阅读说明：本技术 一种从植物中分离纯化红枣多糖的方法 (Method for separating and purifying red date polysaccharide from plants ) 是由 郑宋友 王平 何宇琴 王顺余 何建新 于 2019-08-05 设计创作，主要内容包括：本发明提供一种从植物中分离纯化红枣多糖的方法,在含有红枣多糖的原料以1:1~1:30的料液比加入水或乙醇溶液,充分混合均匀,在微波功率为100~800W下进行微波提取1-30min得到红枣多糖粗提物；在萃取温度为30~80℃、萃取压力为16~30MPa、萃取时间为0.5~3h、CO<Sub>2</Sub>流速为5~8L/min的条件下、使用超临界二氧化碳萃取技术对得到红枣多糖粗提物进行萃取得到红枣多糖萃取液,在红枣多糖萃取液中加入体积分数为60-99%的乙醇溶液,离心得沉淀后干燥,得到红枣多糖。(The invention provides a method for separating and purifying red date polysaccharide from plants, which comprises the steps of adding water or ethanol solution into a raw material containing red date polysaccharide according to the material-liquid ratio of 1: 1-1: 30, fully and uniformly mixing, and performing microwave extraction for 1-30min under the microwave power of 100-800W to obtain a red date polysaccharide crude extract; extracting at 30-80 deg.C under 16-30 MPa for 0.5-3 hr with CO 2 Extracting the obtained red date polysaccharide crude extract by using a supercritical carbon dioxide extraction technology under the condition that the flow rate is 5-8L/min to obtain red date polysaccharide extract, adding an ethanol solution with the volume fraction of 60-99% into the red date polysaccharide extract, centrifuging to obtain a precipitate, and drying to obtain the red date polysaccharide.)

1. A method for separating and purifying red date polysaccharide from plants is characterized by comprising the following specific steps:

adding water or ethanol solution into a raw material containing red date polysaccharide according to a material-to-liquid ratio of 1: 1-1: 30, fully and uniformly mixing, and performing microwave extraction for 1-30min under the microwave power of 100-800W to obtain a red date polysaccharide crude extract; extracting at 30-80 deg.C under 16-30 MPa for 0.5-3 hr with CO₂Extracting the obtained red date polysaccharide crude extract by using a supercritical carbon dioxide extraction technology under the condition that the flow rate is 5-8L/min to obtain red date polysaccharide extract, adding an ethanol solution with the volume fraction of 60-99% into the red date polysaccharide extract, centrifuging to obtain a precipitate, and drying to obtain the red date polysaccharide.

2. The method according to claim 1, wherein the ratio of the feed to the liquid in the microwave extraction is 1:5 to 1: 20.

3. The method of claim 1, wherein the microwave extraction uses an ethanol solution having a volume fraction of no greater than 30 percent.

4. The method of claim 1, wherein the conditions of microwave extraction are: the microwave power is 400-600W, and the microwave extraction time is 2-8 min.

5. The method of claim 1, wherein the supercritical carbon dioxide extraction is performed at an extraction temperature of 50-70 ℃, an extraction pressure of 20-25 MPa, an extraction time of 0.5-2 h, and a CO2 flow rate of 6-7L/min.

6. The method as claimed in claim 1, wherein the ethanol solution with a volume fraction of 75-99% is added into the red jujube polysaccharide extract, and the precipitate is obtained by centrifugation.

7. The method of claim 1, wherein the raw material is red date.

Technical Field

The invention relates to a method for separating and purifying natural products, in particular to a method for quickly separating and purifying red date polysaccharide from plants.

Background

Red jujube polysaccharide (Red jujube polysaccharide) is one of the main chemical active components of the fruits of jujube trees belonging to the genus Ziziphus of the family Rhamnaceae, and is a natural macromolecular compound formed by condensation of a plurality of single molecules. According to the report of the literature, the red jujube polysaccharide can regulate the immune system in a multi-layer and multi-way manner, has obvious anticomplementary activity and the function of promoting the proliferation of lymphocytes, and can obviously slow down the aging. The fructus Jujubae polysaccharide also has antiviral, blood lipid reducing, blood glucose reducing, and free radical scavenging effects.

The red date polysaccharide can be mainly extracted from red dates, the extraction time can be shortened by the ultrasonic cavitation effect, and an optimal optimization process for extracting the red date polysaccharide is not available. At present, the method for separating and purifying red date polysaccharide from red dates mainly comprises the following steps: firstly, mixing petroleum ether and red date powder, carrying out reflux treatment by using a Soxhlet extractor to obtain degreased red date powder, then carrying out ultrasonic extraction and concentration to obtain a crude polysaccharide test solution, then carrying out repeated impurity removal on the crude polysaccharide by using an auxiliary enzyme method to obtain a deproteinized solution, then carrying out alcohol extraction, filtering and freeze drying to obtain crude polysaccharide, and carrying out HSCCC, HPLC and other chromatographic methods to separate to obtain the red date polysaccharide. In the production process, the extraction process is very important, because the stability of the polysaccharide is poor, the degradation of the effective components can be accelerated in a high-temperature or long-time solution state, the extraction time of the enzymolysis method is longer, and the price of the active enzyme with higher purity is higher, so the production cost is improved.

