阅读说明：本技术 一种从鲜黄芩茎叶提取野黄芩苷的方法 (Method for extracting scutellarin from fresh scutellaria baicalensis stem and leaf ) 是由 贾俊宇 贾俊琪 于 2021-07-13 设计创作，主要内容包括：本发明涉及一种从鲜黄芩茎叶提取野黄芩苷的方法。本发明主要是解决现有提取野黄芩苷的方法存在的溶剂用量大、蒸煮消耗能源大和提取成本高的技术问题。本发明采用的技术方案是：其具体步骤如下：1)称取鲜黄芩茎叶压块熟化；2)将熟化后的鲜黄芩茎叶压块放入容器中并加入常温水,然后再加入葡萄酒下脚料,在温度为20°～35°下浸泡发酵12～36小时；3)将发酵好的溶液粗滤至加热器中,加热到60～65°后沉淀1～2小时,再精滤到反应釜中；4)将步骤3)中加入硫酸铝钾的混合液静置3～6小时,去掉上清液,收集沉淀物,并将沉淀物水洗到中性,压饼,烘干,即得含量为55～75％的野黄芩苷粗品。(The invention relates to a method for extracting scutellarin from fresh scutellaria baicalensis stem leaves. The invention mainly solves the technical problems of large solvent consumption, large energy consumption for cooking and high extraction cost in the existing method for extracting scutellarin. The technical scheme adopted by the invention is as follows: the method comprises the following specific steps: 1) weighing fresh scutellaria baicalensis stem leaves, pressing blocks and curing; 2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water, then adding the wine leftovers, and soaking and fermenting for 12-36 hours at the temperature of 20-35 ℃; 3) coarsely filtering the fermented solution into a heater, heating to 60-65 ℃, precipitating for 1-2 hours, and finely filtering into a reaction kettle; 4) and (3) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 3-6 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, and drying to obtain a scutellarin crude product with the content of 55-75%.)

1. A method for extracting scutellarin from fresh scutellaria baicalensis stem leaves is characterized by comprising the following specific steps:

1) weighing 500 g of fresh scutellaria stem and leaf, pressing into blocks and curing;

2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water which is 5 times of the weight of the fresh scutellaria baicalensis stem and leaf, then adding 0.1 g of wine leftovers, and soaking and fermenting for 12-36 hours at the temperature of 20-35 ℃;

3) coarsely filtering the fermented solution into a heater, heating to 60-65 ℃, precipitating for 1-2 hours, finely filtering into a reaction kettle, adding acid salt, wherein the weight ratio of the filtrate to the acid salt is 1000: 3, then adding hydrochloric acid, stirring for 3-5 minutes when the pH value of the filtrate reaches 1-1.5, and then adding aluminum potassium sulfate, wherein the weight ratio of the filtrate to the aluminum potassium sulfate is 1000: 1;

4) and (3) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 3-6 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, and drying to obtain a scutellarin crude product with the content of 55-75%.

2. The method for extracting scutellarin from fresh scutellarin stems and leaves according to claim 1, wherein the scutellarin is extracted from fresh scutellarin stems and leaves by the following steps: the briquetting and curing means that fresh scutellaria baicalensis stem leaves are pressed into blocks by a press and cured for 2-3 minutes at 100 ℃ or cured and then briquetted.

3. The method for extracting scutellarin from fresh scutellarin stems and leaves according to claim 1, wherein the scutellarin is extracted from fresh scutellarin stems and leaves by the following steps: the acid salt is prepared from hydrochloric acid and sodium hydroxide.

4. The method for extracting scutellarin from fresh scutellarin stems and leaves according to claim 1 or 3, wherein the scutellarin is extracted from fresh scutellarin stems and leaves: the concentration of the hydrochloric acid is 36%.

Technical Field

The invention belongs to the technical field of extraction of effective components of Chinese herbal medicines, and particularly relates to a method for extracting scutellarin from fresh scutellarin stems and leaves.

