阅读说明：本技术 一种宁夏栽培柴胡地上部分总黄酮的提取工艺 (Process for extracting total flavonoids from aerial parts of radix bupleuri cultivated in Ningxia ) 是由 郝彩琴 冷晓红 李军 陈海燕 郭超 郭鸿雁 徐超 刘立轩 于 2019-11-21 设计创作，主要内容包括：本发明实施例公开了一种宁夏栽培柴胡地上部分总黄酮的提取工艺,具体涉及总黄酮提取工艺领域,包括粉碎、室温浸泡、静态加热回流提取和浓缩等四个步骤,具体如下：粉碎采用将净选好的柴胡地上部分,粉碎过药典2号筛；粉碎后的柴胡地上部分装入提取容器,加55％的乙醇,料液比1:10,室温密闭浸泡60min；静态加热回流提取3次,每次都按料液比1：10提取72min,合并提取滤液；滤液于56℃以下减压浓缩至溶剂全部蒸干,即得干浸膏。本发明采用粉碎、室温浸泡、回流提取、浓缩等工艺,得到柴胡地上部分的总提取的干浸膏,总黄酮提取率达3.7％,该工艺简单易行,便于实现工业化生产。(The embodiment of the invention discloses an extraction process of general flavone of overground parts of radix bupleuri cultivated in Ningxia, and particularly relates to the field of general flavone extraction processes, wherein the extraction process comprises four steps of crushing, room-temperature soaking, static heating reflux extraction, concentration and the like, and specifically comprises the following steps: pulverizing selected aerial part of bupleuri radix, and sieving with pharmacopeia No. 2 sieve; placing pulverized aerial part of bupleuri radix into an extraction container, adding 55% ethanol at a material-liquid ratio of 1:10, and soaking at room temperature under sealed condition for 60 min; carrying out static heating reflux extraction for 3 times, wherein the ratio of material to liquid is 1: extracting for 72min, and mixing extractive filtrates; concentrating the filtrate at 56 deg.C under reduced pressure until the solvent is completely evaporated to dryness to obtain dry extract. The invention adopts the processes of crushing, room temperature soaking, reflux extraction, concentration and the like to obtain the total extracted dry extract of the overground part of the bupleurum, the extraction rate of the total flavone reaches 3.7 percent, and the process is simple and easy to implement and is convenient for realizing industrial production.)

1. A process for extracting total flavonoids from overground parts of Chinese thorowax roots in Ningxia cultivation is characterized by comprising the following steps: comprises four steps of crushing, room temperature soaking, static heating reflux extraction, concentration and the like.

2. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 1, is characterized in that: the extraction process of the bupleurum total flavonoids in the overground part comprises the following steps:

step one, crushing: selecting aerial part of bupleuri radix, naturally drying, pulverizing with small swing pulverizer, and sieving with pharmacopeia No. two sieve to obtain bupleuri radix coarse powder;

step two, soaking at room temperature: placing the above-ground part coarse powder of bupleuri radix into an extraction container, adding 55% ethanol, and soaking for 50-70min at room temperature under sealed condition;

step three, static reflux extraction: soaking in 55% ethanol at room temperature for 55-60 min, and extracting for 3 times by static heating reflux method;

step four, concentration: and combining the filtrates obtained by the 3 times of extraction, and concentrating the filtrate at the temperature of 55-57 ℃ under reduced pressure until all the solvents are evaporated to dryness to obtain a dry extract.

3. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 2, is characterized in that: in the first step, the coarse powder of the overground part of the radix bupleuri crushed by a small swing crusher is screened by a pharmacopeia No. two screen.

4. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 2, is characterized in that: in the second step, the feed-liquid ratio of the coarse powder of the overground part of the radix bupleuri to 55% ethanol is 0.8-1: 9 to 11.

5. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 2, is characterized in that: in the third step, a static heating reflux method is adopted, and the ratio of the coarse powder of the overground part of the radix bupleuri to 55% ethanol is 0.8-1: 9-11, and the extraction container is a round-bottom flask or a multifunctional extraction tank.

6. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 2, is characterized in that: in the third step, a static heating reflux method is adopted for extraction, and the extraction time is 70-75 min each time.

7. The process for extracting the total flavonoids from the overground parts of the Chinese thorowax roots cultured in Ningxia as claimed in claim 2, is characterized in that: in the fourth step, the filtrate is decompressed and concentrated by a concentration tank, and the vacuum degree in the concentration tank is 0.080MPa-0.090 MPa.

Technical Field

The embodiment of the invention relates to the field of total flavone extraction processes, in particular to an extraction process of overground part of total flavone of radix bupleuri cultivated in Ningxia.

Background

The Bupleurum is derived from the plant of Bupleurum (Bupleurum L.) of Umbelliferae (Umbelliferae), is a common traditional Chinese medicine and is mainly used as a root medicine at present. Is slightly cold in nature, pungent and bitter in taste, has the effects of dispelling pathogenic wind, removing heat, soothing liver and invigorating yang, and is mainly used for treating cold, fever, alternating cold and heat, malaria, irregular menstruation, uterine prolapse and the like. The pharmacodynamic chemical components of the bupleurum root mainly comprise saponin, flavonoid, volatile oil, phytosterol, polysaccharide and the like, wherein the bupleurum flavone has stronger anti-influenza virus effect, better anti-inflammatory and cooling effects and stronger inhibiting or killing effect on various bacteria.

