阅读说明：本技术 一种基于罗布麻组合药物成分的提取方法 (Extraction method based on apocynum venetum combined medicine components ) 是由 王玉珍 于 2019-12-13 设计创作，主要内容包括：本发明公开了一种基于罗布麻组合药物成分的提取方法,属于药物提取技术领域,通过使用磨粉设备将罗布麻叶片粉碎,从而可以增大罗布麻叶片内黄酮提取时与辅助材料之间的接触面积,加热回流时可以将罗布麻叶片中的水分取出,留下固态物,乙醚清理可以去除罗布麻叶片中的叶绿素及蜡质,使得罗布麻叶片更加干净,加入沸水溶解可以使得一些无用的物质可以与固态物分离,并且乙醇可以将滤液中的有效成分进行收集,并且当乙醇被提取回收时就可以得到提取出的黄酮类化合物,使得本方法可以高效率的提取罗布麻叶片中含有的有效物质,并且含有的杂质较少,使得黄酮类化合物的有效含量较高。(The invention discloses an extraction method based on apocynum venetum combined medicine components, belonging to the technical field of medicine extraction, wherein, grinding equipment is used for crushing apocynum venetum leaves, thereby increasing the contact area between the flavone in the apocynum venetum leaves and the auxiliary material during extraction, taking out the water in the apocynum venetum leaves during heating and refluxing, leaving solid substances, removing chlorophyll and wax in the apocynum venetum leaves by ether cleaning, so that the apocynum venetum leaves are cleaner, some useless substances can be separated from solid substances by adding boiling water for dissolution, the ethanol can collect the effective components in the filtrate, and the extracted flavonoids can be obtained when the ethanol is extracted and recovered, the method can efficiently extract the effective substances contained in the apocynum venetum leaves, and has less impurities, so that the effective content of flavonoid compounds is higher.)

1. A method for extracting components based on apocynum venetum combined medicine is characterized by comprising the following steps: including the following materials and tools required:

the materials required to be used are: folium Apocyni Veneti, 65% ethanol, water, and diethyl ether;

the tools needed to be used are: heating equipment, grinding equipment, an extraction container, a glass rod and a heating beaker;

the extraction method of the components of the combined medicine comprises the following specific operation steps:

the method comprises the following steps: firstly, cleaning a proper amount of fresh dogbane leaves by workers, drying the dogbane leaves in the shade at normal temperature, then grinding the dogbane leaves into powder by using proper grinding equipment, and filling the powder into a container for later use;

step two: pouring fifty grams of the dogbane leaf powder extracted in the step one into a heating beaker, adding water, heating and refluxing for two times, and decocting into a paste after two hours each time;

step three: cooling the paste decocted in the step two, and then cleaning with ethyl ether in the same proportion;

step four: adding hot water into the paste washed in the third step for dissolving, stirring by using a glass rod, filtering after waiting for 24 hours, and collecting filtrate;

step five: pouring five hundred milliliters of 65 percent ethanol into the extraction container, pouring the filtrate collected in the step four into the extraction container, and eluting for three hours by using the ethanol;

step six: collecting the eluent generated in the step five, and recovering ethanol in the eluent;

step seven: and concentrating the residual substances in the sixth step under reduced pressure, and then drying in vacuum to finally obtain the flavone extract in the dogbane leaves.

2. The extraction method based on apocynum venetum combined medicine components according to claim 1, characterized by comprising the following steps: the hot water temperature in the fourth step needs to be between 60 and 70 degrees.

3. The extraction method based on apocynum venetum combined medicine components according to claim 1, characterized by comprising the following steps: and in the fifth step, the ethanol is eluted until the eluent is colorless, clear and transparent.

4. The extraction method based on apocynum venetum combined medicine components according to claim 1, characterized by comprising the following steps: in the fourth step, the amount of the hot water which needs to be added is three to five times of that of the paste, and the hot water is added into the paste for dissolving by times.

5. The extraction method based on apocynum venetum combined medicine components according to claim 1, characterized by comprising the following steps: and the environment for vacuum drying in the seventh step is 80 ℃.

Technical Field

The invention belongs to the technical field of medicine extraction, and particularly relates to an extraction method based on apocynum venetum combined medicine components.

