CN104450172B - A kind of extracting method of Silybum Marianum Gaertn Seed Oil - Google Patents
A kind of extracting method of Silybum Marianum Gaertn Seed Oil Download PDFInfo
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- CN104450172B CN104450172B CN201410751965.4A CN201410751965A CN104450172B CN 104450172 B CN104450172 B CN 104450172B CN 201410751965 A CN201410751965 A CN 201410751965A CN 104450172 B CN104450172 B CN 104450172B
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- oil
- filter residue
- milk thistle
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- silybum marianum
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- 235000010841 Silybum marianum Nutrition 0.000 title claims abstract description 45
- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 24
- 244000272459 Silybum marianum Species 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 235000019198 oils Nutrition 0.000 claims abstract description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000605 extraction Methods 0.000 claims abstract description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003208 petroleum Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 125000001033 ether group Chemical group 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims description 50
- 239000000706 filtrate Substances 0.000 claims description 24
- 241000320380 Silybum Species 0.000 claims description 22
- 239000000284 extract Substances 0.000 claims description 18
- 229940096402 milk thistle seed Drugs 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 13
- 238000010992 reflux Methods 0.000 claims description 11
- 150000002170 ethers Chemical class 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000010496 thistle oil Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims 1
- 238000009736 wetting Methods 0.000 abstract 1
- SEBFKMXJBCUCAI-UHFFFAOYSA-N NSC 227190 Natural products C1=C(O)C(OC)=CC(C2C(OC3=CC=C(C=C3O2)C2C(C(=O)C3=C(O)C=C(O)C=C3O2)O)CO)=C1 SEBFKMXJBCUCAI-UHFFFAOYSA-N 0.000 description 12
- SEBFKMXJBCUCAI-HKTJVKLFSA-N silibinin Chemical compound C1=C(O)C(OC)=CC([C@@H]2[C@H](OC3=CC=C(C=C3O2)[C@@H]2[C@H](C(=O)C3=C(O)C=C(O)C=C3O2)O)CO)=C1 SEBFKMXJBCUCAI-HKTJVKLFSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 229960004245 silymarin Drugs 0.000 description 11
- 235000017700 silymarin Nutrition 0.000 description 11
- CYGIJEJDYJOUAN-UHFFFAOYSA-N Isosilychristin Natural products C1=C(O)C(OC)=CC(C2C3C=C(C4C(C3=O)(O)OCC42)C2C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 CYGIJEJDYJOUAN-UHFFFAOYSA-N 0.000 description 8
- MZBGBHVFCYCYLX-UHFFFAOYSA-N Silydianin Natural products COc1cc(ccc1O)C2C3COC4(O)C3C=C(C5Oc6cc(O)cc(O)c6C(=O)C5O)C2C4=O MZBGBHVFCYCYLX-UHFFFAOYSA-N 0.000 description 4
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- CYGIJEJDYJOUAN-JSGXPVSSSA-N silydianin Chemical compound C1=C(O)C(OC)=CC([C@H]2[C@H]3C=C([C@@H]4[C@@](C3=O)(O)OC[C@@H]42)[C@@H]2[C@H](C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 CYGIJEJDYJOUAN-JSGXPVSSSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- RIAZZJBPJQWPIS-UHFFFAOYSA-N Silychristin Natural products COc1cc(ccc1O)C2OC3C(C=C(C=C3O)C4Oc5cc(O)cc(O)c5C(=O)C4O)C2CO RIAZZJBPJQWPIS-UHFFFAOYSA-N 0.000 description 3
- 230000036760 body temperature Effects 0.000 description 3
- BMLIIPOXVWESJG-LMBCONBSSA-N silychristin Chemical compound C1=C(O)C(OC)=CC([C@H]2[C@@H](C3=C(C(=CC(=C3)[C@@H]3[C@H](C(=O)C4=C(O)C=C(O)C=C4O3)O)O)O2)CO)=C1 BMLIIPOXVWESJG-LMBCONBSSA-N 0.000 description 3
- BMLIIPOXVWESJG-UHFFFAOYSA-N silychristin A Natural products C1=C(O)C(OC)=CC(C2C(C3=C(C(=CC(=C3)C3C(C(=O)C4=C(O)C=C(O)C=C4O3)O)O)O2)CO)=C1 BMLIIPOXVWESJG-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 208000004930 Fatty Liver Diseases 0.000 description 2
