阅读说明：本技术 一种以豆脐为原料制备黄豆黄素的方法 (Method for preparing glycitein by taking bean umbilicus as raw material ) 是由 刘汝萃 鲁绪强 韩亮 刘代成 董欣伟 时玉强 崔玉涛 刘杰 于 2019-06-17 设计创作，主要内容包括：本发明公开了一种以豆脐为原料制备黄豆黄素的方法,包括如下步骤：将80-100目豆脐粉在55-65％的乙醇中提取45-60min,每100g豆脐粉中加入乙醇溶液的体积为500-600ml,得提取液,将提取液蒸干,得干渣；向干渣中加入正己烷提取后,弃正己烷上清液,得渣；向渣中加入乙酸乙酯萃取,经离心得上清液,将上清液蒸干,得黄豆黄素。对豆脐粉用特定的工艺进行提取时,可以提取得到单一成分的异黄酮-黄豆黄素,经过正己烷除脂和经乙酸乙酯除杂后,得到黄豆黄素纯品。该方法简单、快速、成本低,可以适用于工业生产。(the invention discloses a method for preparing glycitein by taking bean umbilicus as a raw material, which comprises the following steps: extracting 80-100 mesh bean navel powder in 55-65% ethanol for 45-60min, adding ethanol solution with volume of 500-600ml into per 100g bean navel powder to obtain extractive solution, and evaporating to dry to obtain dry residue; adding n-hexane into the dry residue, extracting, and removing the n-hexane supernatant to obtain residue; adding ethyl acetate into the residue, extracting, centrifuging to obtain supernatant, and evaporating the supernatant to dryness to obtain glycitein. When the soybean navel powder is extracted by a specific process, isoflavone, glycitein, with a single component can be extracted, and a pure glycitein product is obtained after n-hexane degreasing and ethyl acetate impurity removal. The method is simple, rapid, low in cost and suitable for industrial production.)

1. a method for preparing glycitein by taking a bean navel as a raw material is characterized by comprising the following steps: the method comprises the following steps:

Extracting 80-100 mesh bean navel powder in 55-65% ethanol for 45-60min, adding ethanol solution with volume of 500-600ml into per 100g bean navel powder to obtain extractive solution, and evaporating to dry to obtain dry residue;

adding n-hexane into the dry residue, extracting, and removing the n-hexane supernatant to obtain residue;

Adding ethyl acetate into the residue, extracting, centrifuging to obtain supernatant, and evaporating the supernatant to dryness to obtain glycitein.

2. The method for preparing glycitein from umbilicus esculentus according to claim 1, wherein: adding 15-20ml of n-hexane into dry residue per 100g of bean navel powder for removing oil and fat.

3. The method for preparing glycitein from umbilicus esculentus according to claim 1, wherein: adding n-hexane, and extracting for 10-20 min.

4. The method for preparing glycitein from umbilicus esculentus according to claim 1, wherein: and (3) centrifugally separating the system after n-hexane extraction, discarding the n-hexane supernatant, wherein the centrifugal rotation speed is 1000-1500r/min, and the centrifugal time is 5-10 min.

5. The method for preparing glycitein from umbilicus esculentus according to claim 1, wherein: the extraction time of ethyl acetate is 10-20 min.

6. A method for preparing glycitein by taking a bean navel as a raw material is characterized by comprising the following steps: the method comprises the following steps:

Adding n-hexane into the bean navel powder, stirring and extracting to obtain an extracting solution, and evaporating the extracting solution to dryness to obtain bean navel oil;

Adding anhydrous ethanol into the Sophora umbilicalis oil at a volume ratio of the anhydrous ethanol to the Sophora umbilicalis oil of 9-15:1, extracting for 0.5-1h, standing for layering, collecting the upper layer solution, and steaming to obtain paste;

Adding anhydrous ethanol into the paste for extraction, taking supernatant, and evaporating the supernatant to dryness to obtain glycitein.

7. The method for preparing glycitein from umbilicus esculentus according to claim 6, wherein: and (3) repeatedly extracting the bean navel powder by using n-hexane for 5-8 times, wherein the dosage ratio of the n-hexane to the bean navel powder is as follows: 1.5-3: 1, V/M.

