阅读说明：本技术 一种超声水浴加热提取天麻素的方法 (Method for extracting gastrodin by ultrasonic water bath heating ) 是由 曾瞬钦 伍贤进 蒋忠权 陈三春 尹庆铁 田玉桥 曾申磊 于 2019-11-25 设计创作，主要内容包括：本发明公开了一种超声水浴加热提取天麻素的方法,包括：将干燥的天麻粉碎,称取该天麻粉置于反应瓶管中,再加入提取溶剂浸泡,得到浸泡液；将得到的浸泡液注入超声水浴加热装置内进行提取,得到提取液；将得到的提取液经抽滤、离心,取上清液,采用微孔滤膜过滤,收集滤液得到天麻素粗提液；将得到的天麻素粗提液上样至大孔树脂色谱柱,采用乙醇-乙酸乙酯混合溶剂洗脱得到洗脱液,再将洗脱液经旋转蒸发、浓缩、干燥得到天麻素提取物；该方法具有提取时间短、溶剂绿色环保、选择性好、回收率高、溶剂消耗少、良好的环保性以及可自动控制制样条件的特点,且对提高天麻素提取效率和提高提取物质的质量有积极的作用,操作简单,设备易得。(The invention discloses a method for extracting gastrodin by ultrasonic water bath heating, which comprises the following steps: crushing dried gastrodia elata, weighing the gastrodia elata powder, placing the gastrodia elata powder into a reaction bottle tube, and adding an extraction solvent for soaking to obtain a soak solution; injecting the obtained soaking solution into an ultrasonic water bath heating device for extraction to obtain an extracting solution; filtering the obtained extract, centrifuging, collecting supernatant, filtering with microporous membrane, and collecting filtrate to obtain crude gastrodin extract; loading the obtained crude gastrodin extract to a macroporous resin chromatographic column, eluting by using an ethanol-ethyl acetate mixed solvent to obtain an eluent, and performing rotary evaporation, concentration and drying on the eluent to obtain a gastrodin extract; the method has the characteristics of short extraction time, green and environment-friendly solvent, good selectivity, high recovery rate, low solvent consumption, good environmental protection property and capability of automatically controlling sample preparation conditions, has positive effects of improving gastrodin extraction efficiency and improving quality of extracted substances, and is simple to operate and easy to obtain equipment.)

1. A method for extracting gastrodin by ultrasonic water bath heating is characterized by comprising the following steps:

step 1: pulverizing dried rhizoma Gastrodiae, sieving with 40-120 mesh sieve, weighing the rhizoma Gastrodiae powder, placing in a reaction vial, adding extraction solvent, and soaking for 6-12h to obtain soaking solution;

step 2: injecting the soak solution obtained in the step 1 into an ultrasonic water bath heating device for extraction for 2-4 times for 30-120 min/time to obtain an extracting solution;

and step 3: carrying out suction filtration and centrifugation on the extracting solution obtained in the step 2, taking supernatant, filtering by adopting a microporous filter membrane, and collecting filtrate to obtain crude gastrodin extracting solution;

and 4, step 4: and (3) loading the crude gastrodin extract obtained in the step (3) to a macroporous resin chromatographic column, eluting by using an ethanol-ethyl acetate mixed solvent to obtain an eluent, and performing rotary evaporation, concentration and drying on the eluent to obtain a gastrodin extract.

2. The method for extracting gastrodin by heating in ultrasonic water bath according to claim 1, wherein the extraction solvent in the step 1 is 30-90% ethanol solution by volume.

3. The method for extracting gastrodin by heating in ultrasonic water bath according to claim 1, wherein the extraction solvent in step 1 is 70% ethanol solution by volume.

4. The method for extracting gastrodin through ultrasonic water bath heating according to claim 1, wherein the solid-liquid mass ratio of the gastrodia elata powder to the extraction solvent in the step 1 is 1: 5-15.

