CN102993187A - Method for extracting silymarin by nitrogen protection - Google Patents
Method for extracting silymarin by nitrogen protection Download PDFInfo
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- CN102993187A CN102993187A CN2012105649743A CN201210564974A CN102993187A CN 102993187 A CN102993187 A CN 102993187A CN 2012105649743 A CN2012105649743 A CN 2012105649743A CN 201210564974 A CN201210564974 A CN 201210564974A CN 102993187 A CN102993187 A CN 102993187A
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Abstract
The invention discloses a method for extracting silymarin by nitrogen protection. The method comprises the following steps of: by the process of sorting, oil pressing, nitrogen-protective extraction, nitrogen-protective concentration and nitrogen-protective residue removal, silibinin materials and acetone solution are extracted according to the proportion of 1:2, the temperature is controlled to be 40-60 DEG C, saturated liquid in a tank is discharged repeatedly in 24 hours, and nitrogen is introduced; concentration: the silibinin and the acetone solution are added in a concentration tank, and are heated to be 80-90 DEG C, the repeating times between an extraction tank and a concentration tank are 6-7 times, the temperature is increased to be 100 DEG C, and after the acetone is recovered and extracted, the obtained substance is silibinin paste without containing the acetone; nitrogen-protective residue removal: hot water is added in a residue removing tank for residue removal, the heating temperature is higher than 60 DEG C, nitrogen washing is carried out and vacuum sealing is carried out; drying: the nitrogen is introduced in a drying box till the positive pressure is formed without oxygen, so that the environment in the drying box is surrounded by the nitrogen; and after drying, the fined silymarin is 80-100 meshes, and the yield can reach 5.2%.
Description
Technical field
The present invention relates to the elongation method of a kind of Silymarin, particularly a kind of method of extracting Silymarin with the protection of nitrogen.
Background technology
Silymarin is the plant milk extract of the brass wood lipid that forms of the class flavanonol that extracts from the kind skin of feverfew Silymarin [silybum marinaum (L) Gaenrt] seed and phenyl propanoid derivative condensation, be yellow powder or crystalloid powder, bitter, silymarin have radioprotective, anti-ageing, prevent and treat the effects such as arteriosclerosis, delay skin aging.This product can be widely used in the production of the products such as medicine, healthcare products, makeup, food.
At present, silymarin extraction pure method is extracted and alcohol is sent out extraction etc. is arranged.Wherein pure method is extracted, and characteristics are that extraction rate is fast, extraction comparison is complete, but the impurity of extract is many, and also needs to bring up again with ethyl acetate after drying again and get, and just can reach specification of quality; In addition, use ethyl acetate extraction, use the technique of ethyl acetate to need in process of production through recovery, Reusability, moisture in cake slag and the system also just constantly enters in the ethyl acetate, cause reversed reaction, generate ethanol and acetic acid, changed simultaneously solvent polarity and solubility property, and so that the quality of product, yield descend.In addition, the problem of oxidation that exists in existing Silymarin extraction process not yet is resolved.
Summary of the invention
The object of the present invention is to provide a kind of improving the quality of products and the nitrogen protection of yield, the method for silymarin is extracted in the nitrogen protection that improves problem of oxidation.
