阅读说明：本技术 一种从槐角中提取山柰酚的方法 (Method for extracting kaempferol from sophora fruit ) 是由 王德军 王双宁 陶正升 陈小慧 刘红艳 于 2021-08-06 设计创作，主要内容包括：本发明公开了一种从槐角中提取山柰酚的方法,包括如下步骤：称取适量槐角粉料加入NaOH溶液进行浸提,浸提温度为50℃～80℃,得到粗提液；将粗提液过滤,收集滤液加入乙酸调节pH至6～7,静置后浓缩得到浓缩提取液；将浓缩提取液加入酸性溶液进行水解,水解温度为60℃～70℃,然后过滤,收集滤渣；将滤渣水洗至水溶液呈中性后,将中性滤渣采用其3～7倍质量的乙醇进行热提取,70℃～80℃加热回流,过滤,收集所得滤液加入活性炭进行吸附脱色,然后过滤,再次收集滤液浓缩至原体积的1/5～1/7,得到浓缩滤液；将浓缩滤液静置,离心分离,沉淀干燥后粉碎后获得含量为98％的山奈酚成品。本发明提供的山奈酚提取方法工艺相对简洁易操作,适用于工业化生产。(The invention discloses a method for extracting kaempferol from sophora fruit, which comprises the following steps: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at 50-80 ℃ to obtain a crude extract; filtering the crude extract, collecting filtrate, adding acetic acid into the filtrate to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract; adding the concentrated extract into an acid solution for hydrolysis at the hydrolysis temperature of 60-70 ℃, then filtering, and collecting filter residues; washing the filter residue with water until the water solution is neutral, carrying out hot extraction on the neutral filter residue by using ethanol with the mass of 3-7 times of that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to carry out adsorption decoloration, then filtering, collecting the filtrate again, and concentrating the filtrate to 1/5-1/7 of the original volume to obtain concentrated filtrate; standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%. The kaempferol extraction method provided by the invention is relatively simple in process and easy to operate, and is suitable for industrial production.)

1. A method for extracting kaempferol from sophora fruit is characterized by comprising the following steps: the method comprises the following steps:

step 1: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at 50-80 ℃ to obtain a crude extract;

step 2: filtering the crude extract, collecting filtrate, adding acetic acid into the filtrate to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract;

and step 3: adding the concentrated extract into an acid solution for hydrolysis at the hydrolysis temperature of 60-70 ℃, then filtering, and collecting filter residues;

and 4, step 4: washing the filter residue with water until the water solution is neutral, carrying out hot extraction on the neutral filter residue by using ethanol with the mass of 3-7 times of that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to carry out adsorption decoloration, then filtering, collecting the filtrate again, and concentrating the filtrate to 1/5-1/7 of the original volume to obtain concentrated filtrate;

and 5: and standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%.

2. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: the preparation process of the sophora fruit powder comprises the following steps:

screening and cleaning the sophora fruit raw material, naturally drying in a cool and ventilated place, and crushing the dried sophora fruit raw material.

3. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: the proportion of the sophora fruit powder to the NaOH solution is 1kg to 7L, and the mass concentration of the NaOH solution is 2-6%.

4. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: in the step 1, the leaching time is 4-7 h, and the leaching times are 2-3.

5. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: and the standing time in the step 2 is 2-6 h.

6. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the ratio of the amount of the acidic solution used in step 3 to the sophora fruit powder is 1kg: 7L-8L, and the mass concentration of the acidic solution is 3% -6%.

7. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the hydrolysis time in step 3 is 3 hours, and the hydrolysis times are 2 to 3.

8. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the time of each heat extraction in step 4 is 2-4 h, and the number of heat extractions is 3.

9. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the concentration in step 2 and step 4 is performed by vacuum concentration.

10. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the recovery rate of kaempferol finished product obtained in step 5 is 80% -85%.

Technical Field

The invention belongs to the technical field of kaempferol extraction, and particularly relates to a method for extracting kaempferol from sophora fruit.