5. The method for extracting gastrodin through ultrasonic water bath heating according to claim 1, wherein the solid-liquid mass ratio of the gastrodia elata powder to the extraction solvent in the step 1 is 1: 8.

6. the method for extracting gastrodin by ultrasonic water bath heating according to claim 1, characterized in that the extracting solution is added in the step 1 and soaked for 12 h; the extraction times in the step 2 are 3 times, and the time is 90 min/time.

7. The method for extracting gastrodin by ultrasonic water bath heating according to claim 1, wherein the frequency of the ultrasonic water bath heating device in the step 2 is set to 10-90kHz, and the temperature is set to 50-80 ℃.

8. The method for extracting gastrodin by ultrasonic water bath heating according to claim 1, wherein the frequency of the ultrasonic water bath heating device in the step 2 is set to be 30kHz, and the temperature is set to be 60 ℃.

9. The method for extracting gastrodin by ultrasonic water bath heating according to claim 1, wherein the pore size of the microporous filter membrane in the step 3 is 0.45 μm.

10. The method for extracting gastrodin by ultrasonic water bath heating according to claim 1, wherein the macroporous resin is macroporous resin HPD 500; the ethanol-ethyl acetate mixed solvent is ethanol: ethyl acetate 4: 1.

Technical Field

The invention relates to the technical field of pharmaceutical chemicals, in particular to a method for extracting gastrodin by ultrasonic water bath heating.

Background

The rhizoma Gastrodiae is dried tuber of plant of rhizoma Gastrodiae of Gastrodia of Orchidaceae, and is listed as one of four Chinese medicinal materials (Cordyceps, Ginseng radix, and cornu Cervi Pantotrichum), and has effects of calming endogenous wind, relieving spasm, suppressing liver yang, dispelling pathogenic wind, and dredging collaterals. Gastrodine is the main active component in rhizoma Gastrodiae, is a glycoside compound, and has analgesic, antiinflammatory, antiaging, learning improving, and anticonvulsive effects.

The gastrodia elata belongs to a famous and precious medicinal material, the extraction degree of effective components in the gastrodia elata is investigated and influenced by taking the content of gastrodin as an index, and therefore, the improvement of the gastrodin extraction amount has important significance for utilization of the gastrodia elata medicinal material. The gastrodin is a small molecular phenol glycoside with strong polarity, and can be obtained by decocting with water. The method for extracting the effective components in the gastrodia elata mainly adopts a solvent extraction method, and comprises the following steps: extracting with warm water, and refluxing with ethanol. Other new methods comprise a microwave-assisted extraction method, a continuous high-pressure cold leaching method and the like; the traditional reflux extraction method proposed in the research of the extraction process of the effective components of the gastrodia elata can obtain a dredging extraction route, but has the problems of overlong extraction time and low extraction yield. The technological research of extracting gastrodin from gastrodia elata by enzyme method, such as the Baiaiarmy et al, the extraction temperature is sensitive and the extraction time is long although the extraction rate is improved by the proposed enzyme method extraction scheme. The microwave extraction process research of gastrodin in gastrodia elata has short extraction time, but methanol is used as a solvent, so that the solvent has high toxicity, the volatilization condition in the extraction process is high, the solvent loss is serious, and the environment pollution caused by extraction waste liquid is avoided.

Therefore, the traditional gastrodin extraction method has the advantages of long extraction period, high consumption of extraction solvent, more energy consumption and poor extraction efficiency, wherein the traditional thermal extraction method has long heating time and more energy consumption; the soaking extraction method has long extraction period, poor extraction efficiency and large consumption of extraction solvent.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to provide the method for extracting gastrodin by ultrasonic water bath heating, which has the characteristics of short extraction time, green and environment-friendly solvent, good selectivity, high recovery rate, low solvent consumption, good environmental protection property, capability of automatically controlling sample preparation conditions, positive effects of improving gastrodin extraction efficiency and improving quality of extracted substances, simple operation and easy equipment acquisition.

