Preparation method and application of kinsenoside molecularly imprinted membrane component

Abstract

The invention discloses a preparation method and application of a kinsenoside molecularly imprinted membrane component, the prepared kinsenoside molecularly imprinted membrane component can perform high-purity extraction on a single molecule of a kinsenoside monomer, and the problems of complex flow, low purity and high input cost of an existing kinsenoside extraction process are solved.

Description

Technical Field

[0001] The invention relates to the technical field of functional materials, and in particular to a preparation method and application of a roxburghii glycoside molecular imprinting membrane component. Background Art

[0002] Anoectochilus roxburghii (Wall.) Lindl, a plant of the genus Anoectochilus of the orchid family, is fresh or dried, and has the effects of clearing away heat and detoxifying, dispelling wind and removing dampness. Studies in recent years have shown that anoectochilus glycoside is one of the main active ingredients of Anoectochilus roxburghii, and its content is about 10% of the dry weight of Anoectochilus roxburghii medicinal materials. It has pharmacological effects such as protecting the liver, anti-inflammatory, lowering blood sugar, and resisting osteoporosis. Some patent documents also report methods for preparing anoectochilus glycoside from Anoectochilus roxburghii. For example, the Chinese invention patent application with application number 200810236824.3 discloses anoectochilus glycoside and its derivatives, as well as preparation methods and uses. The main steps are: extracting Anoectochilus roxburghii with methanol or ethanol under reflux, recovering ethanol from the extract, suspending in water, and extracting with petroleum ether, ethyl acetate, and n-butanol in sequence. The n-butanol extraction part is separated by silica gel column chromatography and eluted with chloroform-methanol gradient, and the eluate is separated by Sephadex LH-20 to obtain anoectoglucoside; for example, the Chinese invention patent with application number 202111160733.8 discloses a method for extracting anoectoglucoside based on a deep eutectic solvent, wherein the anoectoglucoside powder is added to a deep eutectic solvent-water solution and then ultrasonically extracted, the extract is vacuum concentrated and loaded on a silica gel column, eluted with ethyl acetate / ethanol / acetic acid eluent and the eluent is collected in segments, and the eluent with a anoectoglucoside content greater than 80% is detected by HPLC-ELSD, and then the eluent is combined and vacuum freeze-dried to obtain anoectoglucoside.

[0003] The organic solvent used in the above-mentioned preparation method includes methanol, petroleum ether, ethyl acetate, chloroform, and n-butanol. These reagents are highly toxic, costly, and easily cause environmental pollution, and the product is prone to residual organic solvents, thereby affecting the safety of the product. In addition, the silica gel column chromatography and Sephadex LH-20 separation and purification steps used in the above-mentioned preparation method are cumbersome and time-consuming to operate. The above method is difficult to be used for industrial production. Therefore, there is an urgent need for a simple, efficient, low-cost, and safe extraction and separation technology to solve the problems existing in the prior art. Summary of the invention

[0004] The purpose of the present invention is to provide a preparation method and application of a roxburghii glycoside molecular imprinting membrane component. The prepared roxburghii glycoside molecular imprinting membrane component can perform high-purity extraction on a single molecule of a roxburghii glycoside monomer, thereby solving the problems of complex process, low purity and high investment cost in the current extraction process of roxburghii glycoside.

[0005] In order to achieve the above object, the solution of the present invention is:

[0006] A method for preparing a roxburghii glycoside molecular imprinting membrane assembly comprises the following steps:

[0007] Step 1, firstly, according to the following mass percentages, 0.1% to 3% of roxburghii glycoside, 3% to 6% of functional monomer, 50% to 60% of solvent, 30% to 40% of cross-linking agent and 1% to 3% of initiator are mixed, reacted at 50 to 60° C. for 3 to 24 hours, and then cooled to 30 to 45° C. to obtain a roxburghii glycoside composite solution;

[0008] Step 2, then dissolving 20% ​​to 30% of the polymer base film in 70% to 80% of the solvent to form a film-making solution;

[0009] Step 3, then pouring the obtained anoectin composite solution into the membrane-making solution, stirring to obtain the anoectin molecular imprinting membrane base solution;

[0010] Step 4, then using a tubular membrane manufacturing process to prepare anoectin molecular imprinting membrane tubes from the obtained anoectin molecular imprinting membrane base liquid;

[0011] Step 5: finally assembling the anoectin molecularly imprinted membrane tube into a tubular membrane module housing, using ethanol as an eluent in the membrane device to wash the anoectin template molecules to obtain the anoectin molecularly imprinted membrane module.

