阅读说明：本技术 一种利用芝麻粕制备芝麻素的方法 (Method for preparing sesamin by using sesame seed meal ) 是由 马友水 李丹 马家山 何述栋 孙汉巨 于 2021-09-18 设计创作，主要内容包括：一种利用芝麻粕制备高纯度芝麻素的方法,其包括以下技术步骤。(1)芝麻粕粉碎处理、(2)芝麻粕乳化处理、(3)复合酶解、(4)第一次离心、(5)第二次离心、(6)真空干燥和(7)超临界萃取。本发明采用不同芝麻油生产批次的芝麻粕为原料,平行5组试验提取芝麻素,经过检测和计算,萃取产物中芝麻素含量可达约25-37%；芝麻粕的芝麻素提取率约为0.10-0.12%。(A method for preparing high-purity sesamin by using sesame meal comprises the following technical steps. (1) Crushing sesame seed meal, (2) emulsifying the sesame seed meal, (3) performing compound enzymolysis, (4) performing primary centrifugation, (5) performing secondary centrifugation, (6) performing vacuum drying and (7) performing supercritical extraction. According to the invention, sesame seed meal of different sesame oil production batches is used as a raw material, sesamin is extracted in parallel with 5 groups of experiments, and the content of the sesamin in an extraction product can reach about 25-37% through detection and calculation; the sesamin extraction rate of the sesame seed meal is about 0.10-0.12%.)

1. A method for preparing sesamin by using sesame meal is characterized by comprising the following steps: comprises the following steps:

step 1: crushing sesame seed meal to the fineness of more than or equal to 100 meshes;

step 2: mixing the crushed sesame seed meal obtained in the step 1 with purified water according to the mass ratio of 1: 4-6, and then preparing into emulsion;

and step 3: adding cellulase and neutral protease into the emulsion, performing enzymolysis for 2.5-3.5h under the conditions of pH value of 6.5-8.0, temperature of 40-45 ℃ and stirring speed of 15-30r/min, and collecting enzymolysis liquid;

and 4, step 4: centrifuging the enzymolysis solution at 7500-10000 r/min for 15-30min, and collecting the uppermost layer oily substance;

and 5: mixing the collected oily substance with purified water according to the mass ratio of 1: 3-5, stirring and mixing uniformly, centrifuging at the rotating speed of 5000-;

step 6: drying the oily substance in vacuum, and collecting the dried material;

and 7: placing the dried material into an extraction kettle of a carbon dioxide supercritical extraction device, wherein the extraction pressure is 28-30MPa, the extraction temperature is 50-53 ℃, and the extraction time is 45-60 min; collecting the extracted product.

2. The method for preparing sesamin from sesame seed meal according to claim 1, wherein: and (3) mixing the crushed sesame seed meal obtained in the step (1) with purified water, putting the mixture into emulsification equipment, treating the mixture for 15-30min at the rotation speed of 8000-.

3. The method for preparing sesamin from sesame seed meal according to claim 2, wherein: adding ice blocks with the mass of 2-4% into the purified water.

4. The method for preparing sesamin from sesame seed meal according to claim 1, wherein: the enzyme activity of the cellulase is 5-20 ten thousand U, and the addition amount of the cellulase is 0.15-0.25% of the mass of the sesame seed meal; the enzyme activity of the neutral protease is 5-20 ten thousand U, and the addition amount of the neutral protease is 0.50-0.75% of the mass of the sesame seed meal.

5. The method for preparing sesamin from sesame seed meal according to claim 1, wherein: the process conditions of vacuum drying are as follows: the vacuum gauge pressure is-0.09 to-0.10 MPa, the temperature is 55 to 65 ℃, and the vacuum drying time is 45 to 90 min.

Technical Field

The invention belongs to the technical field of deep processing of agricultural products, and relates to a method for preparing sesamin by using sesame seed meal.

Background

Sesame, also known as flax or flax (the scientific name: Sesamum indicum), is a seed of the annual upright herbaceous plant flax. Sesame has an oil content of 55% and is an important edible oil source in China, and the squeezed oil is called sesame oil, linseed oil and sesame oil and is characterized by mellow smell and high nutritional value. The sesame seed meal is a byproduct after oil extraction of sesame, and mainly contains sesame protein, residual oil, lignans and the like.

Sesamin is one of sesame lignin substances, is a white needle crystal, has a melting point of 120-121 ℃, is easily soluble in chloroform, benzene, acetic acid and acetone, is slightly soluble in diethyl ether and petroleum ether, and is almost insoluble in water. Sesamin has strong antioxidation effect in vivo, and has multiple physiological activity functions. Clinical researches find that sesamin has the effects of resisting hypertension and cardiovascular diseases, protecting liver, resisting oxidation, reducing cholesterol and the like, and is specifically represented as follows: (1) the sesamin can protect the liver by promoting ethanol metabolism and accelerating fatty acid oxidation, and helps the body to remove toxins; (2) antioxidation, sesamin can eliminate organic free radicals and hydroxyl free radicals in vivo; (3) sesamin has effects in inhibiting influenza virus, Sendai virus, and tubercle bacillus. Therefore, the sesamin has wide application prospect in the fields of medicine raw materials, health-care food, cosmetics, food additives, feeds, plant-derived pesticides and the like.