Background

Scutellariae radix is a perennial herb of Labiatae, and the root of Scutellariae radix is a Chinese herbal medicine, has effects of clearing heat, eliminating dampness, clearing pathogenic fire, removing toxic substance, stopping bleeding, and preventing miscarriage, and can be used for treating damp warmth, summer dampness, chest distress, nausea, damp heat, fullness, dysentery, jaundice, cough due to lung heat, hyperpyrexia, polydipsia, etc. Currently, the root of scutellaria baicalensis is mainly used as a traditional medicine, and the stem and leaf of scutellaria baicalensis are regarded as waste to be abandoned. However, researches show that the main component of the stem and leaf of the scutellaria baicalensis is scutellarin, and the stem and leaf of the scutellaria baicalensis are directly discarded to cause waste of medicinal resources.

The existing method for extracting scutellarin from stem and leaf of scutellaria baicalensis comprises the following steps: pulverizing Scutellariae radix stem and leaf; adding ethanol, and heating to boil; filtering the extractive solution, and concentrating under reduced pressure; heating the concentrated solution to boil, adjusting pH to 7-8, and filtering while hot; adjusting the pH value of the filtrate to 1-2, standing to obtain brown precipitate and khaki precipitate, filtering, washing the filter cake with distilled water, then washing with a solvent to neutrality, and drying to obtain crude scutellarin; adding solvent and active carbon, heating, filtering the extractive solution, concentrating the filtrate, standing to precipitate crystal, filtering, and washing with solvent to obtain scutellarin crystal; adding solvent into scutellarin crystal, shaking, adjusting pH to 1-2, standing, filtering, washing precipitate with water to neutral, and drying to obtain high-purity scutellarin. The extraction method has the problems of large solvent consumption, large energy consumption for cooking and high extraction cost.

Disclosure of Invention

The invention aims to solve the technical problems of large solvent consumption, large energy consumption for cooking and high extraction cost of the existing method for extracting scutellarin and provides a method for extracting scutellarin from fresh scutellarin stems and leaves.

In order to solve the technical problems, the invention adopts the technical scheme that:

a method for extracting scutellarin from fresh scutellaria baicalensis stem leaves comprises the following specific steps:

1) weighing 500 g of fresh scutellaria stem and leaf, pressing into blocks and curing;

2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water which is 5 times of the weight of the fresh scutellaria baicalensis stem and leaf, then adding 0.1 g of wine leftovers, and soaking and fermenting for 12-36 hours at the temperature of 20-35 ℃;

3) coarsely filtering the fermented solution into a heater, heating to 60-65 ℃, precipitating for 1-2 hours, finely filtering into a reaction kettle, adding acid salt, wherein the weight ratio of the filtrate to the acid salt is 1000: 3, then adding hydrochloric acid, stirring for 3-5 minutes when the pH value of the filtrate reaches 1-1.5, and then adding aluminum potassium sulfate, wherein the weight ratio of the filtrate to the aluminum potassium sulfate is 1000: 1;

4) and (3) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 3-6 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, and drying to obtain a scutellarin crude product with the content of 55-75%.

Further, the briquetting and curing means that fresh scutellaria baicalensis stems and leaves are pressed into blocks by a press, and the blocks are cured for 2-3 minutes at 100 degrees or are cured firstly and then pressed into blocks.

Further, the acid salt is made from hydrochloric acid and sodium hydroxide.

Further, the concentration of the hydrochloric acid is 36%.

The invention has the beneficial effects that:

by adopting the technical scheme, the fresh scutellarin stems and leaves are cured and compressed and are fermented at low temperature, so that the technical problems of large solvent consumption, large cooking energy consumption and high extraction cost in the existing scutellarin extraction method are solved. Compared with the background art, the invention has the advantages that: 1) the invention only cures the stem and leaf of the scutellaria baicalensis, thereby reducing the energy consumption and the production cost; 2) the invention uses normal temperature water for fermentation, effectively improves the extraction rate, does not use ethanol as a solvent, greatly reduces the cost, recovers the energy required by the ethanol, and further saves the production cost. 3) Because the stem and leaf protective film of the scutellaria baicalensis is weak, the glycosides and the wild glycosides are easy to oxidize, the cured and compressed whole stem and leaf is adopted in the invention, the extraction of the wild baicalin is facilitated, and the later operation is convenient.

Detailed Description

The present invention will be further described with reference to examples.

