阅读说明：本技术 一种沙棘籽油及其萃取工艺 (Sea-buckthorn seed oil and extraction process thereof ) 是由 毕书杰 郝敏 李娜 许瑞 耿成龙 于 2021-08-25 设计创作，主要内容包括：本发明公开了一种沙棘籽油及其萃取工艺,包括以下步骤：步骤1,将沙棘籽进行干燥处理,得到沙棘籽干；步骤2,将沙棘籽干置于研磨装置内进行研磨,得到沙棘籽粉；步骤3,将沙棘籽粉置于容器内,加入油相萃取溶剂,超声混合均匀后,置于微波中处理,得到沙棘籽萃取液；步骤4,向沙棘籽萃取液中加入水相萃取溶剂,将最终收集的有机相减压除去溶剂后,得到沙棘籽提取粗液；步骤5,将沙棘籽提取粗液置于水浴环境中升温至脱胶温度,然后加入氨基化硅胶颗粒,即得到沙棘籽油。本发明提供了一种对设备要求低、成本低以及适合大规模生产的沙棘籽油的生产工艺,该工艺萃取得到的沙棘籽油纯度高,能够满足市场的需要。(The invention discloses sea-buckthorn seed oil and an extraction process thereof, and the sea-buckthorn seed oil comprises the following steps: step 1, drying the sea buckthorn seeds to obtain dried sea buckthorn seeds; step 2, putting the dried sea buckthorn seeds into a grinding device for grinding to obtain sea buckthorn seed powder; step 3, putting the sea buckthorn seed powder into a container, adding an oil phase extraction solvent, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave for treatment to obtain sea buckthorn seed extract; step 4, adding an aqueous phase extraction solvent into the seabuckthorn seed extraction liquid, and removing the solvent from the finally collected organic phase under reduced pressure to obtain crude seabuckthorn seed extraction liquid; and 5, placing the crude sea-buckthorn seed extract in a water bath environment, heating to the degumming temperature, and then adding the aminated silica gel particles to obtain the sea-buckthorn seed oil. The invention provides a production process of sea-buckthorn seed oil, which has low requirement on equipment and low cost and is suitable for large-scale production.)

1. The extraction process of the sea buckthorn seed oil is characterized by comprising the following steps of:

step 1, drying the sea buckthorn seeds to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding an oil phase extraction solvent, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave for treatment to obtain sea buckthorn seed extract;

step 4, adding an aqueous phase extraction solvent into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting at least twice by using the aqueous phase extraction solvent, and removing the solvent from the finally collected organic phase under reduced pressure to obtain crude seabuckthorn seed extraction liquid;

and 5, heating the crude sea buckthorn seed extract liquid in a water bath environment to a degumming temperature, adding the aminated silica gel particles, stirring and dispersing for 0.5-1 h, continuously heating to a temperature higher than the boiling point of water, continuously stirring for 0.2-0.4 h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain the sea buckthorn seed oil.

2. The extraction process of sea buckthorn seed oil according to claim 1, wherein in the step 1, the drying treatment is performed by drying in an oven at a temperature of 50-70 ℃.

3. The extraction process of sea buckthorn seed oil according to claim 1, wherein in the step 2, the sea buckthorn seed oil is sieved by a 30-50 mesh sieve after being ground.

4. The process of claim 1, wherein in step 3, the oil phase extraction solvent comprises at least one of n-hexane, dichloromethane, ethyl acetate, petroleum ether, ethanol and acetone.

5. The extraction process of sea buckthorn seed oil according to claim 1, wherein in the step 3, the microwave power is 200-800W, and the microwave treatment time is 0.2-0.5 h.

6. The extraction process of the seabuckthorn seed oil according to claim 1, wherein in the step 3, the mass ratio of the seabuckthorn seed powder to the oil phase extraction solvent is 1: 30-50.

7. The process of claim 1, wherein in the step 4, the aqueous phase extraction solvent is purified water.

8. The extraction process of seabuckthorn seed oil according to claim 1, wherein in the step 4, the mass ratio of the aqueous phase extraction solvent to the seabuckthorn seed extraction liquid is 1: 0.8-1.

9. The extraction process of seabuckthorn seed oil according to claim 1, wherein in the step 5, the degumming temperature is 75-85 ℃.

10. A seabuckthorn seed oil, which is characterized by being prepared by the extraction process of seabuckthorn seed oil according to claim 1.

Technical Field

The invention relates to the field of plant extraction, and particularly relates to sea-buckthorn seed oil and an extraction process thereof.

Background

Seabuckthorn is a precious resource used as both medicine and food, wherein seabuckthorn seed oil contains a plurality of active ingredients such as abundant flavone, vitamin, carotene, fatty acid, sterol, alkaloid and the like, and has wide application in medicine, food, health care products and medicine.

