阅读说明：本技术 一种基于纳米纤维材料的黄芩苷的提取方法 (Method for extracting baicalin based on nanofiber material ) 是由 戎非 傅志贤 于 2021-08-27 设计创作，主要内容包括：本发明涉及一种基于纳米纤维材料的黄芩苷的提取方法,属于中草药有效成分提取技术领域,通过将纳米纤维引入到天然提取中,以纳米纤维为吸附剂,应用其比表面积大、吸附容量大以及易于针对目标物改性,没有有害物质的夹带等优势,分离提纯传统中药中的重要活性成分。吸附效率和解吸效率明显高于常用的大孔树脂HPD-100和AB-8；同时,本发明的方法操作简单,耗时短,易自动化程序操作,能在线工作,大大降低固定相用量,从而降低提取器件制作成本,适合食品药物生产,使用中有毒有害试剂不用或量少,节约能源而环境友好。(The invention relates to a method for extracting baicalin based on a nanofiber material, which belongs to the technical field of extraction of effective components of Chinese herbal medicines. The adsorption efficiency and desorption efficiency are obviously higher than that of the common macroporous resin HPD-100 and AB-8; meanwhile, the method disclosed by the invention is simple to operate, short in time consumption, easy to operate in an automatic program, capable of working on line and greatly reducing the using amount of the stationary phase, thereby reducing the manufacturing cost of the extraction device, and is suitable for food and drug production, free from or less in toxic and harmful reagents in use, energy-saving and environment-friendly.)

1. A method for extracting baicalin based on a nanofiber material is characterized by comprising the following steps:

(1) adsorption and enrichment of baicalin: passing the filtrate of baicalin through extraction column filled with nanofiber, or pressurizing or vacuum sucking, or static adsorption method to adsorb baicalin component in the filtrate onto nanofiber;

(2) and (3) elution: eluting with 20-50% ethanol solution as eluent, and collecting eluate;

(3) concentrating and drying: and placing the collected eluent into an evaporation vessel, carrying out reduced pressure distillation or rotary evaporation concentration, stopping concentration after the ethanol is evaporated, and drying under reduced pressure to obtain the baicalin.

2. The method for extracting baicalin based on nanofiber material as claimed in claim 1, wherein in the step (1), the baicalin filtrate is obtained by the following steps:

(1.1) pretreating medicinal materials: pulverizing Scutellariae radix, sieving with 40-60 mesh sieve, and packaging in sample bags;

(1.2) extracting: reflux-extracting Scutellariae radix powder and ethanol solution to obtain extractive solution;

(1.3) filtering: mixing extractive solutions, standing to room temperature, filtering, collecting filtrate, centrifuging, and collecting supernatant;

(1.4) acid adjustment: adjusting pH of the extractive solution to 2-3, and adjusting ionic strength of the extractive solution to obtain baicalin filtrate.

3. The method for extracting baicalin based on nanofiber material as claimed in claim 2, wherein: in the step (1.2), the method specifically comprises the following steps: according to the ratio of the mass of the radix scutellariae powder to the mass of the 75% ethanol solution of 1: reflux extracting at 80 deg.C for 3 times at 10-25 deg.C, each time for 1.5-4 hr.

4. The method for extracting baicalin based on nanofiber material as claimed in claim 2, wherein: in the step (1.4), the method specifically comprises the following steps: to the direction ofSlowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH, and adding Na₂SO₄Regulating the ionic strength of the extractive solution to 1-3% to obtain baicalin filtrate.

5. The method for extracting baicalin based on nanofiber material as claimed in claim 1, wherein: in the step (1), the nano-fiber is a high polymer material, and the high polymer material is selected from polystyrene, nylon 6, polyvinylpyrrolidone and polyacrylonitrile.

6. The method for extracting baicalin based on nanofiber material as claimed in claim 5, wherein: and dissolving one or more nano fibers in a tetrahydrofuran, N, N-2 methyl formamide solvent, and obtaining the single-component or multi-component nano fibers by adopting an electrostatic spinning method.