- 206010019708 Hepatic steatosis Diseases 0.000 description 2
- 206010019799 Hepatitis viral Diseases 0.000 description 2
- FDQAOULAVFHKBX-UHFFFAOYSA-N Isosilybin A Natural products C1=C(O)C(OC)=CC(C2C(OC3=CC(=CC=C3O2)C2C(C(=O)C3=C(O)C=C(O)C=C3O2)O)CO)=C1 FDQAOULAVFHKBX-UHFFFAOYSA-N 0.000 description 2
- 235000012000 cholesterol Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 208000010706 fatty liver disease Diseases 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 208000006454 hepatitis Diseases 0.000 description 2
- 231100000283 hepatitis Toxicity 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 231100000240 steatosis hepatitis Toxicity 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- FDQAOULAVFHKBX-KMRPREKFSA-N (+)-Isosilybin A Natural products C1=C(O)C(OC)=CC([C@@H]2[C@H](OC3=CC(=CC=C3O2)[C@@H]2[C@@H](C(=O)C3=C(O)C=C(O)C=C3O2)O)CO)=C1 FDQAOULAVFHKBX-KMRPREKFSA-N 0.000 description 1
- FDQAOULAVFHKBX-HKTJVKLFSA-N (2r,3r)-3,5,7-trihydroxy-2-[(2r,3r)-2-(4-hydroxy-3-methoxyphenyl)-3-(hydroxymethyl)-2,3-dihydro-1,4-benzodioxin-6-yl]-2,3-dihydrochromen-4-one Chemical compound C1=C(O)C(OC)=CC([C@@H]2[C@H](OC3=CC(=CC=C3O2)[C@@H]2[C@H](C(=O)C3=C(O)C=C(O)C=C3O2)O)CO)=C1 FDQAOULAVFHKBX-HKTJVKLFSA-N 0.000 description 1
- QYCJAWYDGRZSTO-IRLTUAEKSA-N (2r,3r)-3,5,7-trihydroxy-2-[(2r,3s)-7-hydroxy-2-(4-hydroxy-3-methoxyphenyl)-3-(hydroxymethyl)-2,3-dihydro-1-benzofuran-4-yl]-2,3-dihydrochromen-4-one Chemical compound C1=C(O)C(OC)=CC([C@H]2[C@@H](C3=C(C(=CC=C3[C@@H]3[C@H](C(=O)C4=C(O)C=C(O)C=C4O3)O)O)O2)CO)=C1 QYCJAWYDGRZSTO-IRLTUAEKSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 241000189115 Catananche Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010056328 Hepatic ischaemia Diseases 0.000 description 1
- 206010020466 Hunger Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- KDMGQPNVTKUNHV-UHFFFAOYSA-N Isosilybin Natural products C1=C(O)C(OC)=CC=C1C1C(CO)OC2=CC=C(C3C(C(=O)C4=C(O)C=C(O)C=C4O3)O)C=C2O1 KDMGQPNVTKUNHV-UHFFFAOYSA-N 0.000 description 1
- 241000254023 Locusta Species 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 241000904014 Pappus Species 0.000 description 1
- 206010063837 Reperfusion injury Diseases 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- VLGROHBNWZUINI-UHFFFAOYSA-N Silybin Natural products COc1cc(ccc1O)C2OC3C=C(C=CC3OC2CO)C4Oc5cc(O)cc(O)c5C(=O)C4O VLGROHBNWZUINI-UHFFFAOYSA-N 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 208000037906 ischaemic injury Diseases 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000006651 lactation Effects 0.000 description 1
- -1 linoleic acid, leukotrienes Chemical class 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 229940106589 milk thistle seed extract Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229940043175 silybin Drugs 0.000 description 1
- 235000014899 silybin Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 201000001862 viral hepatitis Diseases 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
- C11B13/02—Recovery of fats, fatty oils or fatty acids from waste materials from soap stock
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of extracting method of Silybum Marianum Gaertn Seed Oil, comprise the following steps：Fried dry, screw oil expeller oil expression after cleaning, shelling, broken, petroleum ether backflow degreasing, EtOH Sonicate extraction, water wetting, obtain Silybum Marianum Gaertn Seed Oil after merging the oil cake that oil ether moiety, ethanolic moiety and oil expression obtain.This extracting method technique is simple, can obtain the Silybum Marianum Gaertn Seed Oil that loss of effective components is few, quality is high, cost is low.
