CN114105747B - Method for improving curcumin extraction rate and purification effect - Google Patents
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Abstract
A method for improving curcumin extraction rate and purification effect belongs to the technical field of food additive processing. The invention takes infrared freeze-dried turmeric powder as a raw material, obtains curcumin crude extract through radio frequency-assisted ionic liquid-soybean peptide, and then adopts a macromolecular polysaccharide flocculation technology combined with a macroporous resin method for separation and purification to obtain curcumin dry powder, which specifically comprises the steps of prefreezing, drying, grinding, radio frequency-assisted ionic liquid extraction, separation and purification and the like. The invention adopts radio frequency auxiliary ionic liquid-soybean peptide to extract infrared freeze-dried turmeric powder, has short extraction time, and obtains high-purity curcumin by combining an organic macromolecular flocculation technology with a macroporous resin method.
Description
Technical Field
The invention relates to a method for improving curcumin extraction rate and purification effect, in particular to a method for obtaining high-purity curcumin by using infrared freeze-dried turmeric powder as a raw material, obtaining curcumin crude extract through radio frequency assisted ionic liquid, and then separating and purifying by adopting a flocculation technology combined with a macroporous resin method, and belongs to the technical field of food additive processing.
Background
Turmeric is a dried rhizome of turmeric (Curcuma longa l.) belonging to the genus Curcuma of the family zingiberaceae, which has been used for thousands of years, and is widely used in the flavor, color, and pharmaceutical industries. Curcumin compounds (Curcuminoids) are the main active ingredients in turmeric, are diaryl heptane compounds derived from Zingiberaceae plants, and are mainly present in rhizome of medicinal plants such as turmeric, tulip and zedoary. Since the plant is firstly separated from the plant in 1970 and the molecular structure is determined in 1910, researches for many years find that the plant has various biological activities, such as the effects of regulating blood fat, resisting tumors, viruses and inflammation, preventing Alzheimer's disease and the like, and part of the pharmacological activity of the plant is closely related to the antioxidant effect. Dinkova-Kostova et al (2010) found that curcumin can eliminate free radicals and reduce oxidative damage of organisms. Turmeric is a perennial plant, but the harvest season of turmeric roots is susceptible to seasonality. In subtropical regions (especially in the four kingdom of china), harvesting is usually terminated before summer solstice. Furthermore, the fresh turmeric has a moisture content of about 80%, the presence of which is closely related to enzymatic, chemical and microbial reactions that are closely related to the shelf life and characteristics of the product. Therefore, processing is required to extend the shelf life.
Food drying technology is considered to be one of the most effective industrial preservation methods to extend shelf life (Xu et al, 2017). However, it is difficult to avoid loss of nutrients and disruption of food structure during processing. Freeze-drying preserves to the greatest extent the color, flavor, nutritional and textural characteristics of the product, whose product properties are considered the first choice among all drying techniques (Zhang et al, 2017). The change of tissue, nutrition and antioxidant activity after freeze-drying is small. The freeze-dried product has obvious pore structure, small hardness and good brittleness, and has good advantages in further processing. However, the drying efficiency of freeze-drying is relatively limited, and therefore, an improved heating source is a better choice. Wudaofi (2019) research shows that infrared freeze drying has good drying capacity on cordyceps, sweet potatoes and shanghai green petioles. The main characteristic of infrared drying is that no medium is needed for the transmission of infrared radiation energy from a heat source to a medium, and the material to be dried can be regarded as an infrared radiation absorber. For food products, the differential absorption of protein, fat, carbohydrates and water may affect the uniformity of drying. The surface characteristics of the material, the spectral composition of the radiation source and the direction of the incident radiation also determine the infrared absorption.
The most notable active ingredients in turmeric are curcumin and its analogues, and great efforts have been made to separate and purify curcumin by referring to conventional extraction methods. Wherein the organic solvent extraction method, acid-base extraction method, ionic liquid extraction method, enzyme extraction method, ultrasonic-assisted extraction method, microwave-assisted extraction method, and supercritical CO extraction method 2 Extraction methods are commonly used for research. However, these methods still have disadvantages, such as the crude extract obtained by acid-base extraction is easy to dry, but contains a large amount of starch, which is not beneficial for further refining; the enzyme extraction method has high cost and yield, but the reaction condition is harsh, and the industrial production is difficult to realize; supercritical CO 2 The extraction method can maintain the bioactivity of the effective components, but the equipment is expensive, and the consumption of entrainer is large. The organic solvent extraction method has high extraction yield, simple operation and controllable reaction conditions, and the solvent can be recycled (Leruimin, 2013), but the extraction time is long. Therefore, the aim of the invention is to find a suitable extraction method to avoid the defects, further accelerate the extraction efficiency and realize energy conservation and emission reduction.