Example 1:

in this embodiment, a method for extracting scutellarin from fresh scutellaria baicalensis stem and leaf comprises the following specific steps:

1) weighing 500 g of fresh scutellaria stem and leaf, pressing into blocks and curing; the briquetting and curing means that fresh scutellaria baicalensis stem leaves are pressed into blocks by a press machine and cured for 2-3 minutes at 100 ℃;

2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water which is 5 times of the weight of the fresh scutellaria baicalensis stem and leaf, then adding 0.1 g of wine leftovers, and soaking and fermenting for 30-36 hours at the temperature of 20 ℃;

3) coarsely filtering the fermented solution in a heater, heating to 60 ℃, precipitating for 2 hours, finely filtering in a reaction kettle, adding acid salt, wherein the weight ratio of the filtrate to the acid salt is 1000: 3, then adding hydrochloric acid, stirring for 3-5 minutes when the pH value of the filtrate reaches 1-1.5, and then adding aluminum potassium sulfate, wherein the weight ratio of the filtrate to the aluminum potassium sulfate is 1000: 1; the acid salt is prepared from hydrochloric acid and sodium hydroxide;

4) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 3 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, drying, and recovering a crude scutellarin product with the content of 75 percent.

The concentration of the hydrochloric acid is 36%.

Example 2:

in this embodiment, a method for extracting scutellarin from fresh scutellaria baicalensis stem and leaf comprises the following specific steps:

1) weighing 500 g of fresh scutellaria stem and leaf, pressing into blocks and curing; the briquetting and curing means that fresh scutellaria baicalensis stem leaves are pressed into blocks by a press machine and cured for 2-3 minutes at 100 ℃;

2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water which is 5 times of the weight of the fresh scutellaria baicalensis stem and leaf, then adding 0.1 g of wine leftovers, and soaking and fermenting for 12-20 hours at the temperature of 35 ℃;

3) coarsely filtering the fermented solution in a heater, heating to 65 ℃, precipitating for 1 hour, finely filtering in a reaction kettle, adding acid salt, wherein the weight ratio of the filtrate to the acid salt is 1000: 3, then adding hydrochloric acid, stirring for 3-5 minutes when the pH value of the filtrate reaches 1-1.5, and then adding aluminum potassium sulfate, wherein the weight ratio of the filtrate to the aluminum potassium sulfate is 1000: 1; the acid salt is prepared from hydrochloric acid and sodium hydroxide;

4) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 6 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, drying, and recovering a crude scutellarin product with the content of 55%.

The concentration of the hydrochloric acid is 36%.

Example 3

In this embodiment, a method for extracting scutellarin from fresh scutellaria baicalensis stem and leaf comprises the following specific steps:

1) weighing 500 g of fresh scutellaria stem and leaf, pressing into blocks and curing; the briquetting and curing means that fresh scutellaria baicalensis stem leaves are pressed into blocks by a press machine and cured for 2-3 minutes at 100 ℃;

2) putting the cured fresh scutellaria baicalensis stem and leaf briquettes into a container, adding normal temperature water which is 5 times of the weight of the fresh scutellaria baicalensis stem and leaf, then adding 0.1 g of wine leftovers, and soaking and fermenting for 18-30 hours at the temperature of 28 ℃;

3) coarsely filtering the fermented solution in a heater, heating to 62 ℃, precipitating for 1.5 hours, finely filtering in a reaction kettle, adding acid salt, wherein the weight ratio of the filtrate to the acid salt is 1000: 3, then adding hydrochloric acid, stirring for 3-5 minutes when the pH value of the filtrate reaches 1-1.5, and then adding aluminum potassium sulfate, wherein the weight ratio of the filtrate to the aluminum potassium sulfate is 1000: 1; the acid salt is prepared from hydrochloric acid and sodium hydroxide;

4) standing the mixed solution added with the potassium aluminum sulfate in the step 3) for 6 hours, removing supernatant, collecting precipitate, washing the precipitate to be neutral, pressing into cakes, drying, and recovering a crude scutellarin product with the content of 65%.

The concentration of the hydrochloric acid is 36%.

The curing of the briquette in the above embodiment may also be performed after curing.

As the present invention may be embodied in several forms without departing from the spirit or scope of the present invention, it should also be understood that the above-described embodiments are not limited by the details of the foregoing description, but rather should be construed broadly within its scope as defined in the appended claims. It should be noted that, for a person skilled in the art, several modifications and variations within the equivalent scope can be made without departing from the structure of the invention, and these modifications and variations should also be considered as the protection scope of the invention.