Ilex rotunda thunb extract and extraction process thereof

Abstract

The invention relates to the field of traditional Chinese medicine extraction, in particular to an ovateleaf holly bark extract and an extraction process thereof.The ovateleaf holly bark extract containing pedunculoside and syringin is obtained from an ovateleaf holly bark extracting solution and medicine residues in a heating reflux mode, and the ovateleaf holly bark extract containing pedunculoside and syringin is extracted through the heating reflux mode. Compared with the prior art, more pedunculoside and syringin can be obtained, while the extract is prepared through the extracting solution, originally discarded medicine residues are further fully extracted, resources are fully utilized, the production cost is reduced, the content of the extract is increased, and the content of the extract is further increased through cooperation of filtering operation.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicine extraction, and in particular to a scutellaria baicalensis extract and an extraction process thereof. Background Art

[0002] The Chinese medicinal herb Jiubiying is the dried bark of Ilex xanthophylla, a plant of the Aquifoliaceae family. It is widely distributed in southern provinces of China and is commonly used by the folks for clearing away heat and detoxifying, reducing swelling and relieving pain, treating colds and fever, acute and chronic hepatitis, acute gastroenteritis, gastric and duodenal ulcers, and rheumatic joint pain. Therefore, Jiubiying is a medicinal herb with a wide range of uses and is also known as "Jiubingying".

[0003] At present, the extraction process of scutellaria baicalensis mostly adopts water extraction method, and the scutellaria baicalensis residue after extraction is discarded as waste residue, which is not environmentally friendly and a waste. In addition, the water extraction method mainly extracts the water-soluble component syringin in scutellaria baicalensis, while there are still many pentacyclic triterpenoid saponins in the residue that have not been completely extracted, resulting in a waste of resources.

[0004] Therefore, those skilled in the art provide a Herba Lysimachiae extract and an extraction process thereof to solve the problems raised in the above background technology. Summary of the invention

[0005] In order to solve the above technical problems, the present invention aims to provide a method for obtaining a Herba Schizonepetae Extract containing pedunculate glycosides and syringin from the Herba Schizonepetae Extract and the Herba Schizonepetae Reticulatae residues by heating and reflux.

[0006] The present invention provides an extraction process of a scutellaria baicalensis extract, comprising the following steps:

[0007] Step S1: Wash and dry the Jiubiying medicinal materials, crush them and sieve them through 60-80 mesh;

[0008] Step S2: mixing the crushed Jiubing powder with an extraction solvent, performing reflux extraction at a temperature of 85-95° C. for 120-180 min, filtering and collecting the filtrate after extraction to obtain a medicinal residue precipitate and an extract A, respectively;

[0009] Step S3: the extract A is concentrated by alcohol precipitation, filtered to obtain an alcohol precipitate, ethanol is recovered from the alcohol precipitate, concentrated to obtain a concentrated solution A, the concentrated solution A is concentrated to 1 / 2 of the volume of the extract, cooled to room temperature and centrifuged to obtain a precipitate and a supernatant, 50-95% ethanol is added to the precipitate for reflux extraction, the filtrate is concentrated and dried to obtain total saponin A, the supernatant is filtered and the filtrate is collected and concentrated to obtain total saponin B;

[0010] Step S4: adding 90-95% ethanol to the residue precipitate for extraction, filtering to obtain an alcohol extract, recovering the solvent from the alcohol extract, concentrating to obtain a concentrated solution B, concentrating the concentrated solution B to an extract state, adding silica gel to mix, and then drying to obtain an alcohol extract silica gel powder, extracting the alcohol extract silica gel powder with a weakly polar organic solvent to obtain an extract B, recovering the solvent from the extract B, filtering and drying to obtain total saponins C;

[0011] Step S5: The sum of total saponin A, total saponin B and total saponin C is the Herba Cibotii extract obtained by the extraction process.

[0012] Preferably, the weakly polar organic solvent is chloroform, benzene, dichloromethane or petroleum ether.

[0013] Preferably, each 1 g of the Herba Lysimachiae extract contains 304 mg of pedunculate glycoside and 62 mg of syringin.