The radix bupleuri has obvious effect as a common traditional Chinese medicinal material, wild resources are frequently dangerous due to long-term blind excavation, the radix bupleuri is listed as a key variety for plant resource restoration in Ningxia, the radix bupleuri belongs to one of special medicinal materials in Ningxia Liupan mountain areas, large-scale planting is formed at present, the planting area reaches 3 ten thousand mu in 2013, and the radix bupleuri is expected to be planted in 4 thousand mu in the 2020 area in Ningxia traditional Chinese medicinal material industry development planning (2014 and 2020).

By consulting and analyzing the existing literature, the research on planting radix bupleuri in Ningxia is mainly focused on the content analysis and comparison of saikosaponin a and saikosaponin d in the planted radix bupleuri and wild radix bupleuri, the aspects of heavy metal, pesticide residue, fingerprint spectrum and the like of radix bupleuri medicinal materials, and the extraction and separation of flavonoid chemical components are not reported.

In addition, data review shows that the flavone content of the overground part of the bupleurum is much higher than that of the underground part, the medicinal part of the bupleurum is root at present, and the medicinal part of the bupleurum needs to be enlarged in order to better utilize resources.

However, in the prior art, the general flavone is extracted from the bupleurum by directly adopting high-concentration ethanol for direct heating reflux extraction, so that the extraction rate is not high, the extraction time is long, the process is complex, and the industrial production is not facilitated.

Disclosure of Invention

Therefore, the embodiment of the invention provides an extraction process of the total flavonoids in the overground part of the radix bupleuri cultivated in Ningxia, the dry extract of the total extraction of the overground part of the radix bupleuri is obtained by adopting the processes of crushing, room-temperature soaking, reflux extraction, concentration and the like, the extraction rate of the total flavonoids reaches 3.7 percent, zero breakthrough is realized for the extraction process of the total flavonoids in the overground part of the radix bupleuri cultivated in Ningxia, the process is simple and easy to implement, the industrial production is convenient to realize, and the problems in the background art are solved.

In order to achieve the above object, the embodiments of the present invention provide the following technical solutions: an extraction process of the general flavone of the overground part of the Chinese thorowax root cultivated in Ningxia comprises four steps of crushing, room temperature soaking, static heating reflux extraction, concentration and the like.

Further, the extraction process of the total flavonoids in the overground part of the bupleurum comprises the following specific steps:

step one, crushing: selecting aerial part of radix bupleuri cultivated in Ningxia, naturally airing, crushing by a small swing crusher, and sieving by a pharmacopeia No. two sieve to obtain coarse powder of aerial part of radix bupleuri for later use;

step two, soaking at room temperature: placing the coarse powder of the overground part of the radix bupleuri into an extraction container, adding 55% ethanol, and soaking for 50-70min in a closed manner at room temperature;

step three, static reflux extraction: soaking in 55% ethanol at room temperature under sealed condition, and extracting for 3 times by static heating reflux method;

step four, concentration: and combining the filtrates obtained by the 3 times of extraction, and concentrating the filtrate at the temperature of 55-57 ℃ under reduced pressure until all the solvents are evaporated to dryness to obtain a dry extract.

Further, in the step one, the coarse powder of the overground part of the bupleurum root crushed by a small swing crusher is screened by a pharmacopeia No. two sieve.

Further, in the second step, the feed-liquid ratio of the coarse powder of the overground part of the radix bupleuri to 55% ethanol is 0.8-1: 9 to 11.

Further, in the third step, a static heating reflux extraction method is adopted, and the ratio of the coarse powder of the overground part of the radix bupleuri to 55% ethanol is 0.8-1: 9-11, and the extraction container is a round-bottom flask or a multifunctional extraction tank.

Further, in the third step, the time for extracting the filtrate each time by adopting a static heating reflux method is 70-75 min.

And in the fourth step, the filtrate is subjected to reduced pressure concentration by a concentration tank, and the vacuum degree in the concentration tank is 0.080MPa to 0.090 MPa.

The embodiment of the invention has the following advantages:

1. the invention adopts the processes of crushing, room temperature soaking, reflux extraction, concentration and the like to obtain the total extracted dry extract of the overground part of the bupleurum, the extraction rate of the total flavone reaches 3.7 percent, zero breakthrough is realized for the extraction process of the overground part of the bupleurum in Ningxia cultivation, the process is simple and easy to implement, and the industrial production is convenient to realize;

2. the invention adopts room temperature dipping before extraction, which is beneficial for the solvent to fully enter the medicinal material cells, is convenient for extracting effective components and greatly shortens the dipping time;

3. the invention adopts a static heating reflux method for extraction, and the process is simple and easy to implement and is convenient for large-scale production.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.

The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.

FIG. 1 is a flow chart of the process for extracting total flavonoids from aerial parts of Bupleurum scorzonerifolium cultivated in Ningxia provided in embodiment 2 of the present invention;

Detailed Description

The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. 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.

In the invention, when the solvent is selected, 35%, 45%, 55%, 65%, 75% and 85% of ethanol is respectively used as the solvent for extracting the general flavone of the overground part of the radix bupleuri, and the extraction method is respectively used as the method for extracting by using an immersion method, a static heating reflux extraction method, a dynamic heating reflux extraction method, an ultrasonic auxiliary extraction method and a microblog auxiliary extraction method, and on the basis, the 55% of ethanol is emphatically determined as the solvent, the static heating reflux extraction method is used as the extraction method, and orthogonal optimization is carried out on the process, so that the extraction process of the overground part of the general flavone of the radix bupleuri cultivated in Ningxia is provided, zero breakthrough is realized for the extraction process of the overground part of the general flavone of the radix bupleuri cultivated in Ningxia, the process is simple and easy to implement and is convenient for.