阅读说明：本技术 一种提取芝麻中有效成分的方法 (Method for extracting effective components from sesame ) 是由 赵永强 张树元 白高娃 徐旭 高瑞 张野 于 2021-08-16 设计创作，主要内容包括：本发明涉及一种提取芝麻中有效成分的方法。本发明方法通过提取、过滤、浓缩、模拟移动床进行分离、结晶、重结晶、离心、干燥等步骤,实现了芝麻中有效成分的分离,整套工艺可实现连续化操作,最终产物有效成分含量高、收率高,适合规模化生产。(The invention relates to a method for extracting effective components from sesame. The method realizes the separation of the effective components in the sesame through the steps of extraction, filtration, concentration, separation by a simulated moving bed, crystallization, recrystallization, centrifugation, drying and the like, the whole process can realize continuous operation, and the final product has high content of the effective components and high yield and is suitable for large-scale production.)

1. A method for extracting effective components from sesame seeds is characterized by comprising the following steps:

step S10, adding sesame into extraction equipment, adding ethanol, specifically mixing the sesame and 80% ethanol according to the mass volume ratio (kg: L) of 1 (1-3), and treating for 1-4 hours to obtain an initial extraction solution;

s20, filtering the primary extraction liquid, specifically, performing pressure filtration on the primary extraction liquid by using a plate-and-frame filter press, wherein the plate-and-frame filter is filtered by adopting non-woven fabrics, and the aperture size is 240 meshes and 320 meshes to obtain a filtrate;

step S30, concentrating the filtrate to obtain a concentrated solution;

step S40, separating the concentrated solution by using a simulated moving bed to obtain a separated solution;

step S50, transferring the separated liquid into a crystallizing tank for crystallization treatment, specifically transferring the separated liquid into the crystallizing tank, wherein the crystallization temperature is 5-20 ℃, and the crystallization time is 16-32 hours, so as to obtain a crude product;

s60, transferring the crude product into a crystallizing tank for recrystallization, specifically transferring the crude product into the crystallizing tank, dissolving the crude product by using mixed alcohol, adding sesamin seed crystal, and crystallizing at the temperature of 5-10 ℃ for 24-36 hours to obtain a refined product;

and step S70, performing centrifugal separation on the refined product, and drying to obtain the sesame extract.

2. The method according to claim 1, wherein step S10 includes:

step S11, a first-stage extraction step, namely transferring sesame and ethanol into first extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:2, adjusting the pH value to 5.5-6.5 by using glacial acetic acid, and processing for 1 hour to obtain an extracting solution;

adding ethanol into the first extraction equipment while producing the extracting solution, adjusting the pH value of the ethanol to 5.5-6.5 by using glacial acetic acid, adjusting the mass-to-volume ratio (kg: L) of the added sesame to the ethanol to be 1:1, treating the produced solution for 3 hours, and keeping the speed of producing the extracting solution and the speed of adding the ethanol of the first extraction equipment equal to each other to achieve the dynamic balance of the liquid in the first extraction equipment;

the first extraction equipment completes the output of the extracting solution to obtain a first-stage extracting solution;

step S12, a second-stage extraction step, namely adding ethanol into first extraction equipment, mixing sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and processing for 0.5 hour, wherein the first extraction equipment starts to produce an extracting solution to second extraction equipment;

after the first extraction equipment finishes the production of the extracting solution, adding ethanol into the first extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and treating for 0.5 hour; adding sesame into second extraction equipment, wherein the adding amount of the sesame is equal to that of the first extraction equipment, extracting by using the output liquid of the first extraction equipment, and treating for 0.5 hour;

the first extraction equipment and the second extraction equipment simultaneously produce extracting solution, and the specific extracting solution producing mode is that ethanol is added into the first extraction equipment while the first extraction equipment produces the extracting solution, the pH value of the ethanol is adjusted to 4.5-5.5 by using glacial acetic acid, and the mass-to-volume ratio (kg: L) of the added sesame to the ethanol is 1: 1;

the first extraction equipment outputs the extracting solution to the second extraction equipment, the produced solution is treated for 3 hours, the speed of the extracting solution output by the second extraction equipment is kept equal to the speed of the ethanol added by the first extraction equipment, and the dynamic balance of the liquid in the first extraction equipment and the second extraction equipment is achieved;

the second extraction equipment completes the output of the extracting solution to obtain a second-level extracting solution;

the first extraction equipment carries out deslagging treatment and discharges sesame in the equipment;