[0014] Preferably, step S2 can be repeated 2-3 times, and the extraction solvent is 2-10 times of 50-95% ethanol solution.

[0015] Preferably, the filtering steps in step S3 and step S4 include: using coarse filtration, fine filtration, microfiltration and nanofiltration membrane filtration in sequence.

[0016] Technical effects and advantages of the present invention:

[0017] The present invention firstly adopts a heating reflux method, which is different from the room temperature immersion and conventional water extraction methods in the prior art. The extraction process can obtain more pedunculate holly glycoside and syringin.

[0018] While the extract is prepared by the extraction liquid, the originally discarded drug residue is further fully extracted to fully utilize resources, reduce production costs, and increase the content of the extract.

[0019] The concentration of the extract product is further increased by using coarse filtration, fine filtration, microfiltration and nanofiltration membrane filtration in sequence, combined with concentration work. DETAILED DESCRIPTION

[0020] The present invention will be further described in detail below in conjunction with specific embodiments. The embodiments of the present invention are provided for the purpose of illustration and description, and are not intended to be exhaustive or to limit the present invention to the disclosed forms. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments are selected and described to better illustrate the principles and practical applications of the present invention, and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific uses.

[0021] Example 1

[0022] In this embodiment, an extraction process of a scutellaria baicalensis extract is provided, comprising the following steps:

[0023] Step S1: Wash and dry the Jiubiying medicinal materials, crush them and sieve them through 70 meshes;

[0024] Step S2: mixing the crushed Jiubing powder with 2-10 times of 50-95% ethanol solution, refluxing and extracting at 85°C for 150 minutes, filtering and collecting the filtrate after extraction to obtain a medicinal residue precipitate and an extract A respectively; step S2 can be repeated 2-3 times;

[0025] Step S3: the extract A is concentrated by alcohol precipitation, filtered to obtain an alcohol precipitate, ethanol is recovered from the alcohol precipitate, concentrated to obtain a concentrated solution A, the concentrated solution A is concentrated to 1 / 2 of the volume of the extract, cooled to room temperature and centrifuged to obtain a precipitate and a supernatant, 50-95% ethanol is added to the precipitate for reflux extraction, the filtrate is concentrated and dried to obtain total saponin A, the supernatant is filtered and the filtrate is collected and concentrated to obtain total saponin B;

[0026] Step S4: adding 90-95% ethanol to the residue precipitate for extraction, filtering to obtain an alcohol extract, recovering the solvent from the alcohol extract, concentrating to obtain a concentrated solution B, concentrating the concentrated solution B to an extract state, adding silica gel to mix, and then drying to obtain an alcohol extract silica gel powder, extracting the alcohol extract silica gel powder with a weakly polar organic solvent to obtain an extract B, recovering the solvent from the extract B, filtering and drying to obtain total saponins C;

[0027] In the above steps, the filtering step includes coarse filtration, fine filtration, microfiltration and nanofiltration membrane filtration in sequence.

[0028] Step S5: The sum of total saponin A, total saponin B and total saponin C is the Herba Cibotii extract obtained by the extraction process.

[0029] Wherein, the weakly polar organic solvent is chloroform, benzene, dichloromethane or petroleum ether.

[0030] Comparative Example 1

[0031] The conventional ultrasonic treatment method is used to treat the Herba Cibotii medicinal materials to obtain the corresponding Herba Cibotii extracts.

[0032] Comparative Example 2

[0033] Different from Example 1, this solution does not recover and extract the medicinal residue precipitate.