Description
Technical field
The present invention relates to vegetable oil field, specially a kind of extracting method of the Silybum Marianum Gaertn Seed Oil with plurality of health care functions.
Background technology
Milk thistle, 1 year or biennial catananche, mainly with seed for.Stem is upright, high 30~120cm, more
Branch, basal leaf is big, rosette-stape, glossy above leaf, there is many milky spots；Achene ellipse, brown, surface has vertical
Line, body of gland projection.Southern Europe, north African are originated in, Asia also has, and there is introducing and planting in China.Vegetables food is made with leaf and tender shoots earliest in Europe
With, existing more than 2000 years history, while be used as by the use of seed and treat liver, spleen, disease of digestive tract and the herbal medicine for promoting lactation.Milk thistle
Main component have silymarin (silybin) A and silymarin B, silydianin (isosilybin) A, silydianin
B, Silychristin (silychristin), different Silychristin (isosilychristin), silydianin (silydianin), with
On be Flavonoid substances, be often commonly referred to as silymarin (class)；Separately containing tyrasamine, 5,7- dihydroxy chromogen ketones etc..Silymarin-group
(milk thistle seed extract) is to chemically hepatitis, fatty liver, hepatonecrosis, radical damage, liver ischemic injury, viral
Hepatitis has good clinical effectiveness.Silymarin solubility very little in water, the extraction for silymarin, is typically used
Organic solvent is extracted.
Also there is the insatiable hungers such as very high oleic acid, linoleic acid, leukotrienes in oily containing more than 30% oil in milk thistle seed
And aliphatic acid, these compositions have reduction cholesterol, prevent artery sclerosis etc. from acting on.And can equally organic solvent be used to carry out
Extraction.
But at present, prior art, which prepares Silybum Marianum Gaertn Seed Oil, be present, the acetone or ethyl acetate such as used has
Solvent recovery is incomplete；Yield is relatively low；Extraction cost height etc.
The content of the invention
Goal of the invention：To solve problems of the prior art, a kind of loss of effective components of present invention offer is few, quality
The extracting method of Silybum Marianum Gaertn Seed Oil high, cost is low.
Technical scheme：To realize above-mentioned technical purpose, the present invention provides a kind of extracting method of Silybum Marianum Gaertn Seed Oil, including as follows
Step：
(1) clear up：Clean ripe milk thistle seed.General milk thistle blooms at the beginning of 7 months successively from first arrival in May, a head
Locusta from bloom to fruit it is ripe need to 25~30 days, when the withered and yellow inward curl of bract parts a little open into cylinder, top pappus, indicate seed
It is ripe.Ripe milk thistle seed is selected, silt is screened out, is cleaned with clear water, if not cleaning carefully, can be accelerated in oil press
The abrasion of portion's parts, oil yield is reduced, or even cause failure and accident.
(2) shell：Milk thistle seed after cleaning is placed in hulling machine and removes shell, can be carried by being squeezed again after shelling
High productive capacity and oil yield；
(3) crush：Milk thistle seed after shelling is crushed at normal temperatures, obtains coarse powder.Although some greases can be with whole
Expect into squeezing, but squeezed again after crushing, roll embryo, oil yield can be significantly improved.
(4) degreasing：In 60~80 DEG C of backflows after the coarse powder of step (3) is mixed with the petroleum ether of 4~6 times of 30~60 DEG C of amounts
30~60min is extracted, filtrate I and filter residue I is obtained after filtering, the petroleum ethers that filter residue I is reused to 4~6 times of 30~60 DEG C of amounts mix
Close after 60~80 DEG C of 30~60min of refluxing extraction, filtrate II and filter residue II obtained after filtering, filtrate I and filtrate II are merged,
It is concentrated under reduced pressure after removing petroleum ether and obtains milk thistle oil ether moiety.This step is to first obtain refined fine grinding with petroleum ether
Ji oil.The introducing of the step, the efficiency of subsequent extracted step can not only be greatly improved, and the damage of oil expression step can be reduced
Consumption, improve the effect of oil expression.In addition, inventor is found surprisingly that using petroleum ether refluxing extraction compared with centrifuging or standing, energy
Enough greatly improve the yield of refined oil.
