CN102558162A - Processing and extraction method for silybin with low soluble residues and high content - Google Patents
Processing and extraction method for silybin with low soluble residues and high content Download PDFInfo
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- CN102558162A CN102558162A CN2010106000100A CN201010600010A CN102558162A CN 102558162 A CN102558162 A CN 102558162A CN 2010106000100 A CN2010106000100 A CN 2010106000100A CN 201010600010 A CN201010600010 A CN 201010600010A CN 102558162 A CN102558162 A CN 102558162A
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- silybin
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- slb
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- 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 title claims abstract description 14
- 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 title claims abstract description 14
- 238000000605 extraction Methods 0.000 title claims abstract description 12
- 235000014899 silybin Nutrition 0.000 title abstract description 7
- 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 title abstract 6
- VLGROHBNWZUINI-UHFFFAOYSA-N Silybin Natural products COc1cc(ccc1O)C2OC3C=C(C=CC3OC2CO)C4Oc5cc(O)cc(O)c5C(=O)C4O VLGROHBNWZUINI-UHFFFAOYSA-N 0.000 title abstract 6
- 229940043175 silybin Drugs 0.000 title abstract 6
- 238000003672 processing method Methods 0.000 title abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000284 extract Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000012054 meals Nutrition 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 235000011837 pasties Nutrition 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 229960004245 silymarin Drugs 0.000 claims description 7
- 235000017700 silymarin Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 abstract description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract description 5
- 235000010841 Silybum marianum Nutrition 0.000 abstract description 4
- 241000320380 Silybum Species 0.000 abstract 1
- 244000272459 Silybum marianum Species 0.000 description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 235000021050 feed intake Nutrition 0.000 description 3
- 229930003944 flavone Natural products 0.000 description 3
- 150000002212 flavone derivatives Chemical class 0.000 description 3
- 235000011949 flavones Nutrition 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 241000132536 Cirsium Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229950000628 silibinin Drugs 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a processing and extraction method for silybin with low soluble residues and high content. According to the method, milk thistle meal is adopted as a raw material, acetone is added in proportion, the extraction is conducted in feed back, an acetone solvent is recycled, filtered and condensed, then the acetone solvent is recycled again to obtain pasty extract, the extract is put in a jacket pot, water is added to stir the extract and then run off, the step is conducted repeatedly, the extract is put in a vacuum drying tank to be dried so as to obtain silybin dry powder block, and then the block is smashed to be vacuumized for secondary time and dried to obtain silybin dry powder. Due to the adoption of the method, the yield coefficient of the silybin is enhanced, the product quality and extraction purity of the silybin are improved, the residual solution of an organic solvent is low so as to prevent a person or an animal from any harms, n-hexane derosination is not adopted in the extraction process, the solvent and energy are saved, the extraction process is simple, the cost is low, and the gains are high.
Description
Technical field: the present invention relates to a kind of low processing process for extracting that dissolves residual high-content SLB.
Background technology: it is that acetone, ethanol, ETHYLE ACETATE extract with traditional thermal reflux mostly that existing SLB extracts solvent, and its extraction temperature is at the 50-60 degree, owing to temperature is too high; Impurity in the Herba Silybi mariani meal is prone to get in the solution; Influence the purity of Silymarin in the medicinal extract after concentrating, influences its content, with the general flavone content of performance liquid chromatography detection SLB at HPLC＞65%; Though with normal hexane degreasing decon, the residual of normal hexane stayed in the medicinal extract again.The solvent of SLB extraction at present extracts with acetone; Its advantage is that yield is high; But it is residual too high that shortcoming is an acetone solvent, can not be well in later stage extraction process process with the residue removal of acetone solvent, organic solvent residual＜5000PPM; Big as medicine, healthcare products, foodstuff additive or makeup etc. to person harm, and the requirement that does not reach the outlet index.
Summary of the invention: the objective of the invention is to overcome above-mentioned shortcoming; A kind of low processing process for extracting that dissolves residual high-content SLB is provided, solved existing process for extracting can not be well in later stage extraction process process with the problems such as residue removal of acetone solvent.The objective of the invention is to realize like this; It is to be raw material with the Herba Silybi mariani meal, process for extracting: at first feed intake, with the Herba Silybi mariani meal behind the meal in 1: 3-1: 4 ratios add acetone; Carry out feed back with extractor and concentration tank; Extracted 8-10 hour, temperature of charge is controlled at 25-30 ℃, reclaims acetone solvent with condensing surface simultaneously; With solvent filter, concentrate 2-4 hour, temperature 60-65 degree, vapor pressure 1.5 MPas reclaim acetone solvent with condensing surface simultaneously, obtain pasty state medicinal extract; Medicinal extract is put in the chuck pot, adds 1: 5 purification pure water, water temperature is heated to the 80-90 degree; Stirred 1-2 hour, and bled off water, repeat 5-6 time so repeatedly; Because acetone is water-soluble, SLB solution is water insoluble, through repeatedly after 5-6 time; The solvent of acetone can remove more than 90%, can remaining Silymarin Residual oil be removed simultaneously; Silymarin medicinal extract is put into carries out vacuum-drying in the vacuum drying tank, drying temperature 90-120 degree, negative pressure 0.8 MPa was carried out 4-6 hour continuously; Purpose is to use the vacuum pump sucking-off to the gas of acetone and moisture content, obtains the SLB dry powder piece of water cut about 5%, and it is ground into the 80-90 order; Put into vacuum tank again and carry out secondary vacuum, dry 2-4 hour, temperature 80-110 degree; More than negative pressure 0.8 MPa, acetone solvent can remove 95%, promptly obtains the dry powder of SLB.This processing process for extracting integrated use molecular distillation technique, through detecting the SLB general flavone content at HPLC＞78% with performance liquid chromatography, new result's demonstration is looked in the science and technology retrieval through the Heilongjiang Province, and not seeing has relevant achievement Report both at home and abroad; Organic solvent residual＜50PPM, and the export requirement organic solvent residual is superior to export standard below 100PPM; This method of using has improved the yield of SLB greatly, has improved SLB quality product and dna purity, and organic solvent is residual molten low; The person, animal are had no harm, can be widely used in leaching process, need not using the normal hexane degreasing in medicine, healthcare products, foodstuff additive, the animal feedstuff additive; Save solvent, practiced thrift the energy, reduced enterprise's discharging and pollution; Its extraction process is simple, and cost is low, and income is high.