[0034] The extraction process includes the following steps:

[0035] Step S1: Wash and dry the Jiubiying medicinal materials, crush them and sieve them through 70 meshes;

[0036] Step S2: mixing the crushed Jiubing powder with 2-10 times of 50-95% ethanol solution, refluxing and extracting at 85°C for 150 minutes, filtering and collecting the filtrate after extraction to obtain a medicinal residue precipitate and an extract A respectively; step S2 can be repeated 2-3 times;

[0037] Step S3: the extract A is concentrated by alcohol precipitation, filtered to obtain an alcohol precipitate, ethanol is recovered from the alcohol precipitate, concentrated to obtain a concentrated solution A, the concentrated solution A is concentrated to 1 / 2 of the volume of the extract, cooled to room temperature and centrifuged to obtain a precipitate and a supernatant, 50-95% ethanol is added to the precipitate for reflux extraction, the filtrate is concentrated and dried to obtain total saponin A, the supernatant is filtered and the filtrate is collected and concentrated to obtain total saponin B;

[0038] In the above steps, the filtering step includes coarse filtration, fine filtration, microfiltration and nanofiltration membrane filtration in sequence.

[0039] Step S5: The sum of total saponin A and total saponin B is the Herba Cibotii extract obtained by the extraction process.

[0040] Compared with the ultrasonic treatment method in comparative example 1, the extraction process designed in this scheme was used to extract 100g of scutellaria baicalensis to obtain 21g of total glycoside extract, and each 1g of the extract contained 304mg of long-pedunculated holly glycoside and 62mg of syringin. Compared with comparative example 2, the content of total saponins in embodiment 1 was significantly increased.

[0041] Compared with the existing technology, the content of total glycosides extracted is significantly improved.

[0042] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field and related fields without creative work should fall within the scope of protection of the present invention. The structures, devices and operating methods not specifically described and explained in the present invention are implemented according to the conventional means in the field unless otherwise specified and limited.

Claims

1. A Herba Cibotii extract, characterized in that: The method of heating and reflux is adopted to obtain the sauerkraut extract containing hollycoside and syringin from the sauerkraut extract and the dregs of the sauerkraut.

2. An extraction process of a Herba Cibotii extract according to claim 1, characterized in that: The following steps are involved: Step S1: Wash and dry the Jiubiying medicinal materials, crush them and sieve them through 60-80 mesh; Step S2: mixing the crushed Jiubing powder with an extraction solvent, performing reflux extraction at a temperature of 85-95° C. for 120-180 min, filtering and collecting the filtrate after extraction to obtain a medicinal residue precipitate and an extract A, respectively; Step S3: the extract A is concentrated by alcohol precipitation, filtered to obtain an alcohol precipitate, ethanol is recovered from the alcohol precipitate, concentrated to obtain a concentrated solution A, the concentrated solution A is concentrated to 1 / 2 of the volume of the extract, cooled to room temperature and centrifuged to obtain a precipitate and a supernatant, 50-95% ethanol is added to the precipitate for reflux extraction, the filtrate is concentrated and dried to obtain total saponin A, the supernatant is filtered and the filtrate is collected and concentrated to obtain total saponin B; Step S4: adding 90-95% ethanol to the residue precipitate for extraction, filtering to obtain an alcohol extract, recovering the solvent from the alcohol extract, concentrating to obtain a concentrated solution B, concentrating the concentrated solution B to an extract state, adding silica gel to mix, and then drying to obtain an alcohol extract silica gel powder, extracting the alcohol extract silica gel powder with a weakly polar organic solvent to obtain an extract B, recovering the solvent from the extract B, filtering and drying to obtain total saponins C; Step S5: The sum of total saponin A, total saponin B and total saponin C is the Herba Cibotii extract obtained by the extraction process.

3. The extraction process of the extract of the Herba Cibotii according to claim 2, characterized in that: The weakly polar organic solvent is chloroform, benzene, dichloromethane or petroleum ether.

4. The extraction process of the Herba Cibotii extract according to claim 2, characterized in that: Every 1g of the extract of the herb contains 304mg of hollyglossin and 62mg of syringin.

5. The extraction process of the Herba Cibotii extract according to claim 2, characterized in that: The step S2 can be repeated 2-3 times, and the extraction solvent is 2-10 times of 50-95% ethanol solution.

6. The extraction process of the Herba Cibotii extract according to claim 2, characterized in that: The filtering steps in step S3 and step S4 include: using coarse filtration, fine filtration, microfiltration and nanofiltration membrane filtration in sequence.