step S13, a third-stage extraction step, namely adding ethanol into second extraction equipment, mixing sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, treating for 0.5 hour, and enabling the second extraction equipment to start to produce an extracting solution to third extraction equipment;

after the second extraction equipment finishes the production of the extracting solution, adding ethanol into the second extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and treating for 0.5 hour; adding sesame into third extraction equipment, wherein the adding amount of the sesame is equal to that of the second extraction equipment, extracting by using the output liquid of the second extraction equipment, and treating for 0.5 hour;

the second extraction equipment and the third extraction equipment simultaneously produce extracting solution, and the specific extracting solution producing mode is that ethanol is added into the second extraction equipment while the second extraction equipment produces the extracting solution, the pH value of the ethanol is adjusted to 4.5-5.5 by using glacial acetic acid, and the mass-to-volume ratio (kg: L) of the added sesame to the ethanol is 1: 1;

the second extraction equipment outputs the extracting solution to the third extraction equipment, the produced solution is treated for 3 hours, the speed of the extracting solution output by the third extraction equipment is kept equal to the speed of the ethanol added by the second extraction equipment, and the dynamic balance of the liquid in the second extraction equipment and the third extraction equipment is achieved;

the third extraction equipment completes the output of the extracting solution to obtain a third-level extracting solution;

the second extraction equipment carries out deslagging treatment and discharges the sesame in the equipment;

and step S14, mixing the primary extract, the secondary extract and the tertiary extract to obtain an initial extract.

3. The method of claim 2, wherein the extraction temperature of the steps S11, S12, S13 is 78-82 ℃.

4. The method according to claim 1, wherein step S40 includes: the adsorbent filled by the simulated moving bed chromatography is modified ion exchange resin, preferably any one of AB-8 macroporous adsorption resin, D-101 macroporous adsorption resin, HPD-700 macroporous adsorption resin and LSA-10 macroporous adsorption resin; the desorbent is 40-90% ethanol solution, and the dosage of the desorbent is 2-4 times of the volume of the resin; the water washing area is purified water; the resin adsorption regeneration solvent is 95% ethanol or 2-4% sodium hydroxide aqueous solution; the flow speed of the adsorption area is 1-3 BV/h; the flow speed of the desorption area is 1-3 BV/h; the flow rate of the water washing area is 1-3 BV/h; the flow rate of the regeneration area is 2-3 BV/h; controlling the temperature at 40-60 ℃; the pressure is controlled between 0.2MPa and 0.5 MPa.

5. The method according to claim 1, wherein step S60 includes: transferring the crude product into a crystallizing tank, dissolving by using methanol-ethanol mixed alcohol, wherein the concentration of the methanol and the ethanol is 95%, the volume ratio of the methanol to the ethanol is 1 (1-9), heating and dissolving the crude product and the mixed alcohol according to the mass-volume ratio (kg: L) of 1 (4-8), naturally cooling to 5-10 ℃ after complete dissolution, adjusting the pH value to 2-4 by using glacial acetic acid, adding seed crystals, stirring for 15 minutes every 1-3 hours, and separating the mixture liquid after 24-36 hours to obtain the fine product.

6. The method according to claim 1, wherein the sesame extract has an effective ingredient purity of 99% or more, and comprises: 70-90% sesamin and 10-30% (+) -episesamin.

Technical Field

The invention relates to a method for extracting effective components from sesame.

Background

Sesame, also known as Sesamum indicum and flax (the scientific name: Sesamum indicum), is a seed of flax, an annual upright herb, 60-150 cm high. It is distributed throughout tropical regions and parts of the temperate regions of the world. Sesame is one of the main oil crops in China, and has high application value. Its seed oil content is up to 55%.

The sesame has the effects of tonifying liver and kidney, benefiting essence and blood, moistening intestine and dryness and promoting lactation. Can be used for treating asthenia, dizziness, tinnitus, hypertension, hyperlipidemia, cough, asthenia, premature gray hair, anemia, body fluid deficiency, constipation, oliguria, hematuria, etc. The main active substance in sesame is sesame lignan, the sesame lignan content in sesame varies according to different sesame, and the sesame lignan mainly comprises: sesamin, episesamin, sesamol, sesamolin, etc. The sesamol has strong antioxidant activity, and especially sesamol has strong physiological activity.

Sesamin is a white crystalline solid with the molecular formula: c₂₀H₁₈O₆Molecular weight: 354.3533 the natural sesamin is dextrorotatory, insoluble in water, alkaline solution and hydrochloric acid, insoluble in kerosene, and soluble in benzene, acetone, chloroform and acetic acid.