[0012] In step 1, the functional monomer is methacrylic acid, acrylamide or methacrylate, the solvent is ethanol, the cross-linking agent is acrylonitrile or ethylene glycol dimethacrylate, and the initiator is azobisisobutyronitrile.

[0013] In step 2, the polymer base film is a polystyrene polymer film, a polyvinylidene chloride polymer film or a polyethersulfone polymer film.

[0014] In step 2, the solvent is dimethylacetamide or dimethylformamide.

[0015] In step 3, the volume ratio of the roxburghii glycoside composite solution to the film-making solution is 1-2:8-9.

[0016] An application of a roxburghii glycoside molecular imprinting membrane component is to apply the roxburghii glycoside molecular imprinting membrane component to the extraction of roxburghii glycoside.

[0017] After adopting the above technical scheme, the preparation method and application of the anoectodexin molecular imprinting membrane component of the present invention are simple in preparation method and low in cost, and the anoectodexin molecular imprinting membrane component with high selectivity and specificity is obtained, and a single molecule of the anoectodexin monomer can be extracted with high purity, thereby solving the problems of complex process, low purity and high investment cost in the current extraction process of anoectodexin. DETAILED DESCRIPTION

[0018] In order to further explain the technical solution of the present invention, the present invention is described in detail below through specific embodiments.

[0019] Example 1

[0020] A method for preparing a roxburghii glycoside molecular imprinting membrane assembly comprises the following steps:

[0021] Step 1, firstly, according to the following mass percentages, 1% roxburghii glycoside, 3% methacrylic acid, 60% ethanol, 33% acrylonitrile and 3% azobisisobutyronitrile were mixed in a reaction kettle, reacted at 50° C. for 8 hours, and then cooled to 30° C. to obtain a roxburghii glycoside composite solution;

[0022] Step 2, then dissolving 20% ​​polystyrene polymer film in 80% dimethylacetamide to form a film-making solution;

[0023] Step 3, then pouring the obtained anoectin complex solution into the membrane-making solution at a volume ratio of 1:9, and stirring to obtain anoectin molecular imprinting membrane base solution;

[0024] Step 4, then using a non-woven fabric with a width of 10 to 20 mm, rolling it into a tube by a tube rolling machine, and then welding it into a tubular structure by an ultrasonic welding machine, and simultaneously coating the base film with the aureofaena glycoside molecular imprinting membrane base liquid, and then passing through a gel bath tank for curing, and cutting it into a required length to make aureofaena glycoside molecular imprinting membrane tube;

[0025] Step 5, then inject the Anoectochilus stem molecular imprinting membrane tube glue into the outer shell of the tubular membrane assembly to form a membrane assembly, and then assemble the membrane assembly into a complete membrane device equipped with a booster pump, an electronic control, a bracket, and a medicine box, and then use ethanol as an eluent, and use the booster pump to pump ethanol into the membrane device to soak and circulate, elute the Anoectochilus glycoside template molecules, and take out the membrane assembly, thereby obtaining the Anoectochilus glycoside molecular imprinting membrane assembly.

[0026] Example 2

[0027] A method for preparing a roxburghii glycoside molecular imprinting membrane assembly comprises the following steps:

[0028] Step 1, firstly, according to the following mass percentages, 3% roxburghii glycoside, 6% acrylamide, 50% ethanol, 40% ethylene glycol dimethacrylate and 1% azobisisobutyronitrile were mixed in a reaction kettle, reacted at 60° C. for 24 hours, and then cooled to 45° C. to obtain a roxburghii glycoside composite solution;

[0029] Step 2, then dissolving 30% of the polyethersulfone polymer membrane in 70% of dimethylformamide to form a membrane-making solution;

