阅读说明：本技术 一种基于胭脂树树叶的维生素e的制备方法 (Preparation method of vitamin E based on annatto leaves ) 是由 徐晨耀 胡成伟 王建明 张�浩 *** 于 2020-07-22 设计创作，主要内容包括：本发明公开了一种基于胭脂树树叶的维生素E的制备方法,步骤1,将胭脂树树叶放入蒸馏水中清洗干净,并晾干,切丝得到胭脂树叶丝；步骤2,将胭脂树叶丝加入至饱和盐水中浸泡10-20min,然后恒温微波反应10-20min,过滤后晾干得到干燥的胭脂树叶丝；步骤3,将干燥的胭脂树叶丝加入至乙醇水溶液中恒温微波处理2-4h,提取得到醇提液；步骤4,将醇提液加入至离子交换树脂内以无水乙醇为溶剂洗杂,并在在无水乙醇中解析,并负压浓缩得到浓缩液；步骤5,将浓缩液进行脱色和硅胶吸附处理,达到维生素E的富集纯化,得到维生素E。本发明解决了现有胭脂树树叶的提取量低的问题,利用盐水与微波反应相结合,提升盐水渗透性,实现细胞的内外失水,降低细胞保水性。(The invention discloses a preparation method of vitamin E based on annatto leaves, which comprises the following steps of 1, putting the annatto leaves into distilled water, cleaning, airing and shredding to obtain annatto leaf shreds; step 2, adding the annatto leaf shreds into saturated saline water, soaking for 10-20min, then carrying out constant-temperature microwave reaction for 10-20min, filtering and airing to obtain dried annatto leaf shreds; step 3, adding the dried annatto leaves into an ethanol water solution, carrying out constant-temperature microwave treatment for 2-4h, and extracting to obtain an alcohol extract; step 4, adding the alcohol extract into ion exchange resin, washing impurities by using absolute ethyl alcohol as a solvent, resolving in the absolute ethyl alcohol, and concentrating under negative pressure to obtain a concentrated solution; and 5, decoloring the concentrated solution and adsorbing the concentrated solution by silica gel to enrich and purify the vitamin E to obtain the vitamin E. The method solves the problem of low extraction amount of the conventional annatto leaves, improves the permeability of saline water by combining the saline water with microwave reaction, realizes water loss inside and outside cells, and reduces the water retention of the cells.)

1. A preparation method of vitamin E based on annatto leaves is characterized by comprising the following steps: the method comprises the following steps:

step 1, putting annatto leaves into distilled water, cleaning, airing and shredding to obtain annatto leaf shreds;

step 2, adding the annatto leaf shreds into saturated saline water, soaking for 10-20min, then carrying out constant-temperature microwave reaction for 10-20min, filtering and airing to obtain dried annatto leaf shreds;

step 3, adding the dried annatto leaves into an ethanol water solution, carrying out constant-temperature microwave treatment for 2-4h, and extracting to obtain an alcohol extract;

step 4, adding the alcohol extract into ion exchange resin, washing impurities by using absolute ethyl alcohol as a solvent, resolving in the absolute ethyl alcohol, and concentrating under negative pressure to obtain a concentrated solution;

and 5, decoloring the concentrated solution and adsorbing the concentrated solution by silica gel to enrich and purify the vitamin E, wherein in the decoloring process, petroleum ether is used as a dissolved solution, and activated clay and activated carbon are sequentially added to decolor at room temperature.

2. The method of claim 1, wherein the vitamin E is derived from annatto leaves, and comprises: the temperature of the constant temperature microwave reaction in the step 2 is 10-20 ℃, and the microwave power is 100-300W.

3. The method of claim 2, wherein the vitamin E is derived from annatto leaves, and comprises: and 1-3% by mass of citric acid is added into the saturated saline water.

4. The method of claim 1, wherein the vitamin E is derived from annatto leaves, and comprises: the volume concentration of the water in the ethanol water solution in the step 3 is 10-20%, the temperature of the constant-temperature microwave treatment is 20-30 ℃, and the microwave power is 300-500W.

5. The method of claim 4, wherein the vitamin E is derived from annatto leaves, and comprises: the constant temperature microwave treatment adopts gap type microwave treatment, the single microwave reaction time is 40-60s, and the gap time is 20-50 s.

6. The method of claim 1, wherein the vitamin E is derived from annatto leaves, and comprises: and (3) removing water by sepiolite before the alcohol extract in the step (4) enters ion exchange.

7. The method of claim 6, wherein the vitamin E is derived from annatto leaves, and comprises: the absolute ethyl alcohol analysis is carried out under an acidic condition, the acidic regulator is boric acid, and the pH value is regulated to be 3-5.