7. The method for extracting baicalin based on nanofiber material as claimed in claim 6, wherein: the electrostatic spinning method comprises the following steps: dissolving one or more of the polymer materials in a mixed solution of THF and DMF to prepare a spinning solution with the concentration of 10-25%, uniformly stirring, and adding the spinning solution into a glass syringe for electrospinning; the electrostatic spinning conditions comprise that the voltage of a positive electrode is 10.5-12.5kV, the voltage of a negative electrode is 1.5-2.5kV, the receiving distance is 10-25cm, and the flow rate of a spinning solution is 0.8-1.5 mL/h.

8. The method for extracting baicalin based on nanofiber material as claimed in claim 1, wherein: in the step (1), the static adsorption method comprises the following steps: filtering with medical gauze to obtain filtrate containing baicalin, completely submerging the nanofiber in the filtrate, and taking out the nanofiber after enrichment and adsorption.

Technical Field

The invention belongs to the technical field of extraction of effective components of Chinese herbal medicines, and particularly relates to a method for extracting baicalin based on a nanofiber material.

Background

Baicalin is an effective flavonoid component extracted from traditional Chinese medicine scutellaria baicalensis, and experiments in vivo and in vitro prove that the baicalin has remarkable oxidation resistance and can relieve ischemia reperfusion injury of brain tissues and myocardial tissues; can reduce the damage of glutamic acid and hydrogen peroxide to isolated nerve cells; the structural particularity of the iron chelate makes the iron chelate generate strong chelation with metal ions, and the iron chelate can be used for assisting in treating the Parkinson's disease. Recent studies have shown that baicalin may be a prolyl oligopeptidase inhibitor, which is a very attractive basis for the development of new methods for the treatment of schizophrenia.

At present, baicalin tablets have been used as adjuvant drugs for the clinical treatment of hepatitis. Separation and purification means of baicalin have been developed including solvent extraction, solvent separation, supercritical fluid extraction, and High Speed Counter Current Chromatography (HSCCC); however, these methods have disadvantages such as waste of large amounts of solvent, inefficiency, time-consuming, low throughput, or the need for special equipment.

In recent years, the study of efficient and novel adsorption materials has been a new challenge for nanoscience and nanotechnology. Among the different nanostructured materials, nanofiber membranes produced by electrospinning techniques have received much attention due to their structural features, such as high surface area, high porosity and interconnectivity, good structural stability and controllable thickness. Because the nano-fiber can control the form and the required functions through the electrospinning technology, the nano-fiber has high application potential and mainly comprises the fields of medicine, filtration, sensors, composite materials, energy, catalysis and the like. The method is currently used for extracting, removing and filtering environmental pollutants such as heavy metal ions, dyes, pesticides and the like in practical samples.

Disclosure of Invention

The technical problem is as follows: the invention aims to provide a method for extracting baicalin based on a nanofiber material, which introduces nanofibers into natural extraction, takes the nanofibers as an adsorbent, and separates and purifies important active ingredients in the traditional Chinese medicine.

The technical scheme is as follows: the invention adopts the following technical scheme: a method for extracting baicalin based on nanofiber materials comprises the following steps:

(1) adsorption and enrichment of baicalin: passing the filtrate of baicalin through extraction column filled with nanofiber, or pressurizing or vacuum sucking, or static adsorption method to adsorb baicalin component in the filtrate onto nanofiber;

(2) and (3) elution: eluting with 20-50% ethanol solution as eluent, and collecting eluate;

(3) concentrating and drying: and placing the collected eluent into an evaporation vessel, carrying out reduced pressure distillation or rotary evaporation concentration, stopping concentration after the ethanol is evaporated, and drying under reduced pressure to obtain the baicalin.