[0030] Step 3, then pouring the obtained anoectin composite solution into the membrane-making solution at a volume ratio of 2:8, and stirring to obtain the anoectin molecular imprinting membrane base solution;

[0031] Step 4, using a non-woven fabric with a width of 10 to 20 mm, rolling it into a tube by a tube rolling machine, and then welding it into a tubular structure by an ultrasonic welding machine, and simultaneously coating the base film with the anoectin molecular imprinting membrane base liquid, and then passing it through a gel bath tank for curing, and cutting it into a required length to make a anoectin molecular imprinting membrane tube;

[0032] Step 5, then inject the Anoectochilus stem molecular imprinting membrane tube glue into the outer shell of the tubular membrane assembly to form a membrane assembly, and then assemble the membrane assembly into a complete membrane device equipped with a booster pump, an electronic control, a bracket, and a medicine box, and then use ethanol as an eluent, and use the booster pump to pump ethanol into the membrane device to soak and circulate, elute the Anoectochilus glycoside template molecules, and take out the membrane assembly, thereby obtaining the Anoectochilus glycoside molecular imprinting membrane assembly.

[0033] The tubular membrane manufacturing process and the process of assembling the tubular membrane into a membrane device involved in the present invention are both well-known technologies in the art.

[0034] Application Examples

[0035] First, the roxburghii powder is mixed with an ethanol solvent and heated to obtain a roxburghii solution. The obtained roxburghii solution is then separated and purified by a membrane system device assembled with a roxburghii glycoside molecular imprinting membrane components to obtain a roxburghii glycoside extract. Finally, the roxburghii glycoside is sprayed and dried to obtain high-purity roxburghii glycoside powder.

[0036] The above embodiments do not limit the product form and style of the present invention. Any appropriate changes or modifications made by ordinary technicians in the relevant technical field should be deemed to be within the patent scope of the present invention.

Claims

1. A method for preparing a roxburghii glycoside molecular imprinted membrane assembly, characterized in that: The following steps are involved: Step 1, firstly, according to the following mass percentages, 0.1% to 3% of roxburghii glycoside, 3% to 6% of functional monomer, 50% to 60% of solvent, 30% to 40% of cross-linking agent and 1% to 3% of initiator are mixed, reacted at 50 to 60° C. for 3 to 24 hours, and then cooled to 30 to 45° C. to obtain a roxburghii glycoside composite solution; Step 2, then dissolving 20% ​​to 30% of the polymer base film in 70% to 80% of the solvent to form a film-making solution; Step 3, then pouring the obtained anoectin composite solution into the membrane-making solution, stirring to obtain the anoectin molecular imprinting membrane base solution; Step 4, then using a tubular membrane manufacturing process to prepare anoectin molecular imprinting membrane tubes from the obtained anoectin molecular imprinting membrane base liquid; Step 5: finally assembling the anoectin molecularly imprinted membrane tube into a tubular membrane module housing, using ethanol as an eluent in the membrane device to wash the anoectin template molecules to obtain the anoectin molecularly imprinted membrane module.

2. The method for preparing a roxburghii glycoside molecular imprinted membrane assembly according to claim 1, characterized in that: In step 1, the functional monomer is methacrylic acid, acrylamide or methacrylate, the solvent is ethanol, the cross-linking agent is acrylonitrile or ethylene glycol dimethacrylate, and the initiator is azobisisobutyronitrile.

3. The method for preparing a roxburghii glycoside molecular imprinted membrane assembly according to claim 1, characterized in that: In step 2, the polymer base film is a polystyrene polymer film, a polyvinylidene chloride polymer film or a polyethersulfone polymer film.

4. The method for preparing a roxburghii glycoside molecular imprinted membrane assembly according to claim 1, characterized in that: In step 2, the solvent is dimethylacetamide or dimethylformamide.

5. The method for preparing a roxburghii glycoside molecular imprinted membrane assembly according to claim 1, characterized in that: In step 3, the volume ratio of the roxburghii glycoside composite solution to the film-making solution is 1-2:8-9.

6. An application of a roxburghii glycoside molecular imprinting membrane assembly, characterized in that: The method is to apply the anoectoside molecular imprinting membrane component as claimed in claim 1 to the extraction of anoectoside.