Patent CN103335971B discloses a method for extracting red date polysaccharide by ultrasonic technology after alkali liquor extraction, red dates are cleaned, dried, peeled and denucleated, crushed and ground into powder, and the dry weight is weighed; degreasing the treated red date powder with petroleum ether, and air-drying; then, carrying out alkali liquor extraction and dilution on the red dates, and centrifuging to obtain supernatant; performing coarse filtration on the supernatant to obtain a red date polysaccharide crude extraction liquid, performing ultrasonic extraction on the red date polysaccharide crude extraction liquid, putting the red date crude extraction liquid in a 250mL volumetric flask, and extracting for a certain time in water tanks at different temperatures; taking 1mL of red date crude extract diluent, adding 1mL of 6% phenol solution and 2mL of concentrated sulfuric acid, shaking up, cooling, and measuring absorbance A at 490nm wavelength. The polysaccharide in the red dates is mostly acidic, and the dissolution yield of the components can be improved by extracting with alkaline solution according to the chemical properties of the polysaccharides. However, the alkali liquor extraction has destructive effect on the polysaccharide structure, so other methods are used for extraction.

According to the invention, supercritical fluid-microwave assisted extraction is utilized, so that different impurities in the red date polysaccharide extract can be rapidly removed, purer red date polysaccharide can be obtained through purification, experimental operation is reduced, and experimental progress is accelerated, thereby reducing the loss of effective components and maintaining higher yield. Therefore, the technology is a rapid, efficient and environment-friendly method for extracting and purifying the red date polysaccharide.

Disclosure of Invention

The invention provides a method for separating and purifying red date polysaccharide from plants, the red date polysaccharide prepared by the method can rapidly improve the purity of the red date polysaccharide, maintain the stability of the red date polysaccharide and increase the yield, and the process is simple, convenient, feasible, green and environment-friendly, is suitable for industrial mass production and lays a foundation for development and application of related preparations of the red date polysaccharide.

A method for separating and purifying red date polysaccharide from plants comprises the following specific steps:

adding water or ethanol solution into a raw material containing red date polysaccharide according to a material-to-liquid ratio of 1: 1-1: 30, fully and uniformly mixing, and performing microwave extraction for 1-30min under the microwave power of 100-800W to obtain a red date polysaccharide crude extract; extracting at 30-80 deg.C under 16-30 MPa for 0.5-3 hr with CO₂Extracting the obtained red date polysaccharide crude extract by using a supercritical carbon dioxide extraction technology under the condition that the flow rate is 5-8L/min to obtain red date polysaccharide extract, adding an ethanol solution with the volume fraction of 60-99% into the red date polysaccharide extract, centrifuging to obtain a precipitate, and drying to obtain the red date polysaccharide.

In some embodiments of the present invention, the ratio of the material to the liquid in the microwave extraction is 1:5 to 1: 20.

In some embodiments of the invention, the microwave extraction uses an ethanol solution having a volume fraction of no greater than 30 percent.

In some embodiments of the invention, the conditions of the microwave extraction are: the microwave power is 400-600W, and the microwave extraction time is 2-8 min.

In some embodiments of the present invention, the supercritical carbon dioxide extraction temperature is 50-70 ℃, the extraction pressure is 20-25 MPa, the extraction time is 0.5-2 h, and the CO2 flow rate is 6-7L/min.

In some embodiments of the invention, an ethanol solution with a volume fraction of 75-99% is added into the red date polysaccharide extract, and the mixture is centrifuged to obtain a precipitate.

In some embodiments of the invention, the raw material is red date.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, the red date polysaccharide is subjected to microwave-assisted extraction, so that the extraction time is greatly saved, the extraction temperature is reduced, the gelatinization and degradation of the red date polysaccharide are reduced, and the yield of the red date polysaccharide is favorably improved;

2. the method for extracting and purifying the red date polysaccharide by using the supercritical fluid improves the purity of the red date polysaccharide, is favorable for reducing process operation and accelerating the purification speed, thereby reducing the loss of the red date polysaccharide, has higher activity rate, is green and environment-friendly, and is favorable for industrial production.

3. The preparation process capable of accelerating the separation and purification speed of the red date polysaccharide is established, the extraction and purification time can be saved, the speed is accelerated, the stability of the red date polysaccharide is ensured, the yield is increased, the process is simple, convenient and feasible, green and environment-friendly, and a foundation is laid for development and application and industrial development of related preparations of the red date polysaccharide.

Detailed Description

The invention will now be further described with reference to specific examples, without limiting the scope of the invention thereto.