8. The method for preparing glycitein from umbilicus esculentus according to claim 6, wherein: the extraction time of the soybean navel powder by n-hexane is 1-1.5h each time, and the extraction temperature is 15-30 ℃.

9. The method for preparing glycitein from umbilicus esculentus according to claim 6, wherein: the volume ratio of the soybean navel oil to the absolute ethyl alcohol added into the soybean navel oil is 1: 8-12.

10. The method for preparing glycitein from umbilicus esculentus according to claim 6, wherein: the mass ratio of the paste to the absolute ethyl alcohol is 100 times.

Technical Field

The invention particularly relates to a method for preparing glycitein by taking bean umbilicus as a raw material.

Background

the information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.

The soybean is a traditional food in China, contains a large amount of physiologically active substances including oligosaccharides, phospholipids, vitamins, isoflavone, soyasaponin and the like, and the comprehensive development and utilization of the soybean are more and more concerned by various countries in the world along with the continuous and deep research on the functional components of the soybean. The hilum of soybean, also known as the germ, is an important component of soybean seeds. The soybean germ contains 28% protein, 8.7% fat (containing unsaturated fatty acid up to 80%, such as linoleic acid, linolenic acid and oleic acid), large amount of vitamin E, 1.4-1.76% soybean isoflavone and 0.4% sterol. The isoflavone content in the soybean cotyledon is 0.15-0.32%, and the isoflavone content in the seed coat is 0.01-0.02%, so the isoflavone in the soybean is mainly enriched in the germ. The germ can be used to produce soy isoflavones.

The inventor finds that the soybean isoflavone has common basic structures of all components, and the differences of the structures and the properties of all the components are small, so that the soybean isoflavone seems to coexist symbiotically and is difficult to separate. And the oil in the soybean umbilicus is more in variety and is not easy to separate from the soybean isoflavone with weak polarity. The primary extraction methods reported in the literature mainly include an alkali extraction and acid precipitation method, an organic solvent extraction method and a carbon dioxide supercritical extraction method, and a solvent extraction method is more commonly used. The solvent extraction method adopts ethanol, methanol, acetone and weak alkaline aqueous solution as solvent, and the extract contains isoflavone components, and also contains impurities such as oil, protein, cellulose, monosaccharide and polysaccharide. In the prior art, when n-hexane or petroleum ether or 6# gasoline is used as a solvent to remove the oil in the soybean meal and the soybeans, no soybean isoflavone is detected in the extracted oil.

Disclosure of Invention

Aiming at the technical problems in the prior art, the invention aims to provide a method for preparing glycitein by taking the bean umbilicus as a raw material.

In order to solve the technical problems, the technical scheme of the invention is as follows:

One purpose of the invention is to provide a method for preparing glycitein by taking bean umbilicus as a raw material, which comprises the following steps:

Extracting 80-100 mesh bean navel powder in 55-65% ethanol for 45-60min, adding ethanol solution with volume of 500-600ml into per 100g bean navel powder to obtain extractive solution, and evaporating to dry to obtain dry residue;

Adding n-hexane into the dry residue, extracting, and removing the n-hexane supernatant to obtain residue;

Adding ethyl acetate into the residue, extracting, centrifuging to obtain supernatant, and evaporating the supernatant to dryness to obtain glycitein.

The inventors have unexpectedly found in experiments that when soy navel flour is extracted with 55-65% (volume fraction) ethanol for 45-60min, a single ingredient isoflavone-glycitein can be extracted, and if the concentration of ethanol deviates from this range (less than or greater than this range) or the volume of ethanol deviates from this range (less than or greater than this range) or the extraction time deviates from this range (less than or greater than this range), the extract is an isoflavone complex rather than a single ingredient isoflavone-glycitein.

Because the extract contains partial grease, salt, cysteine, polypeptide and other components, the grease in the extract can be removed after n-hexane extraction, and the salt, the cysteine, the polypeptide and other components in the glycitein can be removed after ethyl acetate selective extraction, so that the pure glycitein can be obtained.

In some embodiments, 15-20ml of n-hexane is added per 100g of dry residue prepared from the hilum powder for degreasing.