At present, the more extraction methods of the seabuckthorn seed oil are a squeezing method, a supercritical CO2 fluid extraction separation method and a subcritical low-temperature extraction separation method, the squeezing method adopts a mechanical squeezing mode, the oil yield is low, the impurity content is high, the high temperature generated in the process of squeezing the seabuckthorn seed can damage unsaturated fatty acid in the seabuckthorn seed oil, the supercritical CO2 fluid extraction separation method has good extraction and separation effects and cannot pollute the seabuckthorn seed oil, but the supercritical CO2 fluid extraction separation method is carried out under an ultrahigh pressure state, the production equipment has high requirement on air tightness, the volume of the production equipment is small, and the large-scale and industrialized production of the seabuckthorn seed oil cannot be carried out, so the method is not suitable for large-scale production of the seabuckthorn seed oil, and the subcritical low-temperature extraction separation method keeps an extraction solvent in a subcritical state, namely, the solvent is in a temperature range which is higher than the boiling point but lower than the critical temperature, the subcritical low-temperature extraction technology is a mature technology in a state of liquid existence under certain pressure, does not damage thermosensitive components in the materials, has relatively low requirements on equipment, and is suitable for large-scale production.

Disclosure of Invention

Aiming at the problems of high equipment requirement, high cost and unsuitability for large-scale production in the prior art, the invention aims to provide the sea buckthorn seed oil and the extraction process thereof.

The purpose of the invention is realized by adopting the following technical scheme:

in a first aspect, the invention provides a process for extracting sea buckthorn seed oil, which comprises the following steps:

step 1, drying the sea buckthorn seeds to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding an oil phase extraction solvent, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave for treatment to obtain sea buckthorn seed extract;

step 4, adding an aqueous phase extraction solvent into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting at least twice by using the aqueous phase extraction solvent, and removing the solvent from the finally collected organic phase under reduced pressure to obtain crude seabuckthorn seed extraction liquid;

and 5, heating the crude sea buckthorn seed extract liquid in a water bath environment to a degumming temperature, adding the aminated silica gel particles, stirring and dispersing for 0.5-1 h, continuously heating to a temperature higher than the boiling point of water, continuously stirring for 0.2-0.4 h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain the sea buckthorn seed oil.

Preferably, in the step 1, the drying treatment is performed by placing the mixture in an oven for drying, wherein the temperature of the oven is 50-70 ℃.

Preferably, in the step 2, the mixture is sieved by a sieve of 30-50 meshes after grinding.

Preferably, in the step 3, the oil phase extraction solvent comprises at least one of n-hexane, dichloromethane, ethyl acetate, petroleum ether, ethanol and acetone.

Preferably, in the step 3, the power of the microwave is 200-800W, and the microwave treatment time is 0.2-0.5 h.

Preferably, in the step 3, the mass ratio of the sea buckthorn seed powder to the oil phase extraction solvent is 1: 30-50.

Preferably, in the step 4, the aqueous phase extraction solvent is purified water.

Preferably, in the step 4, the mass ratio of the aqueous phase extraction solvent to the seabuckthorn seed extraction liquid is 1: 0.8-1.

Preferably, in the step 5, the degumming temperature is 75-85 ℃.

Preferably, in the step 5, the addition amount of the aminated silica gel particles is 5-10% of the crude extract of the seabuckthorn seeds.

Preferably, in the step 5, the preparation method of the aminated silica gel particles comprises:

s1, weighing silica gel particles, mixing the silica gel particles with deionized water according to a mass ratio of 1: 5-10, continuously dropwise adding 2-5 drops of sulfuric acid solution with a mass fraction of 98% while stirring, continuously stirring for 2-3 hours after completely dropwise adding, filtering, washing with pure water for three times, and drying to form acidified silica gel particles;

s2, weighing amino acid and deionized water, mixing the amino acid and the deionized water according to a mass ratio of 1: 5-10, stirring and dissolving, adding acidified silica gel particles, heating to 55-65 ℃, continuing stirring for 6-10 hours, filtering and collecting solids, washing the solids with pure water until the washing liquid is neutral, and drying to obtain aminated silica gel; wherein the mass ratio of the amino acid to the acidified silica gel particles is 1: 2-3.

Preferably, the amino acid includes at least one of methionine, cysteine, proline and valine.

Preferably, the particle size of the silica gel particles is 20-50 μm.

In a second aspect, the invention provides a sea buckthorn seed oil, which is prepared by using the extraction process.

The invention has the beneficial effects that:

the invention provides a production process of sea-buckthorn seed oil, which has low requirement on equipment and low cost and is suitable for large-scale production.

