CN105623839A - Method for extracting silybum marianum oil - Google Patents

Method for extracting silybum marianum oil Download PDF

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Publication number
CN105623839A
CN105623839A CN201610052374.7A CN201610052374A CN105623839A CN 105623839 A CN105623839 A CN 105623839A CN 201610052374 A CN201610052374 A CN 201610052374A CN 105623839 A CN105623839 A CN 105623839A
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silybum marianum
oil
seed
minute
product
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CN201610052374.7A
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CN105623839B (en
Inventor
马亚琼
徐旭
赵永强
张成亮
贾洪涛
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INNER MONGOLIA CHANGHUI BIOLOGICAL TECHNOLOGY Co.,Ltd.
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/106Production of fats or fatty oils from raw materials by extracting using ultra-sounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/108Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/10Refining fats or fatty oils by adsorption

Abstract

The invention relates to a method for extracting silybum marianum oil from silybum marianum seeds. By adopting a method of immersing, freeze drying and ultrasonic extraction, the product yield is greatly increased; moreover, the content of unsaturated fatty acid in the oil product reaches more than 50 percent, the loss is basically avoided, and the yield reaches up to more than 95 percent; and moreover, the oil is clear in color, full in fragrance and very suitable for industrialized production. The product can be directly used as healthy edible oil or can be applied to a health product.

