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Method for entraining extraction and supercritical separation purification of squalene from Amaranthus hypochondriacus seeds

A supercritical separation and squalene technology, applied in chemical instruments and methods, adsorption purification/separation, hydrocarbon purification/separation, etc., can solve the high cost of silver nitrate restricting industrial applications, squalene oxidation, separation difficulties, etc. problems, to achieve the effect of improving comprehensive utilization value, avoiding oxidation, and high purity

Active Publication Date: 2019-08-16
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Grain amaranth, also known as Qiansuigu, belongs to the family Amaranthaceae and is an annual herb of the genus Amaranth. The fat content in grain amaranth grains is 5.73%-8.16% (dry material), of which unsaturated fatty acids account for 70%-80%. Grain amaranth Seed oil contains squalene, a precious ingredient, with a content of about 7%-8%. Squalene is a lipid unsaponifiable substance, which belongs to open-chain triterpenes, also known as cod liver oil terpene, which can increase superoxide dismutase in the body. (SOD) activity, enhancing the body's immunity, improving sexual ability, anti-aging, anti-fatigue, anti-tumor and other physiological functions, is a non-toxic marine biological active substance with the effect of preventing and curing diseases. The traditional method is to obtain it from deep-sea fish The cost of extraction from the liver is relatively high. At present, it has become a trend to extract squalene from plants, but the types of organic matter in plants are more complex, especially after the plant tissue has passed the deodorization process, squalene is usually in the form of tocopherol-squalene, sterol- Aggregation compounds such as squalene exist. Due to the similar properties of these components, separation is difficult. Therefore, how to choose an appropriate separation process to separate squalene from these aggregation compounds has become an important point.
[0003] One in the prior art, such as publication number CN104086348A, uses the double bond of squalene itself to form a complex with silver ions to separate it from the raw material. The disadvantage is that the high cost of silver nitrate restricts industrial applications. Publication number CN204022706U utilizes the boiling point difference of each material, adopts the method for rectifying molecule or molecular distillation to purify squalene, and its shortcoming is to cause the oxidation of squalene easily under high temperature condition

Method used

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  • Method for entraining extraction and supercritical separation purification of squalene from Amaranthus hypochondriacus seeds
  • Method for entraining extraction and supercritical separation purification of squalene from Amaranthus hypochondriacus seeds

Examples

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Effect test

Embodiment 1

[0021] Extract grain amaranth seed oil: weigh 100g grain amaranth seed, crush it to 1mm, and dry it at the same time to obtain grain amaranth seed powder for later use; then squeeze it with a rotary oil press to obtain the first oil phase and oil cake; mix the oil cake with 50ml petroleum Mix ether, heat and reflux at 85°C for 2 hours, filter to obtain the filtrate and filter residue, distill the filtrate under reduced pressure to remove petroleum ether, and recycle the petroleum ether to obtain the second oil phase; combine the first oil phase and the second oil phase, and uniformly Stir to obtain virgin amaranth seed oil for subsequent use;

[0022] Steam distillation deodorization: put the amaranth seed oil obtained in the previous step in the steam distillation deodorization device, start the vacuum pump, and when the absolute pressure of the whole system is below 100Pa, turn on the heater and slowly heat the oil to 180°C , then open the cock of the direct steam conduit, a...

Embodiment 2

[0029] Extracting grain amaranth seed oil: Weigh 100g grain amaranth seed, crush to 1.5mm, and dry at the same time to obtain grain amaranth seed powder for later use; then press with a rotary oil press to obtain the first oil phase and oil cake; mix the oil cake with 50ml Mix petroleum ether, heat and reflux at 85°C for 2 hours, filter to obtain filtrate and filter residue, distill the filtrate under reduced pressure to remove petroleum ether, and recycle the petroleum ether to obtain the second oil phase; combine the first oil phase and the second oil phase, Stir evenly to obtain virgin amaranth seed oil for subsequent use;

[0030] Steam distillation deodorization: put the amaranth seed oil obtained in the previous step in the steam distillation deodorization device, start the vacuum pump, and when the absolute pressure of the whole system is below 100Pa, turn on the heater and slowly heat the oil to 180°C , then open the cock of the direct steam conduit, and let in the dir...

Embodiment 3

[0037] Extract grain amaranth seed oil: weigh 100g grain amaranth seed, crush it to 1mm, and dry it at the same time to obtain grain amaranth seed powder for later use; then squeeze it with a rotary oil press to obtain the first oil phase and oil cake; mix the oil cake with 80ml petroleum Mix ether, heat and reflux at 85°C for 2 hours, filter to obtain the filtrate and filter residue, distill the filtrate under reduced pressure to remove petroleum ether, and recycle the petroleum ether to obtain the second oil phase; combine the first oil phase and the second oil phase, and uniformly Stir to obtain virgin amaranth seed oil for subsequent use;

[0038] Steam distillation deodorization: put the amaranth seed oil obtained in the previous step in the steam distillation deodorization device, start the vacuum pump, and when the absolute pressure of the whole system is below 100Pa, turn on the heater and slowly heat the oil to 180°C , then open the cock of the direct steam conduit, a...

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Abstract

A method for entraining extraction and supercritical separation purification of squalene from Amaranthus hypochondriacus seeds, disclosed in the invention, comprises the following steps: (1) deodorizing Amaranthus hypochondriacus seed oil to obtain an Amaranthus hypochondriacus deodorizing distillate; (2) methylating the Amaranthus hypochondriacus deodorizing distillate with a biological enzyme, and washing the methylated distillate with water to obtain a methyl ester liquid filtrate; (3) carrying out reverse phase column chromatography to remove fatty acid methyl ester in the methyl ester liquid filtrate; (4) carrying out ion exchange on the product obtained in step (3) by using an alkaline ion exchange resin to remove tocopherol; and (5) carrying out supercritical extraction to enrich aproduct obtained in step (4) in order to obtain squalene essential oil. The method effectively removes tocopherol and sterol in the tocopherol-squalene and sterol-squalene enriched compound in the extraction process, and the reaction conditions in the process are mild, so oxidation of squalene is avoided, and the resulting squalene has a high purity and a high extraction rate; and the products with high added values in the Amaranthus hypochondriacus are crudely purified, so the comprehensive utilization values of the Amaranthus hypochondriacus are improved.

Description

technical field [0001] The invention relates to the field of food and medicine, in particular to a method for entrained extraction and supercritical separation and purification of squalene from amaranth seeds. Background technique [0002] Grain amaranth, also known as Qiansuigu, belongs to the family Amaranthaceae and is an annual herb of the genus Amaranth. The fat content in grain amaranth grains is 5.73%-8.16% (dry material), of which unsaturated fatty acids account for 70%-80%. Grain amaranth Seed oil contains squalene, a precious ingredient, with a content of about 7%-8%. Squalene is a lipid unsaponifiable substance, which belongs to open-chain triterpenes, also known as cod liver oil terpene, which can increase superoxide dismutase in the body. (SOD) activity, enhancing the body's immunity, improving sexual ability, anti-aging, anti-fatigue, anti-tumor and other physiological functions, is a non-toxic marine biological active substance with the effect of preventing an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/21C07C7/12C07C7/00
CPCC07C7/00C07C7/12C07C11/21Y02P20/54
Inventor 郭嘉姚峰程健袁军丁元早周志丽张严
Owner WUHAN INSTITUTE OF TECHNOLOGY
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