Further, in the step (1), the baicalin filtrate is obtained through the following steps:

(1.1) pretreating medicinal materials: pulverizing Scutellariae radix, sieving with 40-60 mesh sieve, and packaging in sample bags;

(1.2) extracting: reflux-extracting Scutellariae radix powder and ethanol solution to obtain extractive solution;

(1.3) filtering: mixing extractive solutions, standing to room temperature, filtering, collecting filtrate, centrifuging, and collecting supernatant;

(1.4) acid adjustment: adjusting pH of the extractive solution to 2-3, and adjusting ionic strength of the extractive solution to obtain baicalin filtrate.

Further, in the step (1.2), the method specifically comprises the following steps: according to the ratio of the mass of the radix scutellariae powder to the mass of the 75% ethanol solution of 1: reflux extracting at 80 deg.C for 3 times at 10-25 deg.C, each time for 1.5-4 hr.

Further, in the step (1.4), the method specifically comprises the following steps: slowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH, and adding Na₂SO₄Regulating the ionic strength of the extractive solution to 1-3% to obtain baicalin filtrate.

Further, in the step (1), the nanofibers are made of a polymer material, and the polymer material is selected from Polystyrene (PS), nylon 6(PA6), polyvinylpyrrolidone (PVP), and Polyacrylonitrile (PAN).

Further, dissolving one or more nano fibers in tetrahydrofuran, N, N-2 methyl formamide solvent, and obtaining single-component or multi-component nano fibers by adopting an electrostatic spinning method.

Further, the electrostatic spinning method is specifically as follows: dissolving one or more of the above polymeric materials in a mixed solution of THF and DMF to obtain a spinning solution with a concentration of 10-25%, uniformly stirring for 12h, adding the spinning solution into a glass syringe (diameter about 2cm) for electrospinning. The electrostatic spinning conditions comprise that the voltage of a positive electrode is 10.5-12.5kV, the voltage of a negative electrode is 1.5-2.5kV, the receiving distance is 10-25cm, and the flow rate of a spinning solution is 0.8-1.5 mL/h.

Further, in the step (1), the static adsorption method is as follows: filtering with medical gauze to obtain filtrate containing baicalin, completely submerging the nanofiber in the filtrate, and taking out the nanofiber after enrichment and adsorption.

Has the advantages that: compared with the prior art, the extraction method of baicalin based on the nanofiber material has the biggest characteristic that the nanofiber has a large specific surface area, the nanofiber is introduced into natural extraction, and the nanofiber is used as an adsorbent, so that the method has the advantages of large specific surface area, large adsorption capacity, easiness in modification aiming at a target object, no entrainment of harmful substances and the like, and can be used for separating and purifying important active ingredients in the traditional Chinese medicine. The adsorption efficiency and desorption efficiency are obviously higher than that of the common macroporous resin HPD-100 and AB-8; the method has the advantages of simple operation, short consumed time, easy automatic program operation, online work and great reduction of the using amount of the stationary phase, thereby reducing the manufacturing cost of the extraction device, being suitable for food and drug production, having no or little toxic and harmful reagents in use, saving energy and being environment-friendly.

Drawings

FIG. 1 is an electron microscope image of nanofibers;

FIG. 2 adsorption rates of baicalin on different adsorption carriers (7.5% PVP + 15% PS fiber and macroporous resins HPD-100 and AB-8);

FIG. 3 the desorption rate of baicalin on different adsorbents;

Detailed Description

The present invention will be described in detail with reference to the following embodiments.

A method for extracting baicalin based on nanometer materials comprises the following steps:

(1) removing impurities from Scutellariae radix, pulverizing to 40-60 mesh, and weighing a certain amount of Scutellariae radix powder;

(2) according to the ratio of the mass of the radix scutellariae powder to the feed liquid of the 75% ethanol solution of 1: 10-25, reflux extracting at 80 deg.C for 3 times, each time for 1.5-4 hr;

(3) mixing the three extractive solutions, standing to room temperature, filtering with medical gauze, collecting filtrate, centrifuging, and collecting supernatant;

(4) slowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH to 2-3, and adding Na₂SO₄Regulating the ionic strength of the solution to 1-3%;

(5) adsorption and enrichment of baicalin: passing the filtrate through an extraction column filled with nanofibers, or by pressurizing or vacuum suction, or by static adsorption to adsorb baicalin component in the filtrate onto the nanofibers;

(6) and (3) elution: eluting with 20-50% ethanol as eluent, and collecting eluate;

(7) concentrating and drying: and placing the collected eluent into an evaporation vessel, carrying out reduced pressure distillation or rotary evaporation concentration, stopping concentration after the ethanol is evaporated, and drying under reduced pressure to obtain the baicalin.