8. The method of claim 6, wherein the vitamin E is derived from annatto leaves, and comprises: the negative pressure concentration pressure is 60-70% of the standard atmospheric pressure, and the temperature is 60-70 ℃.

9. The method of claim 1, wherein the vitamin E is derived from annatto leaves, and comprises: the silica gel is 100-200 meshes, a petroleum ether-ethyl acetate system is adopted for silica gel adsorption, the volume ratio of the petroleum ether-ethyl acetate system is 4-10:1, and the silica gel is resolved and concentrated in the graphene-ethyl acetate system after adsorption.

Technical Field

The invention belongs to the field of extraction, and particularly relates to a preparation method of vitamin E based on annatto leaves.

Background

The natural vitamin E has unique physiological functions, such as free radical resistance, aging resistance, skin keratinization prevention, physical and cellular immune function improvement of human bodies and animals, cardiovascular and cerebrovascular disease prevention and treatment, reproductive function maintenance and enhancement and other important physiological functions. The performance of the vitamin E is far better than that of the synthetic vitamin E, and the vitamin E is widely applied to industries of cosmetics, foods and the like. At present, natural vitamin E comes from soybean oil residue, sunflower seed oil residue and the like, is mostly tocopherol and has transgenic risk. Thus, there is a need to develop new plant sources of natural vitamin E.

With the development of the technology and the deepening of scientific research, the annatto is used as a new plant source of the vitamin E and enters the sight of researchers, and the annatto can provide less tocotrienols in the market; however, in the actual production process, the residue after the annatto extraction process still contains a lot of tocotrienols, which causes resource waste.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation method of vitamin E based on annatto leaves, which solves the problem of low extraction amount of the conventional annatto leaves, and improves the permeability of saline water by combining the saline water with microwave reaction, realizes the internal and external dehydration of cells, and reduces the water retention of the cells.

In order to achieve the technical purpose, the technical scheme of the invention is as follows:

a preparation method of vitamin E based on annatto leaves comprises the following steps:

step 1, putting annatto leaves into distilled water, cleaning, airing and shredding to obtain annatto leaf shreds;

step 2, adding the annatto leaf shreds into saturated saline water, soaking for 10-20min, then carrying out constant-temperature microwave reaction for 10-20min, filtering and airing to obtain dried annatto leaf shreds; the temperature of the constant-temperature microwave reaction is 10-20 ℃, the microwave power is 100-;

step 3, adding the dried annatto leaves into an ethanol water solution, carrying out constant-temperature microwave treatment for 2-4h, and extracting to obtain an alcohol extract; the volume concentration of water in the ethanol water solution is 10-20%, the temperature of constant-temperature microwave treatment is 20-30 ℃, the microwave power is 300-; the closed cell wall can be slightly opened by the distilled water in the ethanol water, the ethanol can quickly permeate into the cell wall, and the substance components inside and outside the cell can be quickly extracted by utilizing the solubility of the ethanol, so that the extraction amount can be greatly increased, and the vitamin E content in the residue can be reduced;

step 4, adding the alcohol extract into ion exchange resin, washing impurities by using absolute ethyl alcohol as a solvent, resolving in the absolute ethyl alcohol, concentrating under negative pressure to obtain a concentrated solution, and removing water by using sepiolite before the alcohol extract enters ion exchange; the absolute ethyl alcohol is analyzed under an acidic condition, the acidic regulator is boric acid, the pH value is regulated to be 3-5, the pressure of negative pressure concentration is 60-70% of standard atmospheric pressure, and the temperature is 60-70 ℃;

step 5, carrying out decolorization and silica gel adsorption treatment on the concentrated solution to achieve enrichment and purification of vitamin E, wherein in the decolorization process, petroleum ether is used as a dissolved solution, and activated clay and activated carbon are sequentially added to carry out decolorization at room temperature; the silica gel is 100-200 meshes, a petroleum ether-ethyl acetate system is adopted for silica gel adsorption, the volume ratio of the petroleum ether-ethyl acetate system is 4-10:1, and the silica gel is resolved and concentrated in the graphene-ethyl acetate system after adsorption.

From the above description, it can be seen that the present invention has the following advantages:

1. the method solves the problem of low extraction amount of the conventional annatto leaves, improves the permeability of saline water by combining the saline water with microwave reaction, realizes water loss inside and outside cells, and reduces the water retention of the cells.

2. The invention uses ethanol water as ethanol extract, and increases ethanol coverage on the surface of cells sealed by water loss by matching with microwave reaction, thereby improving the ethanol extraction effect.

Detailed Description

A specific embodiment of the present invention will be described in detail with reference to examples, but the present invention is not limited to the claims.