(+) -episesamin, alternative name: (+) -isosesamin, epoxysesamin (P), (+) -epimesesamin, formula: c₂₀H₁₈O₆Molecular weight: 354.3533, and is miscible with acetic acid, acetone, chloroform, and benzene. (+) -episesamin belongs to isomers with sesamin.

Sesamol, also known as 3, 4-methylenedioxyphenol, a fat-soluble lignan compound, is an important aroma component of sesame oil and also an important quality stabilizer of the sesame oil.

Sesamolin, molecular formula: c₂₀H₁₈O₇Molecular weight: 370.3527 has effects in scavenging free radicals, and reducing cholesterol in blood serum.

Disclosure of Invention

In order to establish a set of process which can realize continuous operation, has high content of active ingredients in the final product and high yield and is suitable for large-scale production, the invention completes the following contents.

The method specifically comprises the following steps:

step S10, adding sesame into extraction equipment, adding ethanol, specifically mixing the sesame and 80% ethanol according to the mass volume ratio (kg: L) of 1 (1-3), and treating for 1-4 hours to obtain an initial extraction solution;

s20, filtering the primary extraction liquid, specifically, performing pressure filtration on the primary extraction liquid by using a plate-and-frame filter press, wherein the plate-and-frame filter is filtered by adopting non-woven fabrics, and the aperture size is 240 meshes and 320 meshes to obtain a filtrate;

step S30, concentrating the filtrate to obtain a concentrated solution;

step S40, separating the concentrated solution by using a simulated moving bed to obtain a separated solution;

step S50, transferring the separated liquid into a crystallizing tank for crystallization treatment, specifically transferring the separated liquid into the crystallizing tank, wherein the crystallization temperature is 5-20 ℃, and the crystallization time is 16-32 hours, so as to obtain a crude product;

s60, transferring the crude product into a crystallizing tank for recrystallization, specifically transferring the crude product into the crystallizing tank, dissolving the crude product by using mixed alcohol, adding sesamin seed crystal, and crystallizing at the temperature of 5-10 ℃ for 24-36 hours to obtain a refined product;

and step S70, performing centrifugal separation on the refined product, and drying to obtain the sesame extract.

Optionally, the step S10 includes:

step S11, a first-stage extraction step, namely transferring sesame and ethanol into first extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:2, adjusting the pH value to 5.5-6.5 by using glacial acetic acid, and processing for 1 hour to obtain an extracting solution;

adding ethanol into the first extraction equipment while producing the extracting solution, adjusting the pH value of the ethanol to 5.5-6.5 by using glacial acetic acid, adjusting the mass-to-volume ratio (kg: L) of the added sesame to the ethanol to be 1:1, treating the produced solution for 3 hours, and keeping the speed of producing the extracting solution and the speed of adding the ethanol of the first extraction equipment equal to each other to achieve the dynamic balance of the liquid in the first extraction equipment;

the first extraction equipment completes the output of the extracting solution to obtain a first-stage extracting solution;

step S12, a second-stage extraction step, namely adding ethanol into first extraction equipment, mixing sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and processing for 0.5 hour, wherein the first extraction equipment starts to produce an extracting solution to second extraction equipment;

after the first extraction equipment finishes the production of the extracting solution, adding ethanol into the first extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and treating for 0.5 hour; adding sesame into second extraction equipment, wherein the adding amount of the sesame is equal to that of the first extraction equipment, extracting by using the output liquid of the first extraction equipment, and treating for 0.5 hour;

the first extraction equipment and the second extraction equipment simultaneously produce extracting solution, and the specific extracting solution producing mode is that ethanol is added into the first extraction equipment while the first extraction equipment produces the extracting solution, the pH value of the ethanol is adjusted to 4.5-5.5 by using glacial acetic acid, and the mass-to-volume ratio (kg: L) of the added sesame to the ethanol is 1: 1;

the first extraction equipment outputs the extracting solution to the second extraction equipment, the produced solution is treated for 3 hours, the speed of the extracting solution output by the second extraction equipment is kept equal to the speed of the ethanol added by the first extraction equipment, and the dynamic balance of the liquid in the first extraction equipment and the second extraction equipment is achieved;

the second extraction equipment completes the output of the extracting solution to obtain a second-level extracting solution;

the first extraction equipment carries out deslagging treatment and discharges sesame in the equipment;

step S13, a third-stage extraction step, namely adding ethanol into second extraction equipment, mixing sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, treating for 0.5 hour, and enabling the second extraction equipment to start to produce an extracting solution to third extraction equipment;