For realizing purpose of the present invention, the technical scheme of taking is: the method for silymarin is produced in nitrogen protection, comprises and selecting materials: the screening silybum marianum seed, remove impurity; Oil expression: by mill silybum marianum seed is pulverized, oil is extruded, become the Silymarin muffin; Nitrogen protection is extracted: the Silymarin muffin is added extractor mix with acetone soln, the ratio of Silymarin material cake and acetone soln is 1:3, temperature is controlled at 40-60C °, in 24 hours, repeatedly the saturated solution in the tank is got rid of, is added acetone soln, guard with ultraviolet ray, carry out vacuum-treat, fill 8 cubes in nitrogen with nitrogen gas generator; Concentrated: as through concentration tank the Silymarin material to be soaked with acetone soln again, Silymarin and acetone soln are heated to 80-90C °, then reclaim acetone soln, turn back to again extractor, the number of occurrence between extractor and the concentration tank is 6-7 time, through after being warmed to 100C °, both become the Silymarin cream that does not contain acetone; Nitrogen protection is taken off residual: Silymarin cream is delivered in the groove, enters and take off residual tank heating water and take off residually, Heating temperature pours 4.5 cubes of nitrogen, vacuum sealing with nitrogen gas generator greater than 60C ° thereupon; The nitrogen protection oven dry: the Silymarin material is inputted drying baker by pallet, with being filled with 3 cubes of nitrogen with nitrogen gas generator in the drying baker, is charged to malleation in the situation of original negative pressure, until do not have till the oxygen, makes the interior environment of drying baker among the encirclement of nitrogen.Nitrogen has played provide protection in the production process of whole silymarin.
The invention has the beneficial effects as follows: because the protection of nitrogen is used for the extraction of silymarin; can improve resistance of oxidation; the yield that the method for extracting silymarin with this kind nitrogen protection can make silymarin is from original 4.8%; bring up to 5.2%; the content 80% of brass brings up to 88%, its value gets a promotion thereupon.This kind Silymarin have the protection liver, improves liver function, promotes the effect of choleresis and anti-inflammatory.As powerful antioxidant, can prevent the damage that alcohol, chemical toxicant, heavy metal, medicine, sitotoxin, environmental pollution etc. cause liver, remove the free radical in the human body, delay senility.
The present invention will be further described below in conjunction with embodiment.
Embodiment
(1), the process of selecting materials
Choose silybum marianum seed, remove impurity, by mill silybum marianum seed is pulverized, the oil in the silybum marianum seed is extruded, become cake Silymarin material, both the Silymarin muffin;
(2), extract with nitrogen protection
With add in the extractor 1 ton Herba Silybi mariani powder also, two tons acetone soln, temperature is controlled at 40-60C °,
Time is at 24 hours, the saturated solution in the extractor is got rid of repeatedly within 24 hours, adds after the eliminating again
Enter acetone soln; Leaching process carries out vacuum with the ultraviolet ray monitoring, carries out inflated with nitrogen with nitrogen gas generator and protects
Protect.
(3), concentration process
With Silymarin material input concentration tank, soak with acetone soln, Silymarin and acetone soln are heated to
80-90 °, return extractor, the round number of times between extractor and the concentration tank is 6-7 time, when being warmed to
Reclaim acetone in the time of 100C ° and propose, the Silymarin material does not just contain acetone, becomes Silymarin cream,
(4), nitrogen protection is taken off residual
Silymarin cream is delivered to oxidation in the groove, degreasing-sealing, vacuum, enters and takes off residual tank, takes off residual taking
Heating water takes off residual, and Heating temperature is greater than 60C °;
(5), nitrogen protection oven dry
With pallet the Silymarin material is input into into drying baker, is filled with nitrogen with nitrogen gas generator in the drying baker, in the situation of original negative pressure, be charged to malleation, until do not have till the oxygen, the environment in the drying baker is among the encirclement of nitrogen.
(6), crushing process
Silymarin after the drying is coarse particles, and color is faint yellow or brown color, is machined to 80-120 orders through pulverizing mill again, and this silymarin is no more than 3000ppm.