Background

The pod of sophorae is a dried mature fruit of leguminous plant Sophora japonica (Sophora japonica L.), also called fructus sophorae, Sophora fruit, kidney bean, locust bean and the like, is a common Chinese medicinal material in China, and is listed as the top grade in Shennong Ben Cao Jing. With the rapid development of modern science and technology, a plurality of chemical components in the fructus sophorae are separated and identified, wherein the fructus sophorae is mainly composed of flavone and isoflavone compounds, and the fructus sophorae has great significance and value for researching pharmacological efficacy and corresponding effective components of the fructus sophorae.

Kaempferol (Kaempferol) is used as a main flavonol compound in the fructus sophorae and becomes a research hotspot in fructus sophorae extract because the Kaempferol has the functions of resisting oxidation and cancer, treating diabetes and osteoporosis, inhibiting fertility and the like. The kaempferol is yellow powder, is slightly soluble in water, is dissolved in hot ethanol, alkali and other liquids, and exists in the form of glucoside in the fructus sophorae, so that the kaempferol can be effectively and efficiently extracted through the physicochemical characteristics of the kaempferol in the fructus sophorae, and the efficacy of the kaempferol is exerted and applied to the maximum extent.

The existing kaempferol extraction mode generally adopts enzymolysis to decompose kaempferol and adopts macroporous resin and other methods to purify, the extraction cost is high, and the technological operation process is complicated.

Disclosure of Invention

The invention aims to provide a method for extracting kaempferol from sophora fruit, which integrally adopts alkaline liquor for preliminary extraction, then adopts acid hydrolysis to obtain mixed liquor containing kaempferol, and then adopts ethanol for effective extraction so as to solve the problems of higher extraction cost and more complex process operation process caused by the existing modes of decomposition of kaempferol by enzymolysis, macroporous resin and the like for purification.

The invention is realized by the following technical scheme:

the method for extracting the kaempferol from the sophora fruit comprises the following steps:

step 1: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at 50-80 ℃ to obtain a crude extract;

step 2: filtering the crude extract, collecting filtrate, adding acetic acid into the filtrate to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract;

and step 3: adding the concentrated extract into an acid solution for hydrolysis at the hydrolysis temperature of 60-70 ℃, then filtering, and collecting filter residues;

and 4, step 4: washing the filter residue with water until the water solution is neutral, carrying out hot extraction on the neutral filter residue by using ethanol with the mass of 3-7 times of that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to carry out adsorption decoloration, then filtering, collecting the filtrate again, and concentrating the filtrate to 1/5-1/7 of the original volume to obtain concentrated filtrate;

and 5: and standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%.

As a further illustration of the invention, the preparation process of the sophora fruit powder is as follows:

screening and cleaning the sophora fruit raw material, naturally drying in a cool and ventilated place, and crushing the dried sophora fruit raw material.

As a further explanation of the invention, the proportion of the sophora fruit powder and the NaOH solution is 1kg:7L, and the mass concentration of the NaOH solution is 2-6%.

As a further illustration of the invention, the leaching time in the step 1 is 4-7 h, and the leaching times are 2-3.

As a further explanation of the invention, the standing time in the step 2 is 2 to 6 hours.

As a further description of the invention, the ratio of the amount of the acidic solution used in the step 3 to the sophora fruit powder is 1kg: 7L-8L, and the mass concentration of the acidic solution is 3% -6%.

As a further explanation of the invention, the hydrolysis time in step 3 is 3 hours, and the hydrolysis times are 2 to 3 times.

As a further explanation of the invention, the time of each heat extraction in the step 4 is 2-4 h, and the number of heat extractions is 3.

As a further illustration of the invention, vacuum concentration is adopted in the concentration mode in step 2 and step 4.

As a further illustration of the invention, the recovery rate of the kaempferol finished product obtained in step 5 is 80-85%.

Compared with the prior art, the invention has the following beneficial technical effects:

the method uses alkali liquor for primary extraction, can effectively improve the extraction rate of the kaempferol, and can separate the kaempferol from most of the sophora fruit components in one step.

