CN105623839B - A method of extracting Silybum Marianum Gaertn Seed Oil - Google Patents

A method of extracting Silybum Marianum Gaertn Seed Oil Download PDF

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Publication number
CN105623839B
CN105623839B CN201610052374.7A CN201610052374A CN105623839B CN 105623839 B CN105623839 B CN 105623839B CN 201610052374 A CN201610052374 A CN 201610052374A CN 105623839 B CN105623839 B CN 105623839B
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silybum marianum
oil
seed
minutes
seed oil
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CN105623839A (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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Inner Mongolia Changhui Biotechnology 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 present invention relates to a kind of from silybum marianum seed obtains the preparation method of Silybum Marianum Gaertn Seed Oil.The process employs infiltration-freeze-drying-ultrasonic wave extraction methods to greatly improve product yield, and unsaturated fatty acid content is up to 50% or more in oil product, basic free of losses, yield is up to 95% or more, and oil colours is limpid, full aroma is extremely suitable for industrial production, and product can be directly used as health-care edible oil or in health-oriented products.

Description

A method of extracting Silybum Marianum Gaertn Seed Oil
Technical field
The present invention relates to the methods for extracting Silybum Marianum Gaertn Seed Oil, extract powder-refining with water from milk thistle seed more particularly, to one kind The method of Ji oil.
Background technique
Composite family Silybum milk thistle (Silybum marianum) is the plant for originating in West Europe and north African, to soil, Moisture requirement is not tight, sandy beach, salt-soda soil can plant, it is adaptable, introduce China after in Shaanxi, Gansu, Heilungkiang and river There are commerial growing in the provinces such as north, are mainly used for extracting silymarin.Silymarin is because the effect of its Hepatoprotective cholagogue is known in people, extensively It is general to be used to prevent and treat cardiovascular and cerebrovascular disease.But silybum marianum seed is in addition to containing other than silymarin, also containing a large amount of Silybum Marianum Gaertn Seed Oils, and 2014 National health State Family Planning Commission on April 16, approval silybum marianum seed oil is new raw-food material.
The main component of Silybum Marianum Gaertn Seed Oil (Silybum marianum Seed oil) is unsaturated fatty acid, i.e. linoleic acid (content 45%).Linoleic acid receives greatly to pursue recently as fatty acid needed by human.Silybum Marianum Gaertn Seed Oil oil is good, belongs to natural, nothing The green plants oil of pollution, can be used as family cooking, and long-term consumption can play liver protection, dirty, improving eyesight the health-care effect of shield, have drop Low cholesterol, for preventing and treating atherosclerosis, hypertension, coronary heart disease, softening cardiovascular and cerebrovascular, removing the effect of blood rubbish.
It is still not deep enough to the research of the production preparation of Silybum Marianum Gaertn Seed Oil at present, generally using silybum marianum seed as raw material, take straight The techniques such as cold press, filtering are connect to be made.But this method only passes through natural sedimentation filtering, oil product acid value is high, gastronomical process oil smoke Greatly, edible flavor is poor, and oil yield is low, and cake Residual oil is high.There are also water substitution is used, make cell rupture by impregnating, moisture is impregnated with To inside intact cell, expand gelinite, seed is fried in heating, flows out intracellular oil body, divides oil through succusion It separates out and, this method keeps oil body outflow complete, and can generate special fragrance, but extraction efficiency without squeezing, being not necessarily to solvent Not enough, the whole process takes a long time.There are also use extract by solvents, but due to can dissolve grease solvent be mostly that toxicity is organic molten Agent, thus the Silybum Marianum Gaertn Seed Oil that this method extracts is typically used as iundustrial oil, and can not eat.Recently dioxy is also developed Change the methods of carbon supercritical extract, aqueous enzymatic method extraction etc., separative efficiency is high, but still exist or enterprise at high cost or time compared with The disadvantages of long etc..
Therefore, for drawbacks described above existing for the method for preparing Silybum Marianum Gaertn Seed Oil in the prior art and deficiency, mesh of the invention The preparation method for being to provide a kind of new Silybum Marianum Gaertn Seed Oil, separative efficiency is high, and excellent product quality, is suitable for industrialized production.
Summary of the invention
The present invention provides a kind of from silybum marianum seed extracts the preparation method of high-purity Silybum Marianum Gaertn Seed Oil, including following step It is rapid:
(1) screen: taking milk thistle seed raw material, be sent into screening machine, remove the impurity in raw material, as soil, sandstone, weeds seed, Ghost and dust etc.;
(2) infiltrate: the silybum marianum seed after weighing screening, water is measured in 5-10 times of addition impregnates it in water, while 1-5 is added Weight % tea polyphenols are warming up to 40-60 DEG C, and stirring infiltrates it sufficiently, filters off excessive moisture, the silybum marianum seed that must be infiltrated; Infiltration degree is that the water content of silybum marianum seed is made to reach 30% or more, preferably 30-35%;
(3) frozen dried: being transferred to freeze-drier for the silybum marianum seed of infiltration, is cooled to subzero 5-10 DEG C, maintains 10-15 points Clock, then adjust the temperature to room temperature and kept for 10-15 minutes, then be cooled to subzero 5-10 DEG C, it maintains 5-10 minutes, by silybum marianum seed original Material takes out;
(4) ultrasonication: treated that material is transferred to ultrasonic extractor by freeze-dried, and the water of 0.5-1 times of weight is added And 3-5% Silybum Marianum Gaertn Seed Oil, collaboration are extracted 10-20 minutes, ultrasonic power 250-350w;
(5) be centrifugated: will treated that solution is put into supercentrifuge is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product;
(6) refine: the carclazyte and 2-3 weight % tea polyphenols of oil weight 3-6% is added, temperature is increased to 80-100 degree, and vacuum degree is protected It holds in 96kPa or so, maintains 20-30 minutes, filter off carclazyte through flame filter press, enter odor removing pot and be deodorized, 200-240 DEG C of temperature, Time 1-2 hour, the straying quatity of direct steam is not to cause grease splashing to be advisable;
(7) oil is put into cooler to be cooled to room temperature, filters, be pumped into product tank.
The present invention also provides Silybum Marianum Gaertn Seed Oils made from the above method.