Claims (1)
1. the method for silymarin is extracted in a nitrogen protection, it is characterized in that:
(1) select materials: the screening silybum marianum seed, remove impurity;
(2) oil expression: by mill silybum marianum seed is pulverized, oil is extruded, become the Silymarin muffin;
(3) nitrogen protection is extracted: the Silymarin muffin is added extractor mix the Silymarin thing with acetone soln
The ratio of material cake and acetone soln is 1:3, and temperature is controlled at 40-60C °, in 24 hours repeatedly with tank in
Saturated solution get rid of, add acetone soln, with the ultraviolet ray monitoring, carry out vacuum-treat, fill nitrogen and in tank, add ring Yao type pipeline and add the hole and nitrogen is evenly distributed with material mix, fill 8 cubes in nitrogen with nitrogen gas generator;
(4) concentrated: through concentration tank the Silymarin material is soaked with acetone soln again, Silymarin and acetone is molten
Liquid is heated to 80-90C °, then reclaims acetone soln, turns back to extractor again, and extractor is with concentrated
The number of occurrence between the tank is 6-7 time, through reclaiming after being warmed to 100C °, in that acetone is proposed, becomes
The Silymarin cream that does not contain acetone;
(5) nitrogen protection is taken off residual: Silymarin cream is delivered in the groove, enter take off residual tank heating water 10% take off residual,
Heating temperature pours 4.5 cubes of nitrogen with nitrogen gas generator greater than 60C ° thereupon in ring Yao type pipeline, make
Nitrogen, material are homogeneously mixing together, vacuum sealing; Vacuum tightness-0.4mpa takes off residual, and it is little to take off residual time needs two
The time;
(6) nitrogen protection oven dry: the Silymarin material is inputted drying baker by pallet, will use nitrogen in the drying baker
Producer is filled with 3 cubes of nitrogen, is charged to malleation in the situation of original negative pressure, until do not have till the oxygen,
Make the interior environment of drying baker among the encirclement of nitrogen; Added vacuum-0.8mpa dry 5 hours;
(7) pulverize: the Silymarin material after the oven dry is the silymarin coarse grain, and color is faint yellow or brown color,
Be machined to 80-120 orders, silymarin≤3000ppm through pulverizing mill again;
(8) packing: be machined to 80-120 purpose silymarins through pulverizing mill and be finished product through packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105649743A CN102993187A (en) | 2012-12-24 | 2012-12-24 | Method for extracting silymarin by nitrogen protection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105649743A CN102993187A (en) | 2012-12-24 | 2012-12-24 | Method for extracting silymarin by nitrogen protection |
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| Publication Number | Publication Date |
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| CN102993187A true CN102993187A (en) | 2013-03-27 |
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| CN2012105649743A Pending CN102993187A (en) | 2012-12-24 | 2012-12-24 | Method for extracting silymarin by nitrogen protection |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994026943A1 (en) * | 1993-05-07 | 1994-11-24 | Ibc Advanced Technologies, Inc. | Process for removing, separating, and concentrating metals |
| CN1317486A (en) * | 2001-01-19 | 2001-10-17 | 盘锦第二制药厂 | Process for preparing sematron by aceton method |
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
| CN102023191A (en) * | 2009-09-22 | 2011-04-20 | 复旦大学 | Method for extracting ascorbic acid from vegetables and fruits |
| CN102586357A (en) * | 2012-03-12 | 2012-07-18 | 佳木斯三江水飞蓟素制品有限公司 | Preparation method of silymarin |
-
2012
- 2012-12-24 CN CN2012105649743A patent/CN102993187A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994026943A1 (en) * | 1993-05-07 | 1994-11-24 | Ibc Advanced Technologies, Inc. | Process for removing, separating, and concentrating metals |
| CN1317486A (en) * | 2001-01-19 | 2001-10-17 | 盘锦第二制药厂 | Process for preparing sematron by aceton method |
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
| CN102023191A (en) * | 2009-09-22 | 2011-04-20 | 复旦大学 | Method for extracting ascorbic acid from vegetables and fruits |
| CN102586357A (en) * | 2012-03-12 | 2012-07-18 | 佳木斯三江水飞蓟素制品有限公司 | Preparation method of silymarin |
Non-Patent Citations (1)
| Title |
|---|
| YINGJIA YU，等: "Nitrogen-protected microwave-assisted extraction of ascorbic acid from fruit and vegetables", 《J. SEP. SCI.》 * |
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Application publication date: 20130327 |