The oil cannot be completely removed due to the addition of too little n-hexane, and the waste of n-hexane is easily caused when the addition of too much n-hexane is performed.

Further, the extraction time is 10-20min after adding n-hexane.

Further, after the system after n-hexane extraction is subjected to centrifugal separation, n-hexane supernatant is discarded, the centrifugal rotation speed is 1000-1500r/min, and the centrifugal time is 5-10 min. The separation of the n-hexane supernatant and the solid is easier to realize by centrifugal separation, and the loss of the solid is avoided when the supernatant is discarded.

In some embodiments, the time for ethyl acetate extraction is 10-20 min.

The second purpose of the invention is to provide a second method for preparing glycitein by taking the bean umbilicus as a raw material, which comprises the following steps:

adding n-hexane into the bean navel powder, stirring and extracting to obtain an extracting solution, and evaporating the extracting solution to dryness to obtain bean navel oil;

Adding anhydrous ethanol into the Sophora umbilicalis oil at a volume ratio of the anhydrous ethanol to the Sophora umbilicalis oil of 9-15:1, extracting for 0.5-1h, standing for layering, collecting the upper layer solution, and steaming to obtain paste;

Adding anhydrous ethanol into the paste for extraction, taking supernatant, and evaporating the supernatant to dryness to obtain glycitein.

Before extracting the hilum powder by using normal hexane, in order to verify the prior art, the inventor adopts normal hexane or petroleum ether or No. 6 gasoline to extract soybean meal, soybeans and soybean oil residues, and detects that no soybean isoflavone exists in an extracting solution. The inventor tries to extract the hilum of the soybean by using n-hexane, petroleum ether or No. 6 gasoline, and unexpectedly finds that when the extraction solvent is n-hexane, the extract contains a small amount of glycitein but does not contain other isoflavone. Probably the grease in the soybean umbilicus can promote the dissolution of glycitein in normal hexane.

In order to further separate oil and fat and glycitein in the extract and prepare a pure glycitein product, the inventor carries out a series of experiments and finds that when absolute ethyl alcohol is added into the prepared glycitein oil, the volume ratio of the absolute ethyl alcohol to the glycitein oil is 9-15:1, and the extraction is carried out for 0.5-1h, the glycitein in the glycitein oil can be selectively extracted and further purified, so that the pure glycitein product can be obtained.

In some embodiments, the soybean navel powder is extracted by n-hexane for 5 to 8 times, and the amount ratio of n-hexane to soybean navel powder is: 1.5-3: 1, V/M.

Because the extraction amount of glycitein in the soybean umbilicus by n-hexane is low once, the glycitein powder needs to be repeatedly extracted to completely extract the glycitein in the soybean umbilicus powder as much as possible, and when the dosage ratio of the n-hexane to the glycitein powder extracted each time is as follows: 1.5-3: 1, V/M, the glycitein in the soybean umbilicus can be selectively extracted, and tests show that the selective extraction of glycitein is not facilitated when the n-hexane content is too large or too small.

Further, the extraction time of the bean navel powder by n-hexane is 1-1.5h each time, and the extraction temperature is 15-30 ℃.

In some embodiments, the volume ratio of the soy navel oil to the absolute ethanol added thereto is 1: 8-12.

in some embodiments, the mass ratio of the paste to absolute ethyl alcohol is 100 times.

The beneficial technical effects of the invention are as follows:

The inventor unexpectedly finds that when the soybean navel powder is extracted by a specific process (ethanol extraction with specific concentration, normal hexane degreasing, ethyl acetate impurity removal, or normal hexane extraction with specific volume ratio and absolute ethanol impurity removal), isoflavone, glycitein, with a single component can be extracted, and a pure glycitein product is obtained after degreasing and impurity removal. The method is simple, rapid, low in cost and suitable for industrial production.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.

FIG. 1 is a thin layer separation 3D scan of glycitin, genistin and daidzin;

FIG. 2 is a scanning peak diagram of the thin layer development of the product prepared in example 1.

FIG. 3 is a plot of the thin-layer spread scan peaks of a glycitein standard solution.

Detailed Description

It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 application belongs.

It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.