The purity of curcumin is also an important limitation in the development of the industry, and curcumin also has great potential in pharmaceutical processing. Among them, activated carbon chromatography, column chromatography, thin-layer chromatography, macroporous resin adsorption, flocculation, and recrystallization are commonly used for research. The active carbon chromatography can effectively adsorb active ingredients, but has the disadvantages of large solvent consumption, complex operation and high cost (Wangxian pure, 2000). The yellow pigment and lipid impurities can be purified and separated by column chromatography, and the obtained product has extremely high purity (Lineli, 2013), but the time is too long. The thin-layer chromatography is a trace high-efficiency and quick separation and detection means, is suitable for separating a mixture with a small amount and simple components, and is not suitable for high-efficiency production.
Chumroenphat et al (2020) studied the drying effect of different drying techniques on turmeric, and found that the freeze-drying technique exhibited good nutrient retention and antioxidant activity in the drying of turmeric, further confirming the superiority of freeze-drying in the drying of turmeric. But the method has the disadvantages that the heating efficiency is relatively low by adopting the traditional electric heating plate for heating, and the drying time is obviously longer than that of hot air drying under the same vacuum condition and temperature. The invention is different from the method in that infrared radiation heating is used instead, thereby shortening the drying time and ensuring the product quality.
Zhang Youling et al (2005) used orthogonal experiments to explore the influence of amylase, pectinase and cellulase dosage on curcumin extraction, and the experimental results showed that adding 5mL of amylase solution with 800 μ/mL enzyme activity, 0.5mL of pectinase solution with 300 μ/mL enzyme activity and 2mL of cellulase solution with 30 μ/mL enzyme activity to 30g of turmeric powder, the enzymolysis efficiency was the highest, and the extraction rate was as high as 5.47%. However, the purchase cost of the enzyme solution is high, and the requirements of the enzyme solution on the conditions are severe. The difference between the method and the device is that the radio frequency assisted ionic liquid method is used instead, so that the production cost is reduced.
Liang et al (2017) extracted curcumin using microwave-assisted ionic liquid, and the results showed that the optimal extraction solvent was 0.3mol/L [ OMIM ] Br. The extraction rate is taken as a reference index, and the optimal conditions are as follows: the extraction temperature is 55 ℃, the extraction time is 8min, the solid-to-liquid ratio is 0.5/30 (g/mL), and the average yield of the three curcumins is 1.77%. Compared with ultrasonic-assisted extraction, microwave-assisted extraction is an efficient and pollution-free method, and has shorter extraction time and lower energy consumption. The invention is different from the method in that the radio frequency assisted ionic liquid method is used instead, so that the phenomenon of microwave overheating is alleviated, and the extraction rate of curcumin can be improved.
Rohai et al (2010) used orthogonal experiments to investigate entrainer dosage, extraction pressure, extraction temperature, extraction time and CO 2 The influence of the flow rate on curcumin extraction is found, the dosage of the entrainer is the primary factor influencing the extraction, and the optimal extraction conditions are that the dosage of the entrainer is 200mL, the extraction pressure is 35MPa, the extraction temperature is 40 ℃, the extraction time is 3h, and when the flow of carbon dioxide is 30L/h, the curcumin content is 14.317mg/g. Long extraction time, high machine cost and the like. The invention is different from the method in that the radio frequency assisted ionic liquid method is used, so that the extraction time is shortened, and the processing cost is saved.
The LiRuanmin (2013) adopts a flocculant compounding method for clarifying the fresh turmeric extract. Through screening, the chitosan flocculation effect is found to be good, and the optimal flocculation process is as follows: the adding amount of chitosan is 0.4g/L, the heating time is 1h, and the heating temperature is 40 ℃. The compounding experiment of several reagents shows that the compounding effect of chitosan and polyaluminium chloride is optimal, and the optimal addition amount is as follows: 0.35g/L of chitosan and 0.05g/L of polyaluminum chloride. This document demonstrates the desirability of the flocculation technique of macromolecular cationic polysaccharides for separation, but chitosan is of limited source and costly to prepare.