Disclosure of Invention

The invention aims to provide a method for preparing sesamin by using sesame meal.

In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a method for preparing sesamin from sesame seed meal comprises the following steps:

step 1: crushing sesame seed meal to the fineness of more than or equal to 100 meshes;

step 2: mixing the crushed sesame seed meal obtained in the step 1 with purified water according to the mass ratio of 1: 4-6, and then preparing into emulsion;

and step 3: adding cellulase and neutral protease into the emulsion, performing enzymolysis for 2.5-3.5h under the conditions of pH value of 6.5-8.0, temperature of 40-45 ℃ and stirring speed of 15-30r/min, and collecting enzymolysis liquid;

and 4, step 4: centrifuging the enzymolysis solution at 7500-10000 r/min for 15-30min, and collecting the uppermost layer oily substance;

and 5: mixing the collected oily substance with purified water according to the mass ratio of 1: 3-5, stirring and mixing uniformly, centrifuging at the rotating speed of 5000-;

step 6: drying the oily substance in vacuum, and collecting the dried material;

and 7: placing the dried material into an extraction kettle of a carbon dioxide supercritical extraction device, wherein the extraction pressure is 28-30MPa, the extraction temperature is 50-53 ℃, and the extraction time is 45-60 min; collecting the extracted product.

The preferable technical scheme is as follows: and (3) mixing the crushed sesame seed meal obtained in the step (1) with purified water, putting the mixture into emulsification equipment, treating the mixture for 15-30min at the rotation speed of 8000-.

The preferable technical scheme is as follows: adding ice blocks with the mass of 2-4% into the purified water.

The preferable technical scheme is as follows: the enzyme activity of the cellulase is 5-20 ten thousand U, and the addition amount of the cellulase is 0.15-0.25% of the mass of the sesame seed meal; the enzyme activity of the neutral protease is 5-20 ten thousand U, and the addition amount of the neutral protease is 0.50-0.75% of the mass of the sesame seed meal.

The preferable technical scheme is as follows: the process conditions of vacuum drying are as follows: the vacuum gauge pressure is-0.09 to-0.10 MPa, the temperature is 55 to 65 ℃, and the vacuum drying time is 45 to 90 min.

Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:

according to the invention, sesame seed meal of different sesame oil production batches is used as a raw material, sesamin is extracted in parallel with 5 groups of experiments, and the content of the sesamin in an extraction product can reach about 25-37% through detection and calculation; the sesamin extraction rate of the sesame seed meal is about 0.10-0.12%.

Detailed Description

The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.

Detecting the sesamin content in the extracted product: the detection method is GB/T31579-2015 grain and oil inspection-determination of sesamin and sesamolin in sesame oil-high performance liquid chromatography.

Example 1: method for preparing sesamin by using sesame seed meal

A method for preparing sesamin from sesame seed meal comprises the following steps:

step 1: crushing sesame seed meal to the fineness of more than or equal to 100 meshes; the sesame seed meal raw material is a byproduct of cold pressing sesame oil at low temperature.

Step 2: mixing the crushed sesame seed meal obtained in the step 1 with purified water according to the mass ratio of 1:5, and then preparing into emulsion;

and step 3: adding cellulase and neutral protease into the emulsion, performing enzymolysis for 3h under the conditions of pH value of 7.2, temperature of 42 ℃ and stirring speed of 20r/min, and collecting enzymolysis liquid;

and 4, step 4: centrifuging the enzymolysis solution at 9000 r/min for 20min, and collecting the uppermost layer oily substance;

and 5: mixing the collected oily substance with purified water according to the mass ratio of 1:4, stirring and mixing uniformly, centrifuging at the rotating speed of 5500 r/min for 13min, and collecting the upper oily substance;

step 6: drying the oily substance in vacuum, and collecting the dried material;

and 7: putting the dried material into an extraction kettle of carbon dioxide supercritical extraction equipment, and extracting at the extraction temperature of 51 ℃ for 50min under the extraction pressure of 29 MPa; collecting the extracted product.

The preferred embodiment is: and (3) mixing the crushed sesame seed meal obtained in the step (1) with purified water, putting the mixture into emulsification equipment, treating the mixture for 20min at a rotation speed of 10000r/min until the mixture is in an emulsified state, and collecting the mixture to obtain an emulsion.

The preferred embodiment is: ice cubes in an amount of 3% by mass were added to the purified water.

The preferred embodiment is: the enzyme activity of the cellulase is 10 ten thousand U, and the addition amount of the cellulase is 0.12 percent of the mass of the sesame seed meal; the enzyme activity of the neutral protease is 10 ten thousand U, and the addition amount of the neutral protease is 0.65 percent of the mass of the sesame seed meal.