The kaempferol extraction method provided by the invention is different from other extraction methods, the process flow adopts alkaline liquor for preliminary extraction, the mixed liquor containing kaempferol is obtained through acid hydrolysis, then ethanol is adopted for effective extraction, decomposition of kaempferol is not carried out through enzymolysis, and purification is carried out through methods such as macroporous resin and the like, the cost is reduced, the process is relatively simple and easy to operate, and the method is suitable for industrial production.

Drawings

Fig. 1 is a flow chart of the method for extracting kaempferol from sophora fruit provided by the invention.

Detailed Description

In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

Example 1:

step 1: screening and cleaning the fructus sophorae raw material, naturally airing in a cool and ventilated place, crushing the aired fructus sophorae raw material, weighing 10kg of the crushed fructus sophorae raw material, adding 70L of 2% NaOH solution for leaching at the leaching temperature of 50 ℃ for 4h, and repeatedly leaching for 2 times to obtain a crude extract.

Step 2: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 6, standing for 2 hr, and vacuum concentrating to obtain concentrated extract.

And step 3: adding the obtained concentrated extractive solution into 70L of 3% acetic acid solution for hydrolysis at 60 deg.C for 3 hr, repeating hydrolysis for 2 times, filtering, and collecting residue.

And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue with 3 times of ethanol by mass, performing heating reflux at 70 ℃, repeatedly extracting for 3 times at 2h each time, filtering, collecting filtrate, adding activated carbon for adsorption decoloration, stirring uniformly, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/5 of the original volume to obtain concentrated filtrate;

and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 85% and content of 98.1%.

Example 2:

step 1: screening and cleaning the fructus sophorae raw material, naturally airing in a cool and ventilated place, crushing the aired fructus sophorae raw material, weighing 10kg of the crushed fructus sophorae raw material, adding 70L of 4% NaOH solution for leaching, leaching at 65 ℃ for 5.5h, and repeatedly leaching for 3 times to obtain a crude extract.

Step 2: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 7, standing for 3.5 hr, and vacuum concentrating to obtain concentrated extract.

And step 3: adding the obtained concentrated extractive solution into 75L of 4.5% acetic acid solution, hydrolyzing at 65 deg.C for 3 hr, repeating the hydrolysis for 3 times, filtering, and collecting residue.

And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using ethanol with the mass of 5 times of that of the neutral filter residue, performing heating reflux at 75 ℃, repeatedly extracting for 3 times, extracting for 3 hours each time, filtering, collecting filtrate, adding activated carbon to perform adsorption decoloration, stirring uniformly, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/6 of the original volume to obtain concentrated filtrate;

and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 83% and content of 98.6%.

Example 3:

step 1: screening and cleaning the fructus sophorae raw material, naturally airing in a cool and ventilated place, crushing the aired fructus sophorae raw material, weighing 10kg of the crushed fructus sophorae raw material, adding 70L of 6% NaOH solution for leaching, leaching at 80 ℃ for 7h, and repeatedly leaching for 3 times to obtain a crude extract.

Step 2: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 7, standing for 6 hr, and vacuum concentrating to obtain concentrated extract.

And step 3: adding the obtained concentrated extractive solution into 80L 6% phosphoric acid solution, hydrolyzing at 70 deg.C for 3 hr, repeating the hydrolysis for 3 times, filtering, and collecting residue.

And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using ethanol with the mass of 7 times of that of the neutral filter residue, performing heating reflux at the temperature of 80 ℃, repeatedly extracting for 3 times, extracting for 4 hours each time, filtering, collecting filtrate, adding activated carbon to perform adsorption decoloration, uniformly stirring, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/7 of the original volume to obtain concentrated filtrate;

and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 80% and content of 98.8%.

The method uses alkali liquor for primary extraction, can effectively improve the extraction rate of the kaempferol, and can separate the kaempferol from most of the sophora fruit components in one step.

The kaempferol extraction method provided by the invention is different from other extraction methods, the process flow adopts alkaline liquor for preliminary extraction, the mixed liquor containing kaempferol is obtained through acid hydrolysis, then ethanol is adopted for effective extraction, decomposition of kaempferol is not carried out through enzymolysis, and purification is carried out through methods such as macroporous resin and the like, the cost is reduced, the process is relatively simple and easy to operate, and the method is suitable for industrial production.

Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.