Daihong (2008) concentrating 70% ethanol extractive solution of Curcuma rhizome to obtain crude extract, dissolving with 2.5% NaOH solution, adjusting pH to =7 with glacial acetic acid to obtain yellow flocculent precipitate, and filtering to obtain dry crude curcumin. Recrystallizing the curcumin crude product with n-propanol for 2 times to obtain orange needle-shaped curcumin pure product with the purity of more than 95 percent and the yield of about 2.1 percent. The method meets the requirement of C95 in product purity, but the dosage of the organic solvent is more. The invention is different from the method in that the flocculation technology is combined with a macroporous resin method, so that the use of organic solvent is reduced.
Zhangyu et al (2010) further purified the curcumin reflux extract by silica gel column chromatography, using a mixed solution of chloroform and methanol (75). The column chromatography of the cassia gum has simple experimental process, saves energy and time, has higher extraction efficiency, complete separation and higher yield and purity of the total curcumin, and is more suitable for separating and purifying a small amount of samples in a laboratory. The invention is different from the method in that the flocculation technology is combined with a macroporous resin method, thus being applicable to industrial production and improving the purity of the sample.
Disclosure of Invention
The invention aims to further improve the extraction rate of curcumin and the purity of a final product from the aspects of raw materials (porous and loose nano particles), extraction means (radio frequency assisted ionic liquid combined with soybean peptide) and separation and purification (flocculation technology combined with a macroporous resin method).
The technical scheme of the invention is as follows:
the method for improving the curcumin extraction rate and the purification effect comprises the steps of prefreezing, drying, grinding, radio frequency assisted ionic liquid extraction, centrifugation, separation and purification and the like, and specifically comprises the following steps:
a method for improving curcumin extraction rate and purification effect is characterized by comprising the following specific steps:
(1) Pre-freezing: the dried and cleaned turmeric root tuber is cut according to the thickness of 3-5 mm, and is put into a refrigerator for freezing.
(2) Infrared freeze drying: and after the temperature of the cold trap is reduced to-40 ℃, putting the pre-frozen curcuma longa slices into an infrared drying oven, and performing infrared freeze drying.
(3) Grinding: and grinding the naturally cooled turmeric slices into powder.
(4) Extraction: the [ OMIM ] Br and soybean peptide are selected as extraction solvents, and radio frequency is selected as an auxiliary means for extraction.
(5) Primary purification: separating the crude extract of Curcuma rhizome by flocculation of organic macromolecular Curcuma rhizome polysaccharide.
(6) Deep purification: and (3) purifying the flocculation residual liquid by using DM301 macroporous resin.
Further, the case in the step (1) is specifically: soaking and washing with clear water for 1-2 times, then washing for 2-3 times after removing water, standing at room temperature and draining the external water. The pre-freezing temperature is-40 to-80 ℃, and the pre-freezing time is 6 to 8 hours.
Further, the case in the step (2) is specifically: after the vacuum degree of the drying oven is reduced to 80pa, the heating is started again, the heating temperature is 40-70 ℃, and the drying time is 3-4.5 h.
Further, the condition in the step (3) is specifically that: crushing by a ball mill crusher at a temperature of 3.5-4.5 ℃, wherein the temperature of the ball mill crusher is set to be 3.5-4.5 ℃, and the materials and ZrO are mixed 2 The proportion of grinding beads is 1:5, the particle size of the turmeric powder is 300-600 nm.
Further, the case in the step (4) is specifically: putting the screened powder into a container, adding [ OMIM ] Br and soybean peptide as a combined extraction solvent, wherein the concentrations of [ OMIM ] Br and soybean peptide in the combined extraction solvent are respectively 0.2-0.6 mol/L and 0.1-1% by weight; the ratio of material to liquid is 1: 10-1: 50, extracting under 6kW, 27.12MHz and 10-30 mm plate spacing, centrifuging for 10min at 4000r/min after extracting for 5-30 min, and taking supernatant to obtain curcumin crude extract.
Further, the case in the step (5) is specifically: weighing a proper amount of turmeric crude extract, adding 0.5-1 wt% of prepared turmeric polysaccharide flocculation solution, shaking up, flocculating at the temperature of 20-60 ℃ for 30-90 min, standing at room temperature for a certain time, and filtering to obtain clear liquid.