after the second extraction equipment finishes the production of the extracting solution, adding ethanol into the second extraction equipment, mixing the sesame and the ethanol according to the mass-volume ratio (kg: L) of 1:1, adjusting the pH value to 4.5-5.5 by using glacial acetic acid, and treating for 0.5 hour; adding sesame into third extraction equipment, wherein the adding amount of the sesame is equal to that of the second extraction equipment, extracting by using the output liquid of the second extraction equipment, and treating for 0.5 hour;

the second extraction equipment and the third extraction equipment simultaneously produce extracting solution, and the specific extracting solution producing mode is that ethanol is added into the second extraction equipment while the second extraction equipment produces the extracting solution, the pH value of the ethanol is adjusted to 4.5-5.5 by using glacial acetic acid, and the mass-to-volume ratio (kg: L) of the added sesame to the ethanol is 1: 1;

the second extraction equipment outputs the extracting solution to the third extraction equipment, the produced solution is treated for 3 hours, the speed of the extracting solution output by the third extraction equipment is kept equal to the speed of the ethanol added by the second extraction equipment, and the dynamic balance of the liquid in the second extraction equipment and the third extraction equipment is achieved;

the third extraction equipment completes the output of the extracting solution to obtain a third-level extracting solution;

the second extraction equipment carries out deslagging treatment and discharges the sesame in the equipment;

and step S14, mixing the primary extract, the secondary extract and the tertiary extract to obtain an initial extract.

Optionally, the extraction temperature of the step S11, the step S12 and the step S13 is 78 ℃ to 82 ℃.

Optionally, the step S40 includes: the adsorbent filled by the simulated moving bed chromatography is modified ion exchange resin, preferably any one of AB-8 macroporous adsorption resin, D-101 macroporous adsorption resin, HPD-700 macroporous adsorption resin and LSA-10 macroporous adsorption resin; the desorbent is 40-90% ethanol solution, and the dosage of the desorbent is 2-4 times of the volume of the resin; the water washing area is purified water; the resin adsorption regeneration solvent is 95% ethanol or 2-4% sodium hydroxide aqueous solution; the flow speed of the adsorption area is 1-3 BV/h; the flow speed of the desorption area is 1-3 BV/h; the flow rate of the water washing area is 1-3 BV/h; the flow rate of the regeneration area is 2-3 BV/h; controlling the temperature at 40-60 ℃; the pressure is controlled between 0.2MPa and 0.5 MPa.

Optionally, the step S60 includes: transferring the crude product into a crystallizing tank, dissolving by using methanol-ethanol mixed alcohol, wherein the concentration of the methanol and the ethanol is 95%, the volume ratio of the methanol to the ethanol is 1 (1-9), heating and dissolving the crude product and the mixed alcohol according to the mass-volume ratio (kg: L) of 1 (4-8), naturally cooling to 5-10 ℃ after complete dissolution, adjusting the pH value to 2-4 by using glacial acetic acid, adding seed crystals, stirring for 15 minutes every 1-3 hours, and separating the mixture liquid after 24-36 hours to obtain the fine product.

Optionally, the purity of the effective components of the obtained sesame extract is more than 99%, and the obtained sesame extract comprises: 70-90% sesamin and 10-30% (+) -episesamin.

According to the method for extracting the effective components from the sesame, provided by the invention, a set of process is established, so that continuous operation can be realized, the content of the effective components in the final product is high, the yield is high, and the method is suitable for large-scale production.

Drawings

Fig. 1 is a flow chart of a method for extracting effective components from sesame according to an embodiment of the present invention.

Detailed Description

The present invention will be described in more detail with reference to the following embodiments.

Example 1

Step S10, putting 1600kg of sesame into an extraction tank I, adding 3200L of 80% ethanol, adjusting the pH value to 5.5 by using glacial acetic acid, extracting at 80 ℃ for 1 hour, and beginning to produce an extracting solution to an extracting solution storage tank; while the extracting solution is produced, 1600L of 80% ethanol with pH value adjusted to 5.5 by glacial acetic acid is added into the extraction tank I, liquid production treatment is continuously carried out for 3 hours at 80 ℃, the speed of producing the extracting solution by the extraction tank I is kept equal to the speed of adding the ethanol, and dynamic balance of the liquid in the extraction tank I is achieved; the extraction tank I finishes the extraction of the extracting solution to obtain a first-level extracting solution.