(5) extract：Filter residue II is extracted with 60~80wt% EtOH Sonicates, the time is 60~80min, extraction time 2~4
It is secondary, merge extract solution, be concentrated under reduced pressure after removing ethanol and obtain milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby.Pass through
Extracted with EtOH Sonicate, the higher silymarin extract of purity can be obtained, and height can be avoided before stir-fry and oil expression is steamed
Destruction of the temperature for silymarin isoreactivity composition, retains active component important in Silybum Marianum Gaertn Seed Oil.By ultrasound, heat backflow and
The comparison of soxhlet extraction, it is found that the used time of ultrasonic extraction is short, extraction efficiency is high.
(6) steam and fry：Filter residue III water is soaked, is then stir-fried again through frying pan to drying, obtains filter residue IV.Steam in advance
Frying, which can make oil plant reach technological requirement, enters to squeeze moisture and temperature, can greatly improve oil yield.
(7) extract oil：Filter residue IV after step (6) steaming is fried is squeezed to obtain oil cake with screw oil expeller.Just go out from frying pan
The oil cake filter residue IV temperature come is about 108 DEG C, and oil yield can equally be improved while hot by squeezing.
(8) the milk thistle oil ether moiety for obtaining step (4), the milk thistle ethanolic moiety and step that step (5) obtains
(7) oil cake obtained, which merges, to be mixed, and obtains Silybum Marianum Gaertn Seed Oil.
Preferably, in step (3), the particle diameter of coarse powder is 40~60 mesh.It is highly preferred that the particle diameter of coarse powder is 60 mesh.
Preferably, the degreasing condition of step (4) is：Use 70 DEG C of refluxing extractions after (30-60 DEG C) mixing of 6 times of amount petroleum ethers
60min, filtrate I and filter residue I is obtained after filtering, filter residue I is reused into 70 DEG C of backflows after 6 times of (30-60 DEG C) of amount petroleum ethers mix
60min is extracted, filtrate II and filter residue II are obtained after filtering, filtrate I and filtrate II are merged, is concentrated under reduced pressure after removing petroleum ether and obtains
To milk thistle oil ether moiety.
Preferably, in step (5), ethanol and filter residue II mass ratio are 8~10.It is highly preferred that ethanol is with filter residue II's
Mass ratio is 10, and the optimum condition of extraction is：First using 10 times of amount 80% EtOH Sonicate extraction filter residue II, time 60min, carry
Take number 2 times, merge extract solution, be concentrated under reduced pressure after removing ethanol and obtain milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby
With.
Preferably, in step (6), water and filter residue III mass ratio are 0.2~1.It is highly preferred that the matter of water and filter residue III
Measure ratio 0.5.
Specifically, in step (7), oil expression concretely comprises the following steps：After screw oil expeller is dallied 3~5 minutes, by step 6
Obtained filter residue IV is fed while hot, and starting squeezing when organism temperature reaches 70~80 DEG C obtains oil cake.Preferably, the step of oil expression
Suddenly it is：After screw oil expeller is dallied 3 minutes, the filter residue IV that step 6 obtains is fed while hot, when organism temperature reaches 70 DEG C
Start squeezing and obtain oil cake.
Beneficial effect：Compared with prior art, flowing back in method of the invention, ultrasound, screw oil-extracting etc. are ripe
Technology, simple to operate, easy to get started, but obtained higher yield and the good product of quality.The fine grinding that this method extracts
Ji oil is rich in silymarin isoreactivity composition, and chemically hepatitis, fatty liver, hepatonecrosis, radical damage, hepatic ischemia/reperfusion injury are damaged
Wound, virus hepatitis have good clinical effectiveness, while can also reduce cholesterol, atherosclerosis, have and control
Treat the effect of hypertension.
Embodiment
The present invention is further detailed explanation by the following examples, but protection scope of the present invention is not by specific reality
Any restrictions of example are applied, but are defined in the claims.