Further, the case in the step (6) is specifically: DM301 was selected for purification experiments. In the process of macroporous resin adsorption, 8-10 g of resin is weighed and placed in a container, 100mL of clarified liquid obtained in the step (5) is added, the container is sealed, and the mixture is subjected to constant-temperature water bath oscillation for 24 hours at room temperature and 130r/min for full adsorption. Loading the adsorbed macroporous resin into a column, adding deionized water with the same volume as the macroporous resin, eluting with 70% ethanol solution as eluent, concentrating the collected solution under reduced pressure to recover solvent, and vacuum drying at 50 deg.C.
The invention has the beneficial effects that:
(1) Compared with the hot air drying method, the infrared freeze drying method is adopted to dry the turmeric slices, the drying time is short, the nutrient retention rate is high, and the structure is loose and easy to grind.
(2) Compared with the ionic liquid and soybean peptide combined extraction method, the method for extracting curcumin by adopting the radio frequency assisted ionic liquid and soybean peptide combined extraction method has the advantages of shorter extraction time and higher extraction rate.
(3) The curcumin is purified by adopting a macromolecule curcuma polysaccharide flocculation method and a macroporous resin method, and the purity of the curcumin is high.
Drawings
Fig. 1 is a schematic diagram of an rf device according to the present invention.
Fig. 2 is a schematic diagram of the infrared freeze-drying device of the present invention.
In the figure: 1. a radio frequency oscillator; 2. a control panel; 3. a top/bottom electrode plate; 4. a sample; 5. a conveyor belt; 6. a distributed optical fiber temperature sensor; 7. a computer; 8. a fixed structure; 9. distributing hot air; 10. a hot air generator; 11. a control and display panel; 12. an infrared lamp temperature sensor; 13. a material surface temperature sensor; 14. an infrared heating lamp tube system; 15. a carrier; 16. a load bearing sensor; 17. drying the cavity; 18. an observation window; 19. a drying door; 20. a condenser; 21. a refrigerator and fan system; 22. and a vacuum pump.
Detailed Description
In order to make the content of the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments.
Example 1 drying, extraction, purification of high purity curcumin
In this example, the turmeric pieces were rinsed 2 times with clear water, then rinsed 2 times after removing the water, and left to stand at room temperature to drain the external moisture. The dried and cleaned turmeric root tuber is cut according to the thickness of 3-5 mm and is frozen for 6 hours in a refrigerator at the temperature of minus 80 ℃. Pulverizing Curcuma rhizome slices after infrared freeze drying at 50 deg.C for 4 hr (ball milling pulverizer temperature is 4 deg.C, mixing with ZrO 2 The proportion of grinding beads is 1: 5) To obtain 300nm turmeric powder particles. Weighing 2.0g of Curcuma rhizome powder in a 100mL round-bottom flask, and combining with [ OMIM ] in the extractive solution]The Br concentration is 0.3mol/L, the soybean peptide concentration is 0.3% wt, and the material-liquid ratio is 1:30, extracting at 6kW, 27.12MHz and 20mm plate spacing for 10min. Centrifuging at 4000r/min for 10min, and collecting supernatant to obtain curcumin crude extract. Under the condition, the extraction rate of the crude curcumin is 5.79 percent. Weighing appropriate amount of curcumin crude extract, adding prepared Curcuma rhizome polysaccharide flocculation solution to obtain Curcuma rhizome polysaccharide content of 0.5 wt%, shaking, flocculating at 40 deg.C for 60min, standing at room temperature for a certain time, and filtering to obtain clarified solution. And (3) performing adsorption-desorption purification treatment by adopting DM301, adding macroporous resin DM301 into the obtained ethanol extract according to the mass-volume ratio of 100g/L, oscillating in a constant-temperature water bath at room temperature of 130r/min for 24h, and filtering to obtain the well-adsorbed macroporous adsorption resin. Loading the adsorbed macroporous resin into column, adding deionized water, eluting with 70% ethanol solution at flow rate of 2mL/min, collecting by stages, performing qualitative detection on the collected solution by HPLC, and mixingCollecting liquid containing the same components, and recovering the solvent to dryness; the detection conditions of the HPLC method are as follows: ODS column (5um, 4.6 mm. Times.150 mm), mobile phase: acetonitrile and glacial acetic acid solution with volume concentration of 1.0% 42:58, flow rate of 1mL/min, detection wavelength of 430nm. Washing the obtained solid with water until no ethanol smell is generated, and vacuum drying at 50 deg.C to obtain curcumin powder with purity of 94.3%.