Background

The dogbane, namely the kenaf, the tea flower, the salix chinensis and the like, is erect half shrub, is 1.5-3 m high, grows in sandy land of river banks, mountain ditches and hillsides, is mainly distributed in northern provinces of China Huaihe, Qinling and Kunlun, dry leaves of the dogbane can be used as a medicine, has the functions of calming the liver, relieving pain, nourishing blood, regulating menstruation and astringing yin to stop sweating, and flavonoids are important active ingredients in the dogbane leaves, has the effects of relieving cough, eliminating phlegm, relieving asthma, resisting bacteria, protecting liver and relieving liver toxicity, and can be used for treating acute and chronic hepatitis and liver cirrhosis.

The dogbane tablet is a compound preparation tablet, and because the dogbane tablet is formed by directly using dry powder of a dogbane leaf decoction, part of components in the dry powder of the dogbane leaf decoction are irrelevant to the treatment effect, so that the dosage is large and low when the dogbane tablet is used as a medicine, the transformation burden of a human body is increased, and the extraction process of active ingredients in some dogbane leaves is also provided, but the general method is often an alcohol extraction → water precipitation → ethyl acetate extraction method.

Disclosure of Invention

Technical problem to be solved

In order to overcome the defects in the prior art, the invention provides an extraction method of medicinal components based on apocynum venetum combination, which solves the problems that as apocynum venetum slices are directly prepared from dry powder of an apocynum venetum leaf decoction, partial components in the dry powder of the apocynum venetum leaf decoction are irrelevant to the treatment effect, the dosage of the medicinal components is high, the human body transformation burden is increased, and some effective components in the apocynum venetum leaves are extracted, but the general method is often an alcohol extraction → water precipitation → ethyl acetate extraction method, so that the flavonoid compound extracted by the method has low yield, contains more impurities and has too low content of the flavonoid compound.

(II) technical scheme

In order to achieve the purpose, the invention provides the following technical scheme: a method for extracting medicinal components based on herba Apocyni Veneti comprises the following materials and tools:

the materials required to be used are: folium Apocyni Veneti, 65% ethanol, water, and diethyl ether;

the tools needed to be used are: heating equipment, grinding equipment, an extraction container, a glass rod and a heating beaker;

the extraction method of the components of the combined medicine comprises the following specific operation steps:

the method comprises the following steps: firstly, cleaning a proper amount of fresh dogbane leaves by workers, drying the dogbane leaves in the shade at normal temperature, then grinding the dogbane leaves into powder by using proper grinding equipment, and filling the powder into a container for later use;

step two: pouring fifty grams of the dogbane leaf powder extracted in the step one into a heating beaker, adding water, heating and refluxing for two times, and decocting into a paste after two hours each time;

step three: cooling the paste decocted in the step two, and then cleaning with ethyl ether in the same proportion;

step four: adding hot water into the paste washed in the third step for dissolving, stirring by using a glass rod, filtering after waiting for 24 hours, and collecting filtrate;

step five: pouring five hundred milliliters of 65 percent ethanol into the extraction container, pouring the filtrate collected in the step four into the extraction container, and eluting for three hours by using the ethanol;

step six: collecting the eluent generated in the step five, and recovering ethanol in the eluent;

step seven: and concentrating the residual substances in the sixth step under reduced pressure, and then drying in vacuum to finally obtain the flavone extract in the dogbane leaves.

As a further scheme of the invention: the hot water temperature in the fourth step needs to be between 60 and 70 degrees.

As a further scheme of the invention: and in the fifth step, the ethanol is eluted until the eluent is colorless, clear and transparent.

As a further scheme of the invention: in the fourth step, the amount of the hot water which needs to be added is three to five times of that of the paste, and the hot water is added into the paste for dissolving by times.

As a further scheme of the invention: and the environment for vacuum drying in the seventh step is 80 ℃.