The preferred embodiment is: the process conditions of vacuum drying are as follows: the vacuum gauge pressure is-0.095 MPa, the temperature is 60 ℃, and the vacuum drying time is 70 min.

Sesamin is extracted, and the content of the sesamin in the extracted product can reach 35.6 percent through detection and calculation; the sesamin extraction rate of the sesame seed meal is 0.12%.

Example 2: method for preparing sesamin by using sesame seed meal

A method for preparing sesamin from sesame seed meal comprises the following steps:

step 1: crushing sesame seed meal to the fineness of more than or equal to 100 meshes; the sesame seed meal is a byproduct of peeled black sesame after oil pressing.

Step 2: mixing the crushed sesame seed meal obtained in the step 1 with purified water according to the mass ratio of 1:4, and then preparing into emulsion;

and step 3: adding cellulase and neutral protease into the emulsion, performing enzymolysis for 2.5h under the conditions of pH value of 6.5, temperature of 40 ℃ and stirring speed of 15r/min, and collecting enzymolysis liquid;

and 4, step 4: centrifuging the enzymolysis solution at 7500r/min for 15min, and collecting the uppermost layer oily substance;

and 5: mixing the collected oily substance with purified water according to the mass ratio of 1: 3, stirring and mixing uniformly, centrifuging at the rotating speed of 5000r/min for 10min, and collecting the upper-layer oily substance;

step 6: drying the oily substance in vacuum, and collecting the dried material;

and 7: putting the dried material into an extraction kettle of carbon dioxide supercritical extraction equipment, and extracting for 45min at the extraction pressure of 28MPa and the extraction temperature of 50 ℃; collecting the extracted product.

The preferred embodiment is: and (3) mixing the crushed sesame seed meal obtained in the step (1) with purified water, putting the mixture into emulsification equipment, treating the mixture for 15min at a rotating speed of 8000r/min until the mixture is in an emulsified state, and collecting the mixture to obtain an emulsion.

The preferred embodiment is: ice cubes of 2% of its mass were added to the purified water.

The preferred embodiment is: the enzyme activity of the cellulase is 5 ten thousand U, and the addition amount of the cellulase is 0.25 percent of the mass of the sesame seed meal; the enzyme activity of the neutral protease is 5 ten thousand U U, and the addition amount of the neutral protease is 0.75 percent of the mass of the sesame seed meal.

The preferred embodiment is: the process conditions of vacuum drying are as follows: the vacuum gauge pressure is-0.09 MPa, the temperature is 55 ℃, and the vacuum drying time is 45 min.

Sesamin is extracted, and the content of the sesamin in the extracted product can reach 28.3 percent through detection and calculation; the sesamin extraction rate of the sesame seed meal is about 0.10%.

Example 3: method for preparing sesamin by using sesame seed meal

A method for preparing sesamin from sesame seed meal comprises the following steps:

step 1: crushing sesame seed meal to the fineness of more than or equal to 100 meshes;

step 2: mixing the crushed sesame seed meal obtained in the step 1 with purified water according to the mass ratio of 1: 6, and then preparing into emulsion;

and step 3: adding cellulase and neutral protease into the emulsion, performing enzymolysis for 3.5h under the conditions of pH value of 8.0, temperature of 40-45 ℃ and stirring speed of 30r/min, and collecting enzymolysis liquid;

and 4, step 4: centrifuging the enzymolysis solution at 10000r/min for 30min, and collecting the uppermost layer oily substance;

and 5: mixing the collected oily substance with purified water according to the mass ratio of 1:5, stirring and mixing uniformly, centrifuging at the rotating speed of 6000 r/min for 15min, and collecting the upper-layer oily substance;

step 6: drying the oily substance in vacuum, and collecting the dried material;

and 7: putting the dried material into an extraction kettle of carbon dioxide supercritical extraction equipment, and extracting for 60min at the extraction pressure of 30MPa and the extraction temperature of 53 ℃; collecting the extracted product.

The preferred embodiment is: and (3) mixing the crushed sesame seed meal obtained in the step (1) with purified water, putting the mixture into emulsification equipment, treating the mixture for 30min at a rotating speed of 12000r/min until the mixture is in an emulsified state, and collecting the mixture to obtain an emulsion.

The preferred embodiment is: ice cubes in an amount of 4% by mass were added to the purified water.

The preferred embodiment is: the enzyme activity of the cellulase is 20 ten thousand U, and the addition amount of the cellulase is 0.15 percent of the mass of the sesame seed meal; the enzyme activity of the neutral protease is 20 ten thousand U, and the addition amount of the neutral protease is 0.50 percent of the mass of the sesame seed meal.

The preferred embodiment is: the process conditions of vacuum drying are as follows: the vacuum gauge pressure is-0.10 MPa, the temperature is 65 ℃, and the vacuum drying time is 90 min.

The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.