Comparative example 1 Ionic liquid extraction Process
In this example, the turmeric pieces were rinsed 2 times with clear water, then rinsed 2 times after removal of water, and allowed to stand at room temperature to drain the external moisture. The dried and cleaned turmeric root tuber is cut according to the thickness of 3-5 mm and is frozen for 6 hours in a refrigerator at the temperature of minus 80 ℃. Pulverizing Curcuma rhizome slices after infrared freeze drying at 50 deg.C for 4 hr (ball milling pulverizer temperature is 4 deg.C, mixing with ZrO 2 The proportion of grinding beads is 1: 5) To obtain 300nm turmeric powder particles. Weighing 2.0g of Curcuma rhizome powder in a 100mL round-bottom flask, and combining with [ OMIM ] in the extractive solution]The Br concentration is 0.3mol/L, the feed-liquid ratio is 1:30, the extraction time is 90min. Centrifuging at 4000r/min for 10min, and collecting supernatant to obtain curcumin crude extract. Under the condition, the extraction rate of the crude curcumin is 3.10 percent. Weighing appropriate amount of curcumin crude extract, adding prepared Curcuma rhizome polysaccharide flocculation solution to obtain Curcuma rhizome polysaccharide content of 0.5 wt%, shaking, flocculating at 40 deg.C for 60min, standing at room temperature for a certain time, and filtering to obtain clarified solution. Performing adsorption-desorption purification treatment by using DM301, adding macroporous resin DM301 into the obtained ethanol extract according to the mass-volume ratio of 100g/L, oscillating in a constant-temperature water bath at room temperature of 130r/min for 24h, and filtering to obtain the well-adsorbed macroporous adsorption resin. Loading the adsorbed macroporous resin into a column, adding deionized water mentioned with macroporous resin and the like, eluting by using an ethanol solution with the volume concentration of 70% as an eluent at the flow rate of 2mL/min, collecting in sections, carrying out qualitative detection on the collected liquid by using an HPLC method, combining the collected liquids containing the same components, and recovering the solvent until the solvent is dry; the detection conditions of the HPLC method are as follows: ODS column (5um, 4.6 mm. Times.150 mm), mobile phase: acetonitrile and 1.0% by volume glacial acetic acid solution 42:58, flow rate of 1mL/minThe detection wavelength is 430nm. Washing the obtained solid with water until no ethanol smell is produced, and vacuum drying at 50 deg.C to obtain curcumin powder with purity of 93.8%.
Comparative example 2 macroporous resin DM301 purification comparison
In this example, the turmeric pieces were rinsed 2 times with clear water, then rinsed 2 times after removal of water, and allowed to stand at room temperature to drain the external moisture. The dried and cleaned turmeric root tuber is cut according to the thickness of 3-5 mm and is frozen for 6 hours in a refrigerator at the temperature of minus 80 ℃. Pulverizing Curcuma rhizome slices subjected to infrared freeze drying at 50 deg.C for 4 hr (at 4 deg.C in ball mill pulverizer), mixing with ZrO 2 The proportion of grinding beads is 1: 5) To obtain 300nm turmeric powder particles. Weighing 2.0g of Curcuma rhizome powder in a 100mL round-bottom flask, and combining with [ OMIM ] in the extractive solution]The Br concentration is 0.3mol/L, the soybean peptide concentration is 0.3% wt, and the material-liquid ratio is 1:30, extracting at 6kW, 27.12MHz and 20mm plate spacing for 10min. Centrifuging at 4000r/min for 10min, and collecting supernatant to obtain curcumin crude extract. Under the condition, the extraction rate of the crude curcumin is 5.79 percent. Weighing a proper amount of curcumin crude extract, carrying out adsorption-desorption purification treatment by adopting DM301, adding macroporous resin DM301 into the obtained ethanol extract according to the mass-volume ratio of 100g/L, oscillating in a constant-temperature water bath at room temperature of 130r/min for 24h, and filtering to obtain the well-adsorbed macroporous adsorption resin. Loading the adsorbed macroporous resin into a column, adding deionized water mentioned with the macroporous resin and the like, eluting by using an ethanol solution with the volume concentration of 70% as an eluent at the flow rate of 2mL/min, collecting in sections, carrying out qualitative detection on the collected liquid by using an HPLC method, combining the collected liquids containing the same components, and recovering the solvent until the solvent is dry; the detection conditions of the HPLC method are as follows: ODS column (5 μm,4.6 mm. Times.150 mm), mobile phase: acetonitrile and glacial acetic acid solution with volume concentration of 1.0% 42:58, flow rate of 1mL/min, detection wavelength of 430nm. Washing the obtained solid with water until no ethanol smell is generated, and vacuum drying at 50 deg.C to obtain curcumin powder with purity of 85.7%.