Description

A kind of method extracting Silybum Marianum Gaertn Seed Oil
Technical field
The present invention relates to the method extracting Silybum Marianum Gaertn Seed Oil, more particularly, to a kind of method extracting Silybum Marianum Gaertn Seed Oil from Herba Silybi mariani seed.
Background technology
Compositae Silybum Herba Silybi mariani (Silybummarianum) is the plant originating in West Europe and north African, soil, moisture requirement is not tight, ground, sandy beach, salt-soda soil all can be planted, strong adaptability, introduce after China in Shaanxi, Gansu, Heilungkiang and Hebei etc. are economized commerial growing, are mainly used in extracting silymarin. Silymarin is known by people because of the effect of its hepatic cholagogic, is widely used in preventing and treating cardiovascular and cerebrovascular disease. But silybum marianum seed is except containing silymarin, possibly together with a large amount of Silybum Marianum Gaertn Seed Oils, national health State Family Planning Commission approval on April 16th, 2014 silybum marianum seed oil is new raw-food material.
The main component of Silybum Marianum Gaertn Seed Oil (SilybummarianumSeedoil) is unsaturated fatty acid, i.e. linoleic acid (content 45%). Linoleic acid, as the fatty acid of needed by human, receives greatly to pursue recently. Silybum Marianum Gaertn Seed Oil oil is good, belong to green plants natural, free of contamination oil, can be used as family cooking, long-term edible can playing protects the liver, protects health-care effect dirty, improving eyesight, there is reduction cholesterol, be used for preventing and treating effect of atherosclerosis, hypertension, coronary heart disease, softening cardiovascular and cerebrovascular vessel, removing blood rubbish.
At present that the research producing preparation of Silybum Marianum Gaertn Seed Oil is still not deep enough, generally with silybum marianum seed for raw material, take the techniques such as direct cold pressing, filtration to make. But, this method only filters through natural sedimentation, and oil product acid number is high, and gastronomical process oil smoke is big, and edible flavor is poor, and oil yield is low, and cake Residual oil is high. Also have and adopt water substitution, make cell rupture, moisture be impregnated into inside intact cell by soaking, make gelinite expand, add and propagandize seed hotly, making intracellular oil body flow out, separated by oil through succusion, this method is without squeezing, without solvent, oil body is made to flow out complete, and special fragrance can be produced, but extraction efficiency is inadequate, and whole process time is longer. Also have and adopt extract by solvents, but owing to the solvent of solubilized oils and fats mostly is toxic organic solvent, thus the Silybum Marianum Gaertn Seed Oil that this method extracts is typically used as iundustrial oil, and cannot eat. Recently also developing carbon dioxide supercritical fluid extraction, aqueous enzymatic method extraction etc. method, separation efficiency is high, but still exists or cost height enterprise or time longer etc. shortcoming.
Therefore, the drawbacks described above existed for the method preparing Silybum Marianum Gaertn Seed Oil in prior art and deficiency, the preparation method that it is an object of the invention to provide a kind of new Silybum Marianum Gaertn Seed Oil, separation efficiency is high, and excellent product quality, is suitable to industrialized production.
Summary of the invention
The invention provides a kind of preparation method extracting high-purity Silybum Marianum Gaertn Seed Oil from silybum marianum seed, comprise the following steps:
(1) screening: take Herba Silybi mariani seed raw material, sends into screening machine, removes the impurity in raw material, such as earth, sandstone, weeds seed, ghost and dust etc.;
(2) infiltration: the silybum marianum seed after screening of weighing, adds 5-10 times amount water and makes it be immersed in water, be simultaneously introduced 1-5 weight % tea polyphenols, be warming up to 40-60 DEG C, and stirring makes it fully infiltrate, and crosses elimination excessive moisture, the silybum marianum seed that must infiltrate; Infiltration degree is that the water content making silybum marianum seed reaches more than 30%, it is preferable that 30-35%;
(3) frozen dried: the silybum marianum seed of infiltration is proceeded to freeze-drier, is cooled to subzero 5-10 DEG C, maintains 10-15 minute, then temperature is adjusted to room temperature maintenance 10-15 minute, then is cooled to subzero 5-10 DEG C, maintains 5-10 minute, is taken out by silybum marianum seed raw material;
(4) ultrasonic Treatment: the material after lyophilised process proceeds to ultrasonic extractor, adds water and the 3-5% Silybum Marianum Gaertn Seed Oil of 0.5-1 times of weight, collaborative extraction 10-20 minute, ultrasonic power 250-350w;
(5) centrifugation: the solution after process is put in high speed centrifuge and is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product;
(6) refine: add hargil and the 2-3 weight % tea polyphenols of oil weight 3-6%, temperature is increased to 80-100 degree, vacuum is maintained at about 96kPa, maintain 20-30 minute, through flame filter press elimination hargil, enter odor removing pot deodorize, temperature 200-240 DEG C, 1-2 hour time, the straying quatity of live (open) steam with do not cause oils and fats splash be advisable;
(7) oil is put into cooler and is cooled to room temperature, filter, pump into product tank.
Present invention also offers the Silybum Marianum Gaertn Seed Oil that said method prepares.
The Silybum Marianum Gaertn Seed Oil product oil colours that the inventive method prepares is limpid, full aroma, and product yield reaches more than 95%, without using organic solvent, is useful as very much health-care edible oil or health-oriented products.
The present invention is in the liquefaction process of Silybum Marianum Gaertn Seed Oil; first time proposes to add water soluble ingredient tea polyphenols in liquefaction process; play protective agent effect; unsaturated fatty acid in Silybum Marianum Gaertn Seed Oil is avoided to receive destruction; and have employed the method for infiltration-lyophilizing-ultrasonic extraction and drastically increase product yield; and ensure that in oil product, unsaturated fatty acid content reaches more than 50%, basic free of losses, and yield is up to more than 95%.
