阅读说明：本技术 一种菜籽油中角鲨烯的提取方法 (Method for extracting squalene from rapeseed oil ) 是由 熊净 于 2019-10-17 设计创作，主要内容包括：本发明涉及角鲨烯提取技术领域,具体涉及一种菜籽油中角鲨烯的提取方法,包括如下步骤：(1)向菜籽油中加入含复合酶的水溶液,然后置于脉冲直流电场下处理；(2)向步骤(1)所得物中加入微晶纤维溶液混,再加入转晶剂于50-55℃条件下混合后,保温处理,过滤,去除滤液；(3)向步骤(2)所得物中加入乙醇,同时加入左旋维生素C,置于60-65℃条件下恒温水浴中回流,冷却,水洗直至洗涤液呈中性后,在真空条件下蒸馏；本发明中角鲨烯提取率高,试剂残留少,提高了角鲨烯的纯度,并且降低提取成本。(The invention relates to the technical field of squalene extraction, and particularly relates to a method for extracting squalene from rapeseed oil, which comprises the following steps: (1) adding a water solution containing a complex enzyme into the rapeseed oil, and then placing the rapeseed oil in a pulse direct current electric field for treatment; (2) adding a microcrystalline fiber solution into the product obtained in the step (1), mixing, adding a crystal modifier, mixing at 50-55 ℃, preserving heat, filtering, and removing filtrate; (3) adding ethanol and levovitamin C into the product obtained in the step (2), placing the mixture in a constant-temperature water bath at the temperature of 60-65 ℃ for reflux, cooling, washing with water until the washing liquid is neutral, and distilling under vacuum; the method has the advantages of high squalene extraction rate, less reagent residue, improvement of squalene purity and reduction of extraction cost.)

1. The method for extracting squalene from rapeseed oil is characterized by comprising the following steps of:

(1) adding a water solution containing complex enzyme into the rapeseed oil until the water-oil ratio is 1: (0.2-0.5), and then treating for 10-20min under a pulse direct current electric field;

(2) adding the microcrystalline fiber solution into the product obtained in the step (1), mixing for 10-15min, adding a crystal modifier, mixing for 3-5min at 50-55 ℃, performing heat preservation treatment for 5-10min, filtering, and removing the filtrate;

(3) adding ethanol into the product obtained in the step (2) until the molar ratio of ethanol to oil is (5-7):1, simultaneously adding levovitamin C to 2-6ppm of the total mass fraction of the system, placing in a constant-temperature water bath at 60-65 ℃ for refluxing for 20-30min, cooling, washing with water until the washing liquid is neutral, and distilling under the vacuum condition of 70-90 Pa.

2. The method for extracting squalene from rapeseed oil according to claim 1, wherein the working conditions of the pulse direct current electric field are as follows: the peak voltage is 30-35V, the pulse frequency is 1-2kHz, and the duty ratio is 0.1-0.5.

3. The method for extracting squalene from rapeseed oil according to claim 1, wherein the complex enzyme content in the complex enzyme-containing aqueous solution is 30-50 ppm.

4. The method for extracting squalene from rapeseed oil according to claim 1 or 3, wherein the complex enzyme is prepared from phospholipase, protease and cellulase in a ratio of 1: (0.5-1): (0.2-0.4) in the ratio of the inoculum size.

5. The method for extracting squalene from rapeseed oil according to claim 1, wherein the mass concentration of the microcrystalline fiber solution is 20-25%.

6. The method for extracting squalene from rapeseed oil according to claim 1, wherein the addition amount of said microcrystalline fiber solution is 4-10% of the mass of rapeseed oil.

7. The method for extracting squalene from rapeseed oil according to claim 1, wherein the crystal modifier is a citric acid solution containing catechin, and the mass fraction of the citric acid solution is as follows: catechin 0.01-0.05%, citric acid 10-15%, and water in balance.

8. The method for extracting squalene from rapeseed oil according to claim 1, wherein the addition amount of the crystal modifier is 15-25ppm of the mass of the filtrate.

9. The method for extracting squalene from rapeseed oil according to claim 1, wherein the distillation temperature is 220-230 ℃.

Technical Field

The invention relates to the technical field of squalene extraction, and particularly relates to a method for extracting squalene from rapeseed oil.

Background

Rapeseed oil, also known as rapeseed oil or coriander oil, is also known as clear oil in the southern Hunan region. The edible oil is widely used in daily life of people due to golden color and faint scent, and is one of the main edible oil at home and abroad. The rapeseed oil has the unsaturated fatty acid content of more than 85 percent, contains rich oleic acid, linoleic acid, linolenic acid and phospholipid, has the digestibility of 99 percent to human bodies, and is rich in bioactive components such as vitamin E, polyphenol, squalene, sterol and the like.