Adding 1600L of 80% ethanol with pH adjusted to 4.5 by glacial acetic acid into the extraction tank I, and extracting at 80 deg.C for 0.5 hr; 1600kg of sesame is put into the extraction tank II; the extraction tank I starts to produce an extracting solution to the extraction tank II, sesame in the extraction tank II is extracted by using the produced solution of the extraction tank I, and the extraction is carried out for 0.5 hour at 80 ℃; after the extraction of the extracting solution is completed in the extraction tank I, 1600L of 80% ethanol with pH value adjusted to 4.5 by glacial acetic acid is added into the extraction tank I, and the extraction is carried out for 0.5 hour at 80 ℃; draw jar I and draw jar II simultaneous output extract, produce the liquid mode and be: while the extracting solution is produced in the extracting tank I, 1600L of 80% ethanol with pH value adjusted to 4.5 by glacial acetic acid is added into the extracting tank I; the extracting solution is output from the extracting tank I to an extracting tank II, the extracting tank II is continuously processed for 3 hours at the temperature of 80 ℃, the speed of the extracting solution output from the extracting tank II is kept equal to the speed of the ethanol added into the extracting tank I, and the dynamic balance of the liquid in the extracting tank I and the extracting tank II is achieved; and the extraction tank II finishes the output of the extracting solution to obtain a secondary extracting solution. Sesame is discharged from the extraction tank I.

Adding 1600L of 80% ethanol with pH adjusted to 4.5 by glacial acetic acid into the extraction tank II, and extracting at 80 deg.C for 0.5 hr; 1600kg of sesame is put into the extraction tank III; the extraction tank II starts to produce an extracting solution to the extraction tank III, sesame in the extraction tank III is extracted by using the produced solution of the extraction tank II, and the extraction is carried out for 0.5 hour at 80 ℃; after the extraction liquid is produced in the extraction tank II, 1600L of 80% ethanol with pH value adjusted to 4.5 by glacial acetic acid is added into the extraction tank II, and the extraction is carried out for 0.5 hour at 80 ℃; draw jar II and draw jar III and produce the extract simultaneously, produce the liquid mode and be: while the extracting solution is produced in the extracting tank II, 1600L of 80% ethanol with pH value adjusted to 4.5 by glacial acetic acid is added into the extracting tank III; the extracting tank II outputs extracting solution to the extracting tank III, the extracting solution is continuously processed for 3 hours at the temperature of 80 ℃, the speed of the extracting solution output by the extracting tank III is kept equal to the speed of the extracting tank II for adding ethanol, and the dynamic balance of the liquid in the extracting tank II and the extracting tank III is achieved; and the extraction tank III finishes the output of the extracting solution to obtain a third-level extracting solution. And discharging the sesame from the extraction tank II.

Mixing the first-stage extract, the second-stage extract and the third-stage extract to obtain about 12000L of primary extract.

And step S20, performing pressure filtration on the primary extract by using a plate-and-frame filter press, wherein the plate-and-frame filter is filtered by adopting non-woven fabrics, and the aperture size is 320 meshes to obtain filtrate.

And step S30, concentrating the filtrate by using a triple-effect evaporator at 55 ℃ and 0.01Mpa for 6 hours, and concentrating the filtrate to 2500L.

Step S40, separating the concentrated solution by using a simulated moving bed, and filling AB-8 macroporous adsorption resin into the simulated moving bed chromatogram; the desorbent is 80% ethanol solution, and the dosage is 3 times of the resin volume; the water washing area is purified water; the resin adsorption regeneration solvent is 95% ethanol; the flow rate of the adsorption area is 23 BV/h; the flow rate of the desorption area is 2 BV/h; the flow rate of the water washing area is 2 BV/h; the flow rate of the regeneration area is 2 BV/h; controlling the temperature at 45 ℃; controlling the pressure at 0.2MPa to obtain a separation liquid.

And step S50, transferring the separated liquid into a crystallizing tank, crystallizing at the temperature of 20 ℃ for 24 hours to obtain 81.6g of crude product.

And step S60, transferring the crude product into a crystallizing tank, dissolving the crude product by using 500L of mixed alcohol of 95% methanol and 95% ethanol with the volume ratio of 1:4, cooling to 5 ℃ after complete dissolution, adjusting the pH value to 3 by using glacial acetic acid, adding seed crystals, stirring for 15 minutes every 2 hours, and separating the mixture liquid after 36 hours to obtain 78.6kg of the refined product.

And step S70, performing centrifugal separation on the refined product, and drying to obtain the sesame extract with the weight of 63.51 kg.

The sesame extract was found to be 99.46% pure, containing 84.39% sesamin and 15.07% (+) -episesamin, and no sesamol or sesamolin component was detected.

It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.