Subordinate list is unsaturated fatty acid content and product yield in the product oil that different preparation method is obtained.
Method Unsaturated fatty acid content (%) Product yield (%)
The embodiment of the present invention 1 method 55.58 95.87
Comparison 1 25.29 89.86
Comparison 2 47.64 81.12
Comparison 3 46.17 78.57
Comparison 4 44.95 75.50
Comparison 5 41.58 92.14
Wherein, contrast method 1 is the method identical with the embodiment of the present invention 1, is distinctive in that and is added without tea polyphenols; Contrast method 2 is the method identical with the embodiment of the present invention 1, is distinctive in that the water quantities of infiltration is 20-25%; Contrast method 3 is the method identical with the embodiment of the present invention 1, is distinctive in that and does not comprise immersion step; Contrast method 4 is the method identical with the embodiment of the present invention 1, is distinctive in that and does not comprise frozen dried step; Contrast method 5 is for extracting Silybum Marianum Gaertn Seed Oil through supercritical carbon dioxide extraction method after the broken silybum marianum seed of fine grinding.
As can be seen from the table, it is added without tea polyphenols and can greatly affect the content of unsaturated fatty acid, and tea polyphenols had both played antioxidation in whole method, simultaneously because its water miscible speciality, it is prone to remove, although the character of tea polyphenols as well known to those skilled in the art and performance, but the present inventor does not see has people to add this composition in liquefaction process to improve the content of product oil weight unsaturated fatty acid, simultaneously, inventors have also discovered that not to be that arbitrary antioxidant all can add the method to the present invention, such as vitamin E etc. are then not particularly suited for the inventive method. additionally, water content soaking method and the step of freeze drying crossed of the present invention has a significant impact for the character of oil product, it is generally recognized that if moisture is too high, fuel-displaced oil colours is shallow, and foam is many, if very too low, then oil colours is deep and muddy, has the powdery impurity of suspension. but present invention discover that the water content improving silybum marianum seed reaches more than 30%, it is appreciated that ultrasonic extraction step after lyophilizing, not only without influence on the character of oil product, and drastically increase oil productivity.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearly, below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is a part of embodiment of the present invention, rather than whole probability. The every other embodiment that those of ordinary skill in the art are obtained under not making creative work, both falls within protection scope of the present invention.
Embodiment 1
10 tons of silybum marianum seeds, send into screening machine, remove the impurity in raw material, obtain silybum marianum seed 9.95 tons, add 10 times amount water and make it be immersed in water, it is simultaneously introduced 5 weight % tea polyphenols, being warming up to 40-60 DEG C, stirring makes it fully infiltrate, and infiltration to water content reaches 35%, cross elimination excessive moisture, the silybum marianum seed that must infiltrate; The silybum marianum seed infiltrated is proceeded to freeze-drier, it is cooled to subzero 5-10 DEG C, maintain 15 minutes, temperature is adjusted to room temperature again keep 10-15 minute, then is cooled to subzero 5-10 DEG C, maintain 10 minutes, material after lyophilised process is proceeded to ultrasonic extractor, add equivalent water and 5% Silybum Marianum Gaertn Seed Oil, collaborative extraction 15 minutes, ultrasonic power 350w; Solution after process is put in high speed centrifuge and is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product; Add oil and weigh hargil and the 3 weight % tea polyphenols of 5%, temperature is increased to 80-100 degree, vacuum is maintained at about 96kPa, maintain 20 minutes, through flame filter press elimination hargil, enter odor removing pot deodorize, temperature 200-240 DEG C, 1-2 hour time, the straying quatity of live (open) steam with do not cause oils and fats splash be advisable; Oil is put into cooler and is cooled to room temperature, filter, pump into product tank. After testing, in product oil, the content of unsaturated fatty acid is 55.58%, and product yield is 95.87%.
Embodiment 2
2 tons of silybum marianum seeds, send into screening machine, remove the impurity in raw material, obtain silybum marianum seed 1.93 tons, add 5 times amount water and make it be immersed in water, it is simultaneously introduced 3 weight % tea polyphenols, being warming up to 40-60 DEG C, stirring makes it fully infiltrate, and infiltration to water content reaches 32%, cross elimination excessive moisture, the silybum marianum seed that must infiltrate; The silybum marianum seed infiltrated is proceeded to freeze-drier, it is cooled to subzero 5-10 DEG C, maintain 15 minutes, temperature is adjusted to room temperature again keep 10-15 minute, then is cooled to subzero 5-10 DEG C, maintain 10 minutes, material after lyophilised process is proceeded to ultrasonic extractor, add equivalent water and 4% Silybum Marianum Gaertn Seed Oil, collaborative extraction 15 minutes, ultrasonic power 300w; Solution after process is put in high speed centrifuge and is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product; Add oil and weigh hargil and the 2 weight % tea polyphenols of 4%, temperature is increased to 80-100 degree, vacuum is maintained at about 96kPa, maintain 20 minutes, through flame filter press elimination hargil, enter odor removing pot deodorize, temperature 200-240 DEG C, 1-2 hour time, the straying quatity of live (open) steam with do not cause oils and fats splash be advisable; Oil is put into cooler and is cooled to room temperature, filter, pump into product tank. After testing, in product oil, the content of unsaturated fatty acid is 56.29%, and product yield is 96.12%.