Silybum Marianum Gaertn Seed Oil product oil colours made from the method for the present invention is limpid, full aroma, and up to 95% or more, nothing makes product yield With organic solvent, it is suitable for very much health-care edible oil or health-oriented products.
The present invention proposes that addition water soluble ingredient tea is more during liquefaction during the liquefaction of Silybum Marianum Gaertn Seed Oil for the first time Phenol plays protective agent effect, avoids unsaturated fatty acid in Silybum Marianum Gaertn Seed Oil from receiving destruction, and use infiltration-freeze-drying-ultrasound The method that wave extracts greatly improves product yield, and guarantees that unsaturated fatty acid content is up to 50% or more in oil product, substantially Free of losses, and yield is up to 95% or more.
Subordinate list is unsaturated fatty acid content and product yield in the different obtained product oils of preparation method.
Method Unsaturated fatty acid content (%) Product yield (%)
1 method of the embodiment of the present invention 55.58 95.87
Control 1 25.29 89.86
Control 2 47.64 81.12
Control 3 46.17 78.57
Control 4 44.95 75.50
Control 5 41.58 92.14
Wherein, contrast method 1 is method identical with the embodiment of the present invention 1, and difference is to be added without tea polyphenols;Control side Method 2 is method identical with the embodiment of the present invention 1, and difference is that the amount of moisture infiltrated is 20-25%;Contrast method 3 be and this hair The identical method of bright embodiment 1, difference are not including immersion step;Contrast method 4 is side identical with the embodiment of the present invention 1 Method, difference are not including frozen dried step;Contrast method 5 is to extract after refining broken silybum marianum seed through supercritical carbon dioxide Follow the example of extraction Silybum Marianum Gaertn Seed Oil.
As can be seen from the table, the content of unsaturated fatty acid can greatly be influenced by being added without tea polyphenols, and tea polyphenols exist Antioxidation is both played in entire method, simultaneously because its water-soluble speciality, is easy to remove, although those skilled in the art The property and performance of known tea polyphenols, but the present inventor does not see that the ingredient is added during liquefaction to improve finished product in someone The content of oil weight unsaturated fatty acid, meanwhile, inventors have also discovered that not being arbitrary antioxidant can be added to this hair Bright method, such as vitamin E etc. are then not particularly suited for the method for the present invention.In addition, of the present invention cross water content infiltration Method and step of freeze drying have a significant impact for the property of oil product, it is generally recognized that if moisture is excessively high, fuel-displaced oil colours is shallow, foam More, if very too low, oil colours is deep and muddy, there is the powdery impurity of suspension.But present invention discover that improving containing for silybum marianum seed Water is very beneficial for ultrasonic wave extraction step after freeze-drying up to 30% or more, not only will not influence the property of oil product, and greatly Ground improves oil productivity.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution is clearly and completely described, it is clear that described embodiments are some of the embodiments of the present invention, rather than complete Portion's possibility.Those of ordinary skill in the art's obtained every other embodiment in the case where not making creative work, all falls Enter in protection scope of the present invention.
Embodiment 1
10 tons of silybum marianum seeds are sent into screening machine, remove the impurity in raw material, obtain 9.95 tons of silybum marianum seed, 10 times of amounts are added Water impregnates it in water, while 5 weight % tea polyphenols are added, and is warming up to 40-60 DEG C, and stirring infiltrates it sufficiently, and infiltration is to containing Water filters off excessive moisture up to 35%, the silybum marianum seed that must be infiltrated;The silybum marianum seed infiltrated is transferred to freeze-drier, is dropped Temperature maintains 15 minutes to subzero 5-10 DEG C, then adjusts the temperature to room temperature and kept for 10-15 minutes, then be cooled to subzero 5-10 DEG C, ties up It holds 10 minutes, by freeze-dried treated material is transferred to ultrasonic extractor, equivalent amount of water is added and 5% Silybum Marianum Gaertn Seed Oil, collaboration mention It takes 15 minutes, ultrasonic power 350w;Will treated that solution is put into supercentrifuge is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil Crude product;Addition oil weighs 5% carclazyte and 3 weight % tea polyphenols, temperature are increased to 80-100 degree, and vacuum degree is maintained at 96kPa or so, It maintains 20 minutes, filters off carclazyte through flame filter press, enter odor removing pot deodorization, 200-240 DEG C of temperature, time 1-2 hour directly steams The straying quatity of vapour is not to cause grease splashing to be advisable;Oil is put into cooler to be cooled to room temperature, filters, is pumped into product tank.Through It detects, the content of unsaturated fatty acid is 55.58% in product oil, product yield 95.87%.
Embodiment 2
2 tons of silybum marianum seeds are sent into screening machine, remove the impurity in raw material, obtain 1.93 tons of silybum marianum seed, 5 times of amount water are added It impregnates it in water, while 3 weight % tea polyphenols is added, be warming up to 40-60 DEG C, stirring infiltrates it sufficiently, infiltrates to aqueous Amount filters off excessive moisture, the silybum marianum seed that must be infiltrated up to 32%;The silybum marianum seed infiltrated is transferred to freeze-drier, is cooled down It to subzero 5-10 DEG C, maintains 15 minutes, then adjusts the temperature to room temperature and kept for 10-15 minutes, then be cooled to subzero 5-10 DEG C, maintain 10 minutes, by freeze-dried treated material is transferred to ultrasonic extractor, equivalent amount of water and 4% Silybum Marianum Gaertn Seed Oil is added, collaboration is extracted 15 minutes, ultrasonic power 300w;Will treated that solution is put into supercentrifuge is centrifuged 20 minutes, it is thick to obtain Silybum Marianum Gaertn Seed Oil Product;Addition oil weighs 4% carclazyte and 2 weight % tea polyphenols, temperature are increased to 80-100 degree, and vacuum degree is maintained at 96kPa or so, dimension It holds 20 minutes, filters off carclazyte through flame filter press, enter odor removing pot and be deodorized, 200-240 DEG C of temperature, time 1-2 hour, direct steam Straying quatity with do not cause grease splashing be advisable;Oil is put into cooler to be cooled to room temperature, filters, is pumped into product tank.Through examining It surveys, the content of unsaturated fatty acid is 56.29% in product oil, product yield 96.12%.