The seabuckthorn seeds contain a large amount of oleic acid and linoleic acid, the linoleic acid is an essential fatty acid and can enhance the action of various vitamins, and after the seabuckthorn seed oil is acidified, hydrated and degreased, the treatment mode can cause a large amount of fatty acid compounds in the seabuckthorn seeds, particularly the linoleic acid, to be lost, thereby causing waste. Most of the traditional hydration degumming methods use silica gel particles, so that the surface of the silica gel particles is acidified and then amino acid is adsorbed by the silica gel particles, and the prepared amination silica gel particles are used for hydration degumming, so that the adsorption of linoleic acid components can be reduced to a great extent, and the adsorption capacity of the amination silica gel particles on water is enhanced, so that the extracted sea-buckthorn seed oil has higher quality and activity.

Detailed Description

For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.

The hydration degumming is a degumming method which utilizes the hydrophilicity of peptized impurities such as phospholipid, etc. and adds a certain amount of water (or aqueous solution of acid, alkali and salt) into the crude oil to make the peptized impurities absorb water, coagulate and settle to remove. The impurities which can be removed by coagulation and sedimentation in the hydration degumming process are mainly phospholipid, and protein, glycosyl diglyceride, mucilage, trace metal ions and the like which are combined with the phospholipid.

The invention is further described below with reference to the following examples.

Example 1

A sea buckthorn seed oil extraction process comprises the following steps:

step 1, drying the sea buckthorn seeds in a drying oven at 60 ℃ to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding, and sieving the ground sea buckthorn seeds with a 30-50-mesh sieve to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding n-hexane, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave with the power of 600W for treatment for 0.3h to obtain sea buckthorn seed extract; the mass ratio of the sea buckthorn seed powder to the n-hexane is 1: 40;

step 4, adding purified water into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting with purified water for at least two times, removing the solvent by using the finally collected organic layer under reduced pressure to obtain crude seabuckthorn seed extraction liquid; the mass ratio of the purified water to the sea buckthorn seed extract is 1: 0.9;

step 5, placing the crude sea buckthorn seed extraction liquid in a water bath environment, heating to 80 ℃, then adding the aminated silica gel particles, stirring and dispersing for 0.8h, continuing to heat to a temperature higher than the boiling point of water, continuing to stir for 0.3h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain sea buckthorn seed oil; the addition amount of the aminated silica gel particles is 8% of the crude extract of seabuckthorn seeds.

In the step 5, the preparation method of the aminated silica gel particles comprises the following steps:

s1, weighing silica gel particles with the particle size of 20-50 microns, mixing the silica gel particles with deionized water according to a mass ratio of 1:7, continuously dropwise adding 3 drops of sulfuric acid solution with the mass fraction of 98% while stirring, continuously stirring for 2.5 hours after the dropwise adding is completed, filtering, washing for three times by using pure water, and drying to form acidified silica gel particles;

s2, weighing methionine and deionized water, mixing the methionine and the deionized water according to a mass ratio of 1:7, stirring and dissolving, adding acidified silica gel particles, heating to 60 ℃, continuing stirring for 8 hours, filtering and collecting solids, washing the solids with pure water until the washing liquid is neutral, and drying to obtain aminated silica gel; wherein the mass ratio of the methionine to the acidified silica gel particles is 1: 2.5.

Example 2

A sea buckthorn seed oil extraction process comprises the following steps:

step 1, drying the sea buckthorn seeds in a drying oven at 50 ℃ to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding, and sieving the ground sea buckthorn seeds with a 30-50-mesh sieve to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding dichloromethane, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave with the power of 200W for treatment for 0.2h to obtain sea buckthorn seed extract; the mass ratio of the sea buckthorn seed powder to the dichloromethane is 1: 30;

step 4, adding purified water into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting with purified water for at least two times, removing the solvent by using the finally collected organic layer under reduced pressure to obtain crude seabuckthorn seed extraction liquid; the mass ratio of the purified water to the sea buckthorn seed extract is 1: 0.8;

step 5, placing the crude sea buckthorn seed extraction liquid in a water bath environment, heating to 75 ℃, then adding the aminated silica gel particles, stirring and dispersing for 0.5h, continuing to heat to a temperature higher than the boiling point of water, continuing to stir for 0.2h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain sea buckthorn seed oil; the addition amount of the aminated silica gel particles is 5% of the crude extract of seabuckthorn seeds.