Claims (2)

1. a preparation method for Silybum Marianum Gaertn Seed Oil, comprises the following steps:
(1) screening: take Herba Silybi mariani seed raw material, sends into screening machine, removes the impurity in raw material, such as earth, sandstone, weeds seed, ghost and dust etc.;
(2) infiltration: the silybum marianum seed after screening of weighing, adds 5-10 times amount water and makes it be immersed in water, be simultaneously introduced 1-5 weight % tea polyphenols, be warming up to 40-60 DEG C, and stirring makes it fully infiltrate, and crosses elimination excessive moisture, the silybum marianum seed that must infiltrate; Infiltration degree is that the water content making silybum marianum seed reaches more than 30%, it is preferable that 30-35%;
(3) frozen dried: the silybum marianum seed of infiltration is proceeded to freeze-drier, is cooled to subzero 5-10 DEG C, maintains 10-15 minute, then temperature is adjusted to room temperature maintenance 10-15 minute, then is cooled to subzero 5-10 DEG C, maintains 5-10 minute, is taken out by silybum marianum seed raw material;
(4) ultrasonic Treatment: the material after lyophilised process proceeds to ultrasonic extractor, adds water and the 3-5% Silybum Marianum Gaertn Seed Oil of 0.5-1 times of weight, collaborative extraction 10-20 minute, ultrasonic power 250-350w;
(5) centrifugation: the solution after process is put in high speed centrifuge and is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product;
(6) refine: add hargil and the 2-3 weight % tea polyphenols of oil weight 3-6%, temperature is increased to 80-100 degree, vacuum is maintained at about 96kPa, maintain 20-30 minute, through flame filter press elimination hargil, enter odor removing pot deodorize, temperature 200-240 DEG C, 1-2 hour time, the straying quatity of live (open) steam with do not cause oils and fats splash be advisable;
(7) oil is put into cooler and is cooled to room temperature, filter, pump into product tank.
2. the Silybum Marianum Gaertn Seed Oil that said method prepares.
CN201610052374.7A 2016-01-27 2016-01-27 A method of extracting Silybum Marianum Gaertn Seed Oil Active CN105623839B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107164087A (en) * 2017-07-18 2017-09-15 安徽省华银茶油有限公司 A kind of method that utilization chitosan extracts camellia seed oil with medical stone Combined Processing
CN107674755A (en) * 2017-11-22 2018-02-09 五河县顺鹏农副产品有限公司 A kind of rapid extracting method of wheat-germ oil
CN108753439A (en) * 2018-05-30 2018-11-06 无限极(中国)有限公司 A kind of oil plant squeezes the method for grease and the application of the grease

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102911791A (en) * 2012-09-25 2013-02-06 常州亚环环保科技有限公司 Method for extracting gardenia essential oil
CN103849468A (en) * 2014-03-12 2014-06-11 青海清华博众生物技术有限公司 Garlic essential oil extraction method
CN104194913A (en) * 2014-09-26 2014-12-10 东北农业大学 Method for preparing silybum marianum oil with aqueous enzymatic method
CN104450172A (en) * 2014-12-10 2015-03-25 江苏中兴药业有限公司 Fructussilybi oil extraction method
CN107698572A (en) * 2016-07-29 2018-02-16 内蒙古昶辉生物科技股份有限公司 A kind of extracting method of silymarin

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102911791A (en) * 2012-09-25 2013-02-06 常州亚环环保科技有限公司 Method for extracting gardenia essential oil
CN103849468A (en) * 2014-03-12 2014-06-11 青海清华博众生物技术有限公司 Garlic essential oil extraction method
CN104194913A (en) * 2014-09-26 2014-12-10 东北农业大学 Method for preparing silybum marianum oil with aqueous enzymatic method
CN104450172A (en) * 2014-12-10 2015-03-25 江苏中兴药业有限公司 Fructussilybi oil extraction method
CN107698572A (en) * 2016-07-29 2018-02-16 内蒙古昶辉生物科技股份有限公司 A kind of extracting method of silymarin

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107164087A (en) * 2017-07-18 2017-09-15 安徽省华银茶油有限公司 A kind of method that utilization chitosan extracts camellia seed oil with medical stone Combined Processing
CN107674755A (en) * 2017-11-22 2018-02-09 五河县顺鹏农副产品有限公司 A kind of rapid extracting method of wheat-germ oil
CN108753439A (en) * 2018-05-30 2018-11-06 无限极(中国)有限公司 A kind of oil plant squeezes the method for grease and the application of the grease

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Registration number: Y2022150000027

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Pledgee: Agricultural Bank of China Limited Helingeer County sub branch

Pledgor: INNER MONGOLIA CHANGHUI BIOTECHNOLOGY CO.,LTD.

Registration number: Y2022150000027

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Denomination of invention: A Method for Extracting Silymarin Oil

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Pledgee: China Minsheng Banking Corp Hohhot branch

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Denomination of invention: A Method for Extracting Silymarin Oil

Effective date of registration: 20231101

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Pledgee: China Minsheng Banking Corp Hohhot branch

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Registration number: Y2023150000154