In order to realize the purpose, the invention adopts the technical scheme that:

a method for extracting gastrodin by ultrasonic water bath heating comprises the following steps:

step 1: pulverizing dried rhizoma Gastrodiae, sieving with 40-120 mesh sieve, weighing the rhizoma Gastrodiae powder, placing in a reaction vial, adding extraction solvent, and soaking for 6-12h to obtain soaking solution;

step 2: injecting the soak solution obtained in the step 1 into an ultrasonic water bath heating device for extraction for 2-4 times for 30-120 min/time to obtain an extracting solution;

and step 3: carrying out suction filtration and centrifugation on the extracting solution obtained in the step 2, taking supernatant, filtering by adopting a microporous filter membrane, and collecting filtrate to obtain crude gastrodin extracting solution;

and 4, step 4: and (3) loading the crude gastrodin extract obtained in the step (3) to a macroporous resin chromatographic column, eluting by using an ethanol-ethyl acetate mixed solvent to obtain an eluent, and performing rotary evaporation, concentration and drying on the eluent to obtain a gastrodin extract.

Further, the gastrodia elata is crushed and sieved by a sieve of 80-200 meshes in the step 1.

Further, the extraction solvent in the step 1 is 30-90% of ethanol solution by volume.

Preferably, the extraction solvent in step 1 is 70% ethanol solution by volume.

Further, in the step 1, the solid-liquid mass ratio of the gastrodia elata powder to the extraction solvent is 1: 5-15.

Preferably, in the step 1, the solid-liquid mass ratio of the gastrodia elata powder to the extraction solvent is 1: 8.

preferably, the extracting solution is added in the step 1 for soaking for 12 hours; the extraction times in the step 2 are 3 times, and the time is 90 min/time.

Further, the frequency of the ultrasonic water bath heating device in the step 2 is set to be 10-90kHz, and the temperature is set to be 50-80 ℃.

Preferably, the frequency of the ultrasonic water bath heating device in the step 2 is set to be 30kHz, and the temperature is set to be 60 ℃.

Preferably, the pore size of the microporous filter membrane in the step 3 is 0.45 μm.

Preferably, the macroporous resin is macroporous resin HPD 500; the ethanol-ethyl acetate mixed solvent is ethanol: ethyl acetate 4: 1.

The invention has the beneficial effects that: (1) compared with the traditional soaking extraction method, the method can quickly dissolve the gastrodin serving as the effective component of the gastrodia elata into the solvent, has the characteristics of short extraction time, green and environment-friendly solvent, good selectivity, high recovery rate, low solvent consumption, good environmental friendliness and capability of automatically controlling sample preparation conditions, has positive effects of improving the gastrodin extraction efficiency and improving the quality of extracted substances, is simple to operate, is easy to obtain equipment, has high extraction efficiency, and can be widely applied to industrial production;

(2) the ultrasonic extraction technology adopted by the invention is used for extracting gastrodin which is an effective component of gastrodia elata, the principle is that the multi-stage effects of strong vibration, strong cavitation diffusion, smashing and the like generated by ultrasonic waves are utilized, the molecular motion frequency and speed of a substance are increased, instantaneous cavitation can generate instantaneous pressure up to thousands of atmospheric pressures, the penetrating power of a solution is increased, the ultrasonic waves also have other effects of crushing, stirring and the like, cells in the gastrodia elata are broken, the effective component is accelerated to enter the solvent, mutual permeation is accelerated, and dissolution is carried out, so that the leaching rate of the gastrodin is improved, and the extraction time is shortened;

(3) the ultrasonic water bath heating method adopted by the invention is a new technology for improving the extraction efficiency by utilizing the ultrasonic frequency, can effectively improve the yield of the extract, plays a role in environmental protection, and can greatly promote the development of the gastrodia elata in the aspects of medicines and the like.

Detailed Description

For a better understanding of the present invention, embodiments of the present invention are described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.