The nano extraction fiber extraction membrane is made of high molecular materials such as Polystyrene (PS), nylon 6(PA6), polyvinylpyrrolidone (PVP), Polyacrylonitrile (PAN) and the like, and one or more materials are mixed into a solvent of tetrahydrofuran and N, N-2 methyl formamide to obtain single-component or multi-component nano fibers by an electrostatic spinning method.

The static adsorption method comprises the following steps: filtering with medical gauze to obtain filtrate containing baicalin, completely submerging the nanofiber in the filtrate, and taking out the nanofiber after enrichment and adsorption.

Example 1

A method for extracting baicalin based on nanometer materials comprises the following steps:

firstly, preparing a nanofiber membrane:

2.04gPS was put into a mixed solution of THF and DMF (both volumes 10 mL: 10mL) to prepare a 10 wt% PS dope, which was uniformly stirred for 12 hours and then charged into a glass syringe (diameter about 2cm) to carry out electrospinning. The spinning voltage is 12kV at the anode, 2kV at the cathode, the polar distance is 20cm, and the advancing speed is 1.5 mL/h. And after spinning is finished, taking the nanofiber membrane off the aluminum foil, and drying the nanofiber membrane in a vacuum drying oven for 1.5 hours at the temperature of 70 ℃ to remove residual solvent so as to ensure the safety of the used material. Thus, nanofibers for baicalin extraction can be obtained (fig. 1).

II, extraction:

(1) removing impurities from Scutellariae radix, pulverizing to 40-60 mesh, and weighing 10g Scutellariae radix powder.

(2) According to the mass of the radix scutellariae powder and 75% ethanol, the ratio of material to liquid is 1: 10 mixing, and extracting under reflux at 80 deg.C for 3 times, each time under reflux for 1.5 hr.

(3) And (3) filtering: mixing extractive solutions, standing to room temperature, filtering with medical gauze, collecting filtrate, centrifuging, and collecting supernatant.

(4) Acid adjustment: slowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH to 3, and adding Na₂SO₄The solution was adjusted to 1% ionic strength.

(5) Adsorption and enrichment of baicalin: the filtrate is passed through an extraction column containing nanofibers, or by suction under pressure or vacuum.

(6) And (3) elution: eluting with 50% ethanol as eluent, and collecting eluate. The desorption rate was calculated to be 90.2%.

(7) Concentrating and drying: placing the collected eluate in an evaporation vessel, distilling under reduced pressure or rotary evaporation concentrating, stopping concentrating after ethanol is evaporated, and vacuum drying to obtain baicalin.

Example 2

A method for extracting baicalin based on nanometer materials comprises the following steps:

firstly, preparing a nanofiber membrane:

2.04g of PVP was put into a mixed solution of THF and DMF (both in a volume of 10 mL: 10mL) to prepare a 10 wt% PVP spinning solution, which was uniformly stirred for 12 hours and then charged into a glass syringe (diameter about 2cm) to carry out electrospinning. The spinning voltage is 11kV at the positive electrode, 1.5kV at the negative electrode, the polar distance is 13cm, and the advancing speed is 1.0 mL/h. And after spinning is finished, taking the nanofiber membrane off the aluminum foil, and drying the nanofiber membrane in a vacuum drying oven for 1.5 hours at the temperature of 70 ℃ to remove residual solvent so as to ensure the safety of the used material. Thus, the nanofiber for baicalin extraction can be obtained.

