane.

[0029] The pore size of the ceramic membrane is 1-1200 nm, preferably 4-200 nm.

[0030] The pore size of the organic membrane is 20-500nm.

[0031] The molecular weight cut-off of the ultrafiltration membrane is 1KD-100KD, preferably the molecular weight cut-off of the membrane is 1KD-10KD.

[0032] The invention also comprises a desorption liquid storage tank connected to the adsorption resin column and used for supplying desorption liquid into the adsorption resin column.

[0033] The desorption liquid storage tank is filled with ethanol water solution. Beneficial effects

[0034] The advantages of this utility model are: the use of membrane or "membrane + resin" purification process has a short process and short time consumption, which can effectively improve production efficiency, reduce labor costs, and improve product quality and yield. In addition, compared with traditional processes, this process occupies a small area, has a high degree of automation, low operating costs, can reduce evaporation energy consumption, and has good regeneration performance and a long service life, thus achieving efficient, high-quality, and energy-saving production of puerarin. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a process flow chart of the utility model.

[0036] Figure 2 It is an apparatus diagram of the present utility model.

[0037] Among them, 1. extraction kettle; 2. ceramic membrane; 3. ultrafiltration membrane; 4. first nanofiltration membrane; 5. adsorption resin column; 6. desorption liquid storage tank; 7. second nanofiltration membrane; 8. spray dryer. DETAILED DESCRIPTION

[0038] Example

[0039] 200 L of the puerarin extract after water extraction was filtered through a 50 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration to 20 times, demineralized water was added for rinsing at a rate of 30 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 2500 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 150 Da and an operating pressure of 3.0 MPa, yielding a nanofiltration permeate and a nanofiltration concentrate. The nanofiltration concentrate was then fed into a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 51%.

[0040] Example

[0041] 200 L of the puerarin extract after water extraction was filtered through an 8 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration to 20 times, demineralized water was added for rinsing at a rate of 40 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 2000 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 150 Da and an operating pressure of 3.0 MPa, yielding a nanofiltration permeate and a nanofiltration concentrate. The nanofiltration concentrate was then fed into a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 57%.

[0042] Example

[0043] 200 L of ethanol-extracted puerarin extract was filtered through a 100 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration reached 20 times, demineralized water was added for rinsing at a rate of 30 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 3500 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 200 Da and an operating pressure of 3.0 MPa, yielding a nanofiltration permeate and a nanofiltration concentrate. The nanofiltration concentrate was then passed into a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 55%.

[0044] Example

[0045] 200 L of ethanol-extracted puerarin extract was filtered through a 4 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration to 20 times, demineralized water was added for rinsing at a rate of 30 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 3000 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 150 Da and an operating pressure of 2.5-3.5 MPa, yielding nanofiltration permeate 1 and nanofiltration concentrate 1. The nanofiltration concentrate was then passed through an AB-8 adsorption resin and resolved using 40% ethanol to obtain a resolved solution. The lysate was then concentrated through a nanofiltration membrane with a molecular weight cutoff of 100 Da and an operating pressure of 3.0 MPa, yielding nanofiltration permeate 2 and nanofiltration concentrate 2. Nanofiltration concentrate 2 then entered a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 87%.

[0046] Example

[0047] 200 L of ethanol-extracted puerarin extract was filtered through a 100 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration to 20 times, demineralized water was added for rinsing at a rate of 30 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 3500 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 200 Da and an operating pressure of 2.5-3.5 MPa, yielding nanofiltration permeate 1 and nanofiltration concentrate 1. The nanofiltration concentrate was then passed through an AB-8 adsorption resin and resolved using 40% ethanol to obtain a resolved solution. The lysate was then concentrated through a nanofiltration membrane with a molecular weight cutoff of 100 Da and an operating pressure of 3.0 MPa, yielding nanofiltration permeate 2 and nanofiltration concentrate 2. Nanofiltration concentrate 2 then entered a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 82%.

[0048] Example

[0049] 200 L of the puerarin extract after water extraction was filtered through a 50 nm ceramic membrane at a temperature of 25-55°C and a pressure of 0.25 MPa. After concentration to 20 times, demineralized water was added for rinsing at a rate of 30 L, yielding a ceramic membrane permeate and a ceramic membrane concentrate, respectively. The ceramic membrane permeate was further purified by ultrafiltration using an organic membrane with a molecular weight cutoff of 2500 Da and an operating pressure of 2.5 MPa, yielding an ultrafiltration permeate and an ultrafiltration concentrate. The ultrafiltration permeate was then concentrated using a nanofiltration membrane with a molecular weight cutoff of 150 Da and an operating pressure of 2.5-3.5 MPa, yielding nanofiltration permeate 1 and nanofiltration concentrate 1. The nanofiltration concentrate was then passed through an AB-8 adsorption resin and resolved using 40% ethanol to obtain a resolved solution. The lysate was then concentrated through a nanofiltration membrane with a molecular weight cutoff of 100 Da and an operating pressure of 3.0 MPa, yielding nanofiltration permeate 2 and nanofiltration concentrate 2. Nanofiltration concentrate 2 then entered a drying tower with an inlet air temperature of 150°C. The atomizer was activated and the liquid was spray-dried, resulting in a puerarin product with a purity of 84%.

Claims

1. A purifying device for puerarin extract, characterized in that: include: An extraction kettle (1) is used to extract puerarin and obtain an extract; A microfiltration membrane (2) is connected to the extraction kettle (1) and is used to perform microfiltration treatment on the extract; An ultrafiltration membrane (3) is connected to the permeation side of the microfiltration membrane (2) and is used to perform ultrafiltration treatment on the permeate; A first nanofiltration membrane (4) connected to the permeate side of the ultrafiltration membrane (3) and used for concentrating the permeate; The spray dryer (8) is connected to the interception side of the first nanofiltration membrane (4) and is used to spray dry the concentrated liquid.

2. The purifying device for puerarin extract according to claim 1, characterized in that: Also includes: An adsorption resin column (5) and a second nanofiltration membrane (7); the concentration side of the first nanofiltration membrane (4) is connected to the feed side of the second nanofiltration membrane (7) through the adsorption resin column (5), and the permeation side of the second nanofiltration membrane (7) is further connected to a spray dryer (8); the adsorption resin column (5) is used to perform adsorption and desorption purification treatment on the concentrated liquid obtained from the first nanofiltration membrane (4), and the second nanofiltration membrane (7) is used to perform concentration treatment on the desorbed liquid obtained from the adsorption resin column (5).

3. The purification device for puerarin extract according to claim 2, characterized in that: The molecular weight cutoff of the first nanofiltration membrane and / or the second nanofiltration membrane is 100-1000 Da.

4. The purification device for puerarin extract according to claim 2, characterized in that: The microfiltration membrane is a ceramic membrane or an organic membrane.

5. The purification device for puerarin extract according to claim 4, characterized in that: The pore size of the ceramic membrane is 1-1200nm.

6. The purifying device for puerarin extract according to claim 4, characterized in that: The pore size of the organic membrane is 20-500nm.

7. The purifying device for puerarin extract according to claim 1, characterized in that: The molecular weight cut-off of the ultrafiltration membrane is 1KD-100KD.

8. The purifying device for puerarin extract according to claim 1, characterized in that: Also includes: The desorption liquid storage tank (6) is connected to the adsorption resin column (5) and is used to supply the desorption liquid to the adsorption resin column (5).

9. The purifying device for puerarin extract according to claim 8, characterized in that: The desorption liquid storage tank (6) is filled with ethanol aqueous solution.

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