Squalene is a highly unsaturated hydrocarbon compound, a lipid unsaponifiable substance, has a chemical name of 2,6,10,15,19, 23-hexamethyl-2, 6,10,14,18, 22-tetracosahexaene, is an open-chain triterpenoid compound, has various physiological functions of improving the activity of superoxide dismutase (SOD) in vivo, enhancing the immunity of organisms, improving sexual functions, resisting aging, fatigue, tumors and the like, and is widely applied to the fields of medicines, foods, cosmetics, chemical engineering and the like.

For example, patent document CN201510956808.1 discloses a method for extracting a plant-derived squalene composition, a method for preparing a squalene-containing medicine, a squalene-containing medicine prepared by the method, and applications thereof. The method for extracting the plant source squalene composition comprises the following steps: sequentially carrying out pretreatment and enrichment separation on the raw material rich in squalene, wherein the enrichment separation conditions are controlled so that the obtained plant source squalene composition contains 35-80 wt% of squalene, and the raw material rich in squalene contains 5-30 wt% of squalene and 10-40 wt% of sterol.

For another example, patent document CN201110027119.4 discloses a method for extracting squalene from camellia seeds, which comprises the following steps: preparing materials, crushing, leaching, concentrating, carrying out methyl esterification reaction, carrying out complexing agent-borax reaction, carrying out macroporous resin chromatographic separation and purification, concentrating, extracting, washing and concentrating to obtain crude squalene oil, and extracting with supercritical carbon dioxide to obtain squalene essential oil with squalene content being more than or equal to 80%; the tea oil squalene soft capsule is prepared from the following raw materials in percentage by weight: 87-90 parts of squalene essential oil with the squalene content being more than or equal to 80%, 3-5 parts of polyethylene glycol 4003, 2-3 parts of beeswax and 2-5 parts of phospholipid.

In the literature, "influence of refining on the quality of rapeseed oil" (published in 2018 by equantry et al), it is also mentioned that "the acid value, peroxide value, color and phosphorus content of refined rapeseed oil are all reduced, and the contents of VE, sterol, polyphenol and squalene are obviously reduced; the contents of trans fatty acid and 3-chloropropanol are not changed greatly, so the application extracts squalene in order to prevent the reduction of squalene content and the reduction of squalene utilization value.

Disclosure of Invention

The invention provides a method for extracting squalene from rapeseed oil to solve the technical problems.

The method is realized by the following technical scheme:

a method for extracting squalene from rapeseed oil comprises the following steps:

(1) adding a water solution containing complex enzyme into the rapeseed oil until the water-oil ratio is 1: (0.2-0.5), and then treating for 10-20min under a pulse direct current electric field;

(2) adding the microcrystalline fiber solution into the product obtained in the step (1), mixing for 10-15min, adding a crystal modifier, mixing for 3-5min at 50-55 ℃, performing heat preservation treatment for 5-10min, filtering, and removing the filtrate;

(3) adding ethanol into the product obtained in the step (2) until the molar ratio of ethanol to oil is (5-7):1, simultaneously adding levovitamin C to 2-6ppm of the total mass fraction of the system, placing in a constant-temperature water bath at 60-65 ℃ for refluxing for 20-30min, cooling, washing with water until the washing liquid is neutral, and distilling under the vacuum condition of 70-90 Pa.

The working conditions of the pulse direct current electric field are as follows: the peak voltage is 30-35V, the pulse frequency is 1-2kHz, and the duty ratio is 0.1-0.5.

The compound enzyme content in the compound enzyme-containing aqueous solution is 30-50 ppm.

The compound enzyme is prepared from phospholipase, protease and cellulase according to the proportion of 1: (0.5-1): (0.2-0.4) in the ratio of the inoculum size.

The temperature of the distillation is 220-230 ℃.

The mass concentration of the microcrystalline fiber solution is 20-25%.

The addition amount of the microcrystalline fiber solution is 4-10% of the mass of the rapeseed oil.

The crystal transformation agent is a citric acid solution containing catechin, and the mass fraction of the crystal transformation agent is as follows: catechin 0.01-0.05%, citric acid 10-15%, and water in balance.

The addition amount of the crystal transformation agent is 15-25ppm of the mass of the filtrate.

Has the advantages that:

the method has the advantages of high squalene extraction rate and less reagent residue, improves the squalene purity, reduces the extraction cost, and specifically comprises the following steps:

firstly, the invention uses the water solution containing complex enzyme and the pulse direct current electric field to promote the rapeseed oil to break emulsion and provide conditions for fully releasing effective substances.

Secondly, the invention utilizes the action of the cellulose in the microcrystalline fibers and the complex enzyme to damage the crystal structure of the microcrystalline fibers, coats the fatty acid and the impurity elements in the mixing process, and utilizes the crystal transformation agent to improve the crystal structure, so that the effective separation of the squalene, the fatty acid and the impurity elements is realized.

Then, the rapeseed oil is esterified, and the levorotatory vitamin C is added during the esterification to prevent oxidation, so that the yield of squalene is improved.

Finally, the invention utilizes vacuum distillation to effectively cathode squalene, simultaneously reduces the residual quantity of reagents and improves the purity and yield of squalene.

Detailed Description

The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.