Embodiment 1
A kind of extracting method of Silybum Marianum Gaertn Seed Oil, comprises the following steps：
(1) clear up：Ripe milk thistle seed 10kg is selected, silt is screened out, is cleaned with clear water；
(2) shell：Milk thistle seed after cleaning is placed in hulling machine and removes shell；
(3) crush：It will at normal temperatures be crushed except the milk thistle seed after shell, obtain the mesh of coarse powder 60；
(4) degreasing：Above-mentioned coarse powder is used into 70 DEG C of refluxing extraction 60min after (30-60 DEG C) mixing of 6 times of amount petroleum ethers, mistake
Filtrate I and filter residue I is obtained after filter, filter residue I is reused into 70 DEG C of refluxing extractions after 6 times of (30-60 DEG C) of amount petroleum ethers mix
60min, filtrate II and filter residue II are obtained after filtering, filtrate I and filtrate II are merged, be concentrated under reduced pressure after removing petroleum ether and obtain water
Fly Ji oil ether moiety；
(5) extract：Using 10 times of amount 80% EtOH Sonicate extraction filter residue II, time 60min, extraction time 2 times, merge
Extract solution, it is concentrated under reduced pressure after removing ethanol and obtains milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby；
(6) steam and fry：Filter residue III is soaked with the water of 0.5 times of amount, is then stir-fried again through frying pan to drying, obtains filter residue
IV；
(7) extract oil：After screw oil expeller is dallied 3 minutes, the filter residue IV that step 6 obtains is fed while hot, when body temperature
Degree starts squeezing when reaching 70 DEG C and obtains oil cake；
(8) the milk thistle oil ether moiety for obtaining step 4, the milk thistle ethanolic moiety and step 7 that step 5 obtains obtain
Oil cake merge mix, obtain Silybum Marianum Gaertn Seed Oil.
After testing, oily 2.42kg, oil yield 24.2% are obtained；Contain silymarin 15.69% in the Silybum Marianum Gaertn Seed Oil.This product is yellow
Color is transparent, free from admixture, quality better, fragrant odour.
Embodiment 2
A kind of extracting method of Silybum Marianum Gaertn Seed Oil, comprises the following steps：
(1) clear up：Ripe milk thistle seed 10kg is selected, silt is screened out, is cleaned with clear water；
(2) shell：Milk thistle seed after cleaning is placed in hulling machine and removes shell；
(3) crush：It will at normal temperatures be crushed except the milk thistle seed after shell, obtain the mesh of coarse powder 40；
(4) degreasing：Above-mentioned coarse powder is used into 70 DEG C of refluxing extraction 40min after (30-60 DEG C) mixing of 5 times of amount petroleum ethers, mistake
Filtrate I and filter residue I is obtained after filter, filter residue I is reused into 70 DEG C of refluxing extractions after 5 times of (30-60 DEG C) of amount petroleum ethers mix
40min, filtrate II and filter residue II are obtained after filtering, filtrate I and filtrate II are merged, be concentrated under reduced pressure after removing petroleum ether and obtain water
Fly Ji oil ether moiety；
(5) extract：Using 8 times of amount 70% EtOH Sonicate extraction filter residue II, time 80min, extraction time 3 times, merge
Extract solution, it is concentrated under reduced pressure after removing ethanol and obtains milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby；
(6) steam and fry：Filter residue III is soaked with the water of 0.2 times of amount, is then stir-fried again through frying pan to drying, obtains filter residue IV；
(7) extract oil：After screw oil expeller is dallied 3 minutes, the filter residue IV that step 6 obtains is fed while hot, when body temperature
Degree starts squeezing when reaching 70 DEG C and obtains oil cake；
(8) the milk thistle oil ether moiety for obtaining step 4, the milk thistle ethanolic moiety and step 7 that step 5 obtains obtain
Oil cake merge mix, obtain Silybum Marianum Gaertn Seed Oil.
After testing, oily 2.34kg, oil yield 23.4% are obtained；Contain silymarin 16.85% in the Silybum Marianum Gaertn Seed Oil.This product is yellow
Color is transparent, free from admixture, quality better, fragrant odour.