II, extraction:

(1) removing impurities from Scutellariae radix, pulverizing to 40-60 mesh, and weighing 10g Scutellariae radix powder.

(2) According to the mass of the radix scutellariae powder and 75% ethanol, the ratio of material to liquid is 1: mixing at 25 deg.C, extracting under reflux at 80 deg.C for 3 times, and refluxing for 4 hr each time.

(3) And (3) filtering: mixing extractive solutions, standing to room temperature, filtering with medical gauze, collecting filtrate, centrifuging, and collecting supernatant.

(4) Acid adjustment: slowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH to 3, and adding Na₂SO₄The solution was adjusted to an ionic strength of 2%.

(5) Adsorption and enrichment of baicalin: the filtrate is passed through an extraction column containing nanofibers, or by suction under pressure or vacuum.

(6) And (3) elution: eluting with 30% ethanol as eluent, and collecting eluate. The desorption rate was calculated to be 85.1%.

(7) Concentrating and drying: placing the collected eluate in an evaporation vessel, distilling under reduced pressure or rotary evaporation concentrating, stopping concentrating after ethanol is evaporated, and vacuum drying to obtain baicalin.

Example 3

A method for extracting baicalin based on nanometer materials comprises the following steps:

firstly, preparing a nanofiber membrane:

3.55gPS and 1.78g of PVP (7.5% PVP + 15% PS) were added to a mixed solution of THF and DMF (both in a volume of 10 mL: 10mL) to prepare a 15 wt% PS and 7.5 wt% PVP spinning solution, and after stirring uniformly for 12 hours, the spinning solution was charged into a glass syringe (diameter about 2cm) to carry out electrospinning. The spinning voltage is 12kV at the anode, 2kV at the cathode, the polar distance is 20cm, and the advancing speed is 1.5 mL/h. And after spinning is finished, taking the nanofiber membrane off the aluminum foil, and drying the nanofiber membrane in a vacuum drying oven for 1.5 hours at the temperature of 70 ℃ to remove residual solvent so as to ensure the safety of the used material. Thus, the nanometer fiber for extracting baicalin can be obtained

II, extraction:

(1) removing impurities from Scutellariae radix, pulverizing to 40 mesh, and weighing 10g Scutellariae radix powder.

(2) According to the mass of the radix scutellariae powder and a 75% ethanol solution, the ratio of material to liquid is 1: 10 mixing, and extracting under reflux at 80 deg.C for 3 times, each time under reflux for 1.5 hr.

(3) And (3) filtering: mixing extractive solutions, standing to room temperature, filtering with medical gauze, collecting filtrate, centrifuging, and collecting supernatant.

(4) Acid adjustment: slowly adding dilute hydrochloric acid solution into the extractive solution, adjusting pH to 2, and adding Na₂SO₄The solution was adjusted to an ionic strength of 2%.

(5) Adsorption and enrichment of baicalin: adsorbing for 4 hr by static adsorption method, and adsorbing baicalin component in the filtrate onto the nanofiber. It can be seen from FIG. 2 that the adsorption rate of the nanofibers is significantly higher than that of the macroporous resins HPD-100 and AB-8. This is not only due to the advantages of large specific surface area and large adsorption capacity of nanofibers, but also the similar polarity of the fibers and the target.

(6) And (3) elution: eluting with 50% ethanol as eluent, and collecting eluate. The calculated desorption rate was 92.5%, which is significantly higher than that of the macroporous resins HPD-100 and AB-8 (FIG. 3). The nano-fiber adsorbent has strong regeneration capacity and is beneficial to repeated use.

(7) Concentrating and drying: and placing the collected eluent into an evaporation vessel, carrying out reduced pressure distillation or rotary evaporation concentration, stopping concentration after the ethanol is evaporated, and drying under reduced pressure to obtain the baicalin.

The above embodiments are merely illustrative of the features and contents of the present invention, and the scope of the present invention is not limited thereto, and the contents of the claims of the present invention are subject to the claims. Any modification or variation made in accordance with the spirit of the present invention falls within the scope of the present invention.