Claims (7)
1. A method for improving curcumin extraction rate and purification effect is characterized by comprising the following specific steps:
(1) Pre-freezing: cutting the drained and cleaned turmeric root tuber according to the thickness of 3-5 mm, and putting the turmeric root tuber into a refrigerator for freezing;
(2) And (3) infrared freeze drying: after the temperature of the cold trap is reduced to-40 ℃, putting the pre-frozen curcuma longa slices into an infrared drying oven, and performing infrared freeze drying;
(3) Grinding: grinding the naturally cooled turmeric slices into powder;
(4) Extraction: extracting by using [ OMIM ] Br in combination with soybean peptide as an extraction solvent and using radio frequency as an auxiliary means; the method specifically comprises the following steps: putting the screened powder into a container, adding [ OMIM ] Br and soybean peptide as a combined extraction solvent, wherein the concentrations of the [ OMIM ] Br and the soybean peptide in the combined extraction solvent are 0.2-0.6 mol/L and 0.1-1% by weight respectively; the ratio of material to liquid is 1: 10-1: 50; the radio frequency is extracted for 5-30 min under the conditions of 6kW, 27.12MHz and 10-30 mm plate spacing;
(5) Primary purification: separating the crude extract of Curcuma rhizome by flocculation of organic macromolecular Curcuma rhizome polysaccharide; the method specifically comprises the following steps: weighing a proper amount of turmeric crude extract, adding 0.5-1 wt% of prepared turmeric polysaccharide flocculation solution, shaking up, flocculating at the temperature of 20-60 ℃ for 30-90 min, standing at room temperature for a certain time, and filtering to obtain a clarified liquid;
(6) Deep purification: and purifying the flocculation residual liquid by using DM301 macroporous resin.
2. The method for improving the extraction rate and the purification effect of curcumin as claimed in claim 1, wherein the condition of step (1) is specifically: soaking and washing for 1-2 times by using clear water, then washing for 2-3 times after removing water, and standing at room temperature to drain external water; the pre-freezing temperature is-40 to-80 ℃, and the pre-freezing time is 6 to 8 hours.
3. The method for improving curcumin extraction rate and purification effect as claimed in claim 1, wherein the condition of step (2) is specifically: and after the vacuum degree of the drying oven is reduced to 80pa, starting heating, wherein the heating temperature is 40-70 ℃, and the drying time is 3-4.5 h.
4. The method for improving the extraction rate and the purification effect of curcumin as claimed in claim 1, wherein the condition of step (3) is specifically: crushing by a ball mill crusher at the temperature of 3.5-4.5 ℃, wherein the temperature of the ball mill crusher is set to be between material and ZrO 2 The proportion of grinding beads is 1: and 5, the particle size of the turmeric powder is 300-600 nm.
5. The method for improving the extraction rate and purification effect of curcumin as claimed in claim 1, wherein in step (4), after extraction, centrifugation is carried out at 4000r/min for 10min, and the supernatant is taken to obtain crude curcumin extract.
6. The method for improving curcumin extraction rate and purification effect as claimed in claim 1, wherein the condition of step (6) is specifically: selecting DM301 for purification experiment; and (3) weighing 8-10 g of resin in the macroporous resin adsorption process, placing the resin in a container, adding 100mL of the clarified liquid obtained in the step (5), sealing, and oscillating in a constant-temperature water bath at room temperature and 130r/min for 24 hours for full adsorption.
7. The method as claimed in claim 6, wherein in step (6), the adsorbed macroporous resin is loaded into a column, deionized water with the same volume as that of the macroporous resin is added for eluting, an ethanol solution with a volume concentration of 70% is used as an eluent for elution, the collected solution is subjected to reduced pressure concentration to recover the solvent, and vacuum drying is performed at 50 ℃.
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