Claims (2)

1. a kind of preparation method of Silybum Marianum Gaertn Seed Oil, is made of following steps:
(1) screen: taking milk thistle seed raw material, be sent into screening machine, remove the impurity in raw material, including soil, sandstone, weeds seed, sky Shell and dust;
(2) infiltrate: the silybum marianum seed after weighing screening, water is measured in 5-10 times of addition impregnates it in water, while 1-5 weight is added % tea polyphenols are measured, are warming up to 40-60 DEG C, stirring infiltrates it sufficiently, filters off excessive moisture, the silybum marianum seed that must be infiltrated; Infiltration degree is that the water content of silybum marianum seed is made to reach 30-35%;
(3) frozen dried: being transferred to freeze-drier for the silybum marianum seed of infiltration, is cooled to subzero 5-10 DEG C, maintains 10-15 minutes, then It adjusts the temperature to room temperature to be kept for 10-15 minutes, then is cooled to subzero 5-10 DEG C, maintain 5-10 minutes, silybum marianum seed raw material is taken Out;(4) ultrasonication: treated that material is transferred to ultrasonic extractor by freeze-dried, be added 0.5-1 times of weight water and 3-5% Silybum Marianum Gaertn Seed Oil, collaboration are extracted 10-20 minutes, ultrasonic power 250-350w;
(5) be centrifugated: will treated that solution is put into supercentrifuge is centrifuged 20 minutes, obtain Silybum Marianum Gaertn Seed Oil crude product;
(6) refine: the carclazyte and 2-3 weight % tea polyphenols of oil weight 3-6% is added, temperature is increased to 80-100 degree, and vacuum degree is kept It in 96kPa, maintains 20-30 minutes, filters off carclazyte through flame filter press, enter odor removing pot and be deodorized, 200-240 DEG C of temperature, time 1-2 Hour, the straying quatity of direct steam is not to cause grease splashing to be advisable;
(7) oil is put into cooler to be cooled to room temperature, filters, be pumped into product tank.
2. the Silybum Marianum Gaertn Seed Oil as made from claim 1 method.
CN201610052374.7A 2016-01-27 2016-01-27 A method of extracting Silybum Marianum Gaertn Seed Oil Active CN105623839B (en)

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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)

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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

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