Embodiment 3
A kind of extracting method of Silybum Marianum Gaertn Seed Oil, comprises the following steps：
(1) clear up：Ripe milk thistle seed 10kg is selected, silt is screened out, is cleaned with clear water；
(2) shell：Milk thistle seed after cleaning is placed in hulling machine and removes shell；
(3) crush：It will at normal temperatures be crushed except the milk thistle seed after shell, obtain the mesh of coarse powder 60；
(4) degreasing：Above-mentioned coarse powder is used into 80 DEG C of refluxing extraction 30min after (30-60 DEG C) mixing of 4 times of amount petroleum ethers, mistake
Filtrate I and filter residue I is obtained after filter, filter residue I is reused into 80 DEG C of refluxing extractions after 4 times of (30-60 DEG C) of amount petroleum ethers mix
30min, filtrate II and filter residue II are obtained after filtering, filtrate I and filtrate II are merged, be concentrated under reduced pressure after removing petroleum ether and obtain water
Fly Ji oil ether moiety；
(5) extract：Using 10 times of amount 75% EtOH Sonicate extraction filter residue II, time 80min, extraction time 3 times, merge
Extract solution, it is concentrated under reduced pressure after removing ethanol and obtains milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby；
(6) steam and fry：Filter residue III is soaked with the water of 0.6 times of amount, is then stir-fried again through frying pan to drying, obtains filter residue IV；
(7) extract oil：After screw oil expeller is dallied 5 minutes, the filter residue IV that step 6 obtains is fed while hot, when body temperature
Degree starts squeezing when reaching 80 DEG C and obtains oil cake；
(8) the milk thistle oil ether moiety for obtaining step 4, the milk thistle ethanolic moiety and step 7 that step 5 obtains obtain
Oil cake merge mix, obtain Silybum Marianum Gaertn Seed Oil.
After testing, oily 2.28kg, oil yield 22.8% are obtained；Contain silymarin 17.07% in the Silybum Marianum Gaertn Seed Oil.This product is yellow
Color is transparent, free from admixture, quality better, smell virtue.
Claims (2)
1. a kind of extracting method of Silybum Marianum Gaertn Seed Oil, it is characterised in that comprise the following steps：
(1) clear up：Clean ripe milk thistle seed；
(2) shell：Milk thistle seed after cleaning is placed in hulling machine and removes shell；
(3) crush：Milk thistle seed after shelling is crushed at normal temperatures, obtains coarse powder；
(4) degreasing：In 60~80 DEG C of refluxing extractions after the coarse powder of step (3) is mixed with the petroleum ether of 4~6 times of 30~60 DEG C of amounts
30~60min, filtrate I and filter residue I is obtained after filtering, after the petroleum ethers mixing that filter residue I is reused to 4~6 times of 30~60 DEG C of amounts
In 60~80 DEG C of 30~60min of refluxing extraction, filtrate II and filter residue II are obtained after filtering, filtrate I and filtrate II are merged, decompression
Concentration obtains milk thistle oil ether moiety after removing petroleum ether；
(5) extract：Filter residue II is extracted with 60~80wt% EtOH Sonicates, the time is 60~80min, extraction time 2~4 times, is closed
And extract solution, it is concentrated under reduced pressure after removing ethanol and obtains milk thistle ethanolic moiety, the filter residue III for extracting to obtain is standby, wherein, ethanol
Mass ratio with filter residue II is 8~10；
(6) steam and fry：Filter residue III water is soaked, then stir-fried again through frying pan to drying, obtains filter residue IV, water and filter residue III
Mass ratio be 0.2~1；
(7) extract oil：Filter residue IV after step (6) steaming is fried is squeezed to obtain oil cake with screw oil expeller, wherein, the specific step of oil expression
Suddenly it is：After screw oil expeller is dallied 3~5 minutes, the filter residue IV that step 6 obtains is fed while hot, when organism temperature reaches 70
Start squeezing at~80 DEG C and obtain oil cake；
(8) the milk thistle oil ether moiety for obtaining step (4), the milk thistle ethanolic moiety and step (7) that step (5) obtains
The oil cake arrived, which merges, to be mixed, and obtains Silybum Marianum Gaertn Seed Oil.
2. the extracting method of Silybum Marianum Gaertn Seed Oil according to claim 1, it is characterised in that in step (3), the particle diameter of coarse powder is
40~60 mesh.
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| CN105838496A (en) * | 2016-04-12 | 2016-08-10 | 北京林业大学 | Method for preparing edible oil with comprehensive nutrition by using oil cake obtained after oil expression |
| CN106589052B (en) * | 2017-01-16 | 2020-06-23 | 江苏中兴药业有限公司 | Method for degreasing and dehydrating silybum marianum seed kernel protein coarse powder |
| CN107595910A (en) * | 2017-09-08 | 2018-01-19 | 江苏中兴药业有限公司 | A kind of Silybum Marianum Gaertn Seed Oil composition and its application |
| CN109971540A (en) * | 2019-03-29 | 2019-07-05 | 江苏大学 | A kind of extraction of highly active milk thistle oil and preparation method of microcapsules |
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| CN102260589A (en) * | 2011-06-24 | 2011-11-30 | 江苏江大源生态生物科技有限公司 | Method for preparing silybum marianum oil |
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