In the step 5, the preparation method of the aminated silica gel particles comprises the following steps:

s1, weighing silica gel particles with the particle size of 20-50 microns, mixing the silica gel particles with deionized water according to a mass ratio of 1:5, continuously dropwise adding 2 drops of sulfuric acid solution with the mass fraction of 98% while stirring, continuously stirring for 2 hours after the sulfuric acid solution is completely dropwise added, filtering, washing with pure water for three times, and drying to form acidified silica gel particles;

s2, weighing cysteine and deionized water, mixing the cysteine and the deionized water according to a mass ratio of 1:5, stirring and dissolving, adding acidified silica gel particles, heating to 55 ℃, continuing stirring for 6 hours, filtering and collecting solids, washing the solids with pure water until the washing liquid is neutral, and drying to obtain aminated silica gel; wherein the mass ratio of the cysteine to the acidified silica gel particles is 1:2.

Example 3

A sea buckthorn seed oil extraction process comprises the following steps:

step 1, drying the sea buckthorn seeds in an oven at 70 ℃ to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding, and sieving the ground sea buckthorn seeds with a 30-50-mesh sieve to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding ethanol, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave with the power of 800W for treatment for 0.5h to obtain sea buckthorn seed extract; the mass ratio of the sea buckthorn seed powder to the ethanol is 1: 50;

step 4, adding purified water into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting with purified water for at least two times, removing the solvent by using the finally collected organic layer under reduced pressure to obtain crude seabuckthorn seed extraction liquid; the mass ratio of the purified water to the sea buckthorn seed extract is 1: 1;

step 5, placing the crude sea buckthorn seed extraction liquid in a water bath environment, heating to 85 ℃, then adding the aminated silica gel particles, stirring and dispersing for 1h, continuing to heat to a temperature higher than the boiling point of water, continuing to stir for 0.4h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain sea buckthorn seed oil; the addition amount of the aminated silica gel particles is 10% of the crude extract of seabuckthorn seeds.

In the step 5, the preparation method of the aminated silica gel particles comprises the following steps:

s1, weighing silica gel particles with the particle size of 20-50 microns, mixing the silica gel particles with deionized water according to a mass ratio of 1:10, continuously dropwise adding 5 drops of sulfuric acid solution with the mass fraction of 98% while stirring, continuously stirring for 3 hours after complete dropwise adding, filtering, washing with pure water for three times, and drying to form acidified silica gel particles;

s2, weighing proline and deionized water, mixing the proline and the deionized water according to a mass ratio of 1:10, stirring and dissolving, adding acidified silica gel particles, heating to 65 ℃, continuing stirring for 10 hours, filtering and collecting solids, washing the solids with pure water until the washing liquid is neutral, and drying to obtain silicon amide gel; wherein the mass ratio of the proline to the acidified silica gel particles is 1: 3.

Comparative example

A sea buckthorn seed oil extraction process comprises the following steps:

step 1, drying the sea buckthorn seeds in a drying oven at 60 ℃ to obtain dried sea buckthorn seeds;

step 2, putting the dried sea buckthorn seeds into a grinding device for grinding, and sieving the ground sea buckthorn seeds with a 30-50-mesh sieve to obtain sea buckthorn seed powder;

step 3, putting the sea buckthorn seed powder into a container, adding n-hexane, carrying out ultrasonic mixing uniformly, and then putting the mixture into a microwave with the power of 600W for treatment for 0.3h to obtain sea buckthorn seed extract; the mass ratio of the sea buckthorn seed powder to the n-hexane is 1: 40;

step 4, adding purified water into the seabuckthorn seed extraction liquid, uniformly mixing, separating an organic layer, repeatedly extracting with purified water for at least two times, removing the solvent by using the finally collected organic layer under reduced pressure to obtain crude seabuckthorn seed extraction liquid; the mass ratio of the purified water to the sea buckthorn seed extract is 1: 0.9;

step 5, heating the crude sea buckthorn seed extraction liquid to 80 ℃ in a water bath environment, adding silica gel particles with the particle size of 20-50 microns, stirring and dispersing for 0.8h, continuing to heat to a temperature higher than the boiling point of water, continuing to stir for 0.3h, cooling to room temperature, filtering out solids, and drying the liquid under reduced pressure to obtain sea buckthorn seed oil; the addition amount of the silica gel particles is 8 percent of the crude extract of the seabuckthorn seeds.

In order to more clearly illustrate the present invention, the present invention performed the detection of the yield of the seabuckthorn seed oil and the content of linoleic acid in the seabuckthorn seed oil with respect to the seabuckthorn seed oil prepared by the extraction processes of examples 1 to 3 and the comparative example, and the results are shown in the following table:

	example 1	Example 2	Example 3	Comparative example
					Sea buckthorn seed oil yield (%)	97	96	96	92
Linoleic acid content (wt%)	16.2	14.7	15.8	7.1

As can be seen from the above table, the sea buckthorn seed oil obtained by the method of embodiments 1 to 3 of the present invention has a higher yield and a higher linoleic acid content, which indicates that the loss of linoleic acid is less during the extraction process.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, 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 can 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.