(III) advantageous effects

According to the extraction method based on the apocynum venetum combined medicinal ingredients, the apocynum venetum leaves are crushed, so that the contact area between the apocynum venetum leaves and auxiliary materials can be increased during extraction of flavone, water in the apocynum venetum leaves can be taken out during heating reflux, solid matters are left, chlorophyll and wax in the apocynum venetum leaves can be removed through ether cleaning, the apocynum venetum leaves are enabled to be cleaner, some useless substances can be separated from the solid matters through dissolving by adding boiling water, the effective ingredients in filtrate can be collected through ethanol, and the extracted flavonoid compounds can be obtained when the ethanol is extracted and recovered, so that the method can efficiently extract the effective substances contained in the apocynum venetum leaves, and has fewer impurities, and the effective content of the flavonoid compounds is high.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a technical scheme that: a method for extracting medicinal components based on herba Apocyni Veneti comprises the following materials and tools:

the materials required to be used are: folium Apocyni Veneti, 65% ethanol, water, and diethyl ether;

the tools needed to be used are: heating equipment, grinding equipment, an extraction container, a glass rod and a heating beaker;

the extraction method of the components of the combined medicine comprises the following specific operation steps:

the method comprises the following steps: firstly, cleaning a proper amount of fresh dogbane leaves by workers, drying the dogbane leaves in the shade at normal temperature, then grinding the dogbane leaves into powder by using proper grinding equipment, and filling the powder into a container for later use;

step two: pouring fifty grams of the dogbane leaf powder extracted in the step one into a heating beaker, adding water, heating and refluxing for two times, and decocting into a paste after two hours each time;

step three: cooling the paste decocted in the step two, and then cleaning with ethyl ether in the same proportion;

step four: adding hot water into the paste washed in the third step for dissolving, stirring by using a glass rod, filtering after waiting for 24 hours, and collecting filtrate;

step five: pouring five hundred milliliters of 65 percent ethanol into the extraction container, pouring the filtrate collected in the step four into the extraction container, and eluting for three hours by using the ethanol;

step six: collecting the eluent generated in the step five, and recovering ethanol in the eluent;

step seven: and concentrating the residual substances in the sixth step under reduced pressure, and then drying in vacuum to finally obtain the flavone extract in the dogbane leaves.

The hot water temperature in the fourth step needs to be between 60 and 70 degrees.

And in the fifth step, the ethanol is eluted until the eluent is colorless, clear and transparent.

In the fourth step, the amount of the hot water which needs to be added is three to five times of that of the paste, and the hot water is added into the paste for dissolving by times.

And the environment for vacuum drying in the seventh step is 80 ℃.

Each organ of apocynum venetum contains flavonoid compounds with different contents, and the total flavonoid contents in each organ are in the sequence of leaves, roots and stems. The content in leaves was 2.5%, roots 1.7%, stems 0.58%. The content of total flavone in the leaves at the highest period (month 9) is 24 times of the content of total flavone in the stems at the highest period (month 8), and the content of total flavone in the apocynum venetum leaves is obviously higher than that in the stems, so that the apocynum venetum leaves are preferably used for extraction in the extraction process.

The effective data and test methods provided herein are 1. Effect of ethanol solvent concentration on flavone extraction yield

When the ethanol extraction concentration is 25%, the total extraction rate of flavone is 1.90%;

when the ethanol extraction concentration is 35%, the total extraction rate of flavone is 2.10%;

when the ethanol extraction concentration is 45%, the total extraction rate of flavone is 2.20%;

when the ethanol extraction concentration is 55%, the total extraction rate of flavone is 2.70%;

when the ethanol extraction concentration is 65%, the total extraction rate of flavone is 2.75%;

when the ethanol extraction concentration is 75%, the total extraction rate of flavone is 2.60%;

when the ethanol extraction concentration is 85%, the total extraction rate of flavone is 2.10%;

when the ethanol extraction concentration is 95%, the total extraction rate of flavone is 1.05%;

it can be seen that the total extraction rate of flavone increases with increasing solvent concentration at 25% -65% solvent concentration. At solvent concentrations greater than 65%, the total extraction rate of flavonoids decreased with increasing solvent concentration. Therefore, the flavone yield is highest when the solvent concentration is 65%, and 2.75% of flavone is extracted.

2. Influence of extraction time on total flavone extraction rate

When the extraction time is 1h, the total extraction rate of flavone is 1.73%;

when the extraction time is 2h, the total extraction rate of flavone is 2.42%;

when the extraction time is 3h, the total extraction rate of flavone is 2.53%;

when the extraction time is 4h, the total extraction rate of flavone is 2.50%;

when the extraction time is 5h, the total extraction rate of flavone is 2.43%;

the final result shows that if the extraction time is between 1h and 3h, the total extraction rate of the flavone is higher and higher when the time is longer and longer; when the extraction time is between 3h and 5h, the total extraction rate of the flavone is reduced along with the increase of the time, because the ethanol volatilizes during the reaction, so that the heating time lasts too long, or the boiling point of the reaction liquid is higher and higher, so that the structure of the flavonoid compound is damaged, and the extraction rate is reduced along with the increase of the time between 3h and 5 h. Therefore, the dogbane leaf flavonoid compound extracted by the ethanol extraction method has ideal extraction effect when the extraction time is controlled to be 3 hours, and 2.53 percent of flavone can be extracted.

3. Influence of extraction temperature on total flavone extraction rate

When the extraction temperature is 50 ℃, the total extraction rate of flavone is 2.01 percent;

when the extraction temperature is 60 ℃, the total extraction rate of flavone is 2.45%;

when the extraction temperature is 70 ℃, the total extraction rate of flavone is 2.51%;

when the extraction temperature is 80 ℃, the total extraction rate of flavone is 2.52%;

when the extraction temperature is 90 ℃, the total extraction rate of flavone is 2.44%;

when the extraction temperature is 100 ℃, the total extraction rate of flavone is 1.93%;

it can be seen that when the temperature is less than 80 ℃, the extraction rate of flavone is higher and higher along with the increasing temperature. Especially, the extraction rate of flavone is increased sharply when the temperature is 50 ℃ and T is less than 60 ℃, and the extraction rate of flavone is increased slowly when the temperature is 60 ℃ and T is less than 80 ℃; when T is greater than 80 deg.C, the total extraction rate of flavone decreases with increasing temperature, at 80 deg.C < T <90 deg.C, the extraction rate of flavone slowly decreases with increasing temperature, and when T is greater than 90 deg.C, the extraction rate of flavone rapidly decreases with increasing temperature. Therefore, the reason that the temperature exceeds a certain limit, which causes volatilization or structural damage of some flavonoid compounds, is suspected, so that the dogbane leaf flavonoid compounds are extracted by an ethanol extraction method, the extraction temperature is controlled at 80 ℃, the optimal extraction effect can be obtained, and 2.52 percent of flavone can be extracted.

4. Influence of extraction frequency on total extraction rate of flavone

The total extraction rate of flavone is 1.91% in the first extraction;

during the second extraction, the total extraction rate of flavone is 2.58%;

in the third extraction, the total extraction rate of flavone is 2.58%;

in the fourth extraction, the total extraction rate of flavone is 2.59%;

the results show that the total extraction rate of flavone increases along with the increase of times after 1-2 times of extraction. However, if the number of times is more than 2, the increase change will be weaker and weaker. Therefore, considering the industrial procedure, the dogbane leaf flavone is basically and completely dissolved out after 2 times of extraction. Therefore, the optimal process condition was finally determined to be 2 extractions.

The hot reflux extraction process of the flavone in the dogbane leaves is optimized, and test results show that the optimized process can obviously improve the extraction amount of the flavone, the concentration of ethanol is a significant factor influencing the extraction of quercetin, the content of the quercetin in the dogbane is 0.2220 mg per gram under the optimal extraction process condition, and the process has the advantages of stability, feasibility and high efficiency;

in conclusion, the optimal concentration of ethanol is 65% during flavone extraction, the optimal extraction time is three hours, the optimal extraction temperature is 80 ℃, and the optimal extraction times are two times.

According to the extraction method based on the apocynum venetum combined medicinal ingredients, the apocynum venetum leaves are crushed, so that the contact area between the apocynum venetum leaves and auxiliary materials can be increased during extraction of flavone, water in the apocynum venetum leaves can be taken out during heating reflux, solid matters are left, chlorophyll and wax in the apocynum venetum leaves can be removed through ether cleaning, the apocynum venetum leaves are enabled to be cleaner, some useless substances can be separated from the solid matters through dissolving by adding boiling water, the effective ingredients in filtrate can be collected through ethanol, and the extracted flavonoid compounds can be obtained when the ethanol is extracted and recovered, so that the method can efficiently extract the effective substances contained in the apocynum venetum leaves, and has fewer impurities, and the effective content of the flavonoid compounds is high.

The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only illustrative of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.