It is following to detect the plain detection index of high-content low solubility residual water setose thistle for twice through Dalian Inst of Chemicophysics, Chinese Academy of Sciences:
General flavone content detects: (performance liquid detection) HPLC＞81.6-83.5%
Silibinin content＞39.2-40.9%
The different guest content＞7.8-8.0% of Silymarin
Through detecting all other indexs:
Organic solvent residual＜50PPM
Pesticide residue: do not have
Heavy metal＜5PPM
Intestinal bacteria detect: do not have
Mould and yeast: do not have
Salmonellas: do not have
Other bacteria total amount detected result＜20CFU/g
Embodiment:
Embodiment 1: most preferred embodiment
The silybum marianum seed of a, selection full seed, cleaning, drying rolls oily machine with machinery and adopts three grades of milling process to squeeze, and 100 jin of silybum marianum seed compressibles go out 15 jin of oil, and the dregs of rice after the squeezing carry out meal, and are subsequent use;
B, feed intake, every jar of Herba Silybi mariani meal that drops into behind 1.5 tons of meal was by 1: 4 ratio adding acetone; Promptly 1 ton of Herba Silybi mariani meal adds 4 tons of acetone; Carry out feed back with extractor and concentration tank and extracted 10 hours, temperature of charge is controlled at 25 degree, reclaims acetone solvent with condensing surface simultaneously;
C, with solvent filter, concentrate 2 hours, temperature 60 degree, vapor pressure 1.5 MPas reclaim acetone solvent with condensing surface simultaneously, obtain pasty state medicinal extract;
D, medicinal extract is put in the chuck pot, adds 1: 5 purification pure water, promptly 1 kilogram of medicinal extract adds 5 kg of water, and water temperature is heated to 80 degree, stirs 1 hour, bleeds off water, repeats so repeatedly 6 times;
E, Silymarin medicinal extract is put in the vacuum drying tank, carries out vacuum-drying, drying temperature 120 degree, negative pressure 0.8 MPa was carried out 4-6 hour continuously, obtained the dry powder piece of the SLB of water cut about 5%, and it is ground into the 80-90 order;
F, the SLB after will pulverizing is put into vacuum tank and is carried out secondary vacuum again, and dry 2-4 hour, temperature 80 degree, negative pressure 0.8 MPa promptly gets SLB dry powder.
Embodiment 2:
The silybum marianum seed of a, selection full seed, cleaning, drying rolls oily machine with machinery and adopts three grades of milling process to squeeze, and the dregs of rice after the squeezing carry out meal, and are subsequent use;
B, feed intake, every jar of Herba Silybi mariani meal that drops into behind 1.5 tons of meal was by 1: 3 ratio adding acetone; Promptly 1 ton of Herba Silybi mariani meal adds 3 tons of acetone; Carry out feed back with extractor and concentration tank and extracted 8 hours, temperature of charge is controlled at 30 degree, reclaims acetone solvent with condensing surface simultaneously;
C, with solvent filter, concentrate 4 hours, temperature 65 degree, vapor pressure 1.5 MPas reclaim acetone solvent with condensing surface simultaneously, obtain pasty state medicinal extract;
D, medicinal extract is put in the chuck pot, adds 1: 5 purification pure water, promptly 1 kilogram of medicinal extract adds 5 kg of water, and water temperature is heated to 90 degree, stirs 2 hours, bleeds off water, repeats so repeatedly 5 times;
E, Silymarin medicinal extract is put in the vacuum drying tank, carries out vacuum-drying, drying temperature 90 degree, negative pressure 0.8 MPa was carried out 4-6 hour continuously, obtained the SLB dry powder piece of water cut about 5%, and it is ground into the 80-90 order;
F, the SLB after will pulverizing is put into vacuum tank and is carried out secondary vacuum again, and dry 2-4 hour, temperature 110 degree, negative pressure 0.8 MPa promptly gets SLB dry powder.
Claims (1)
1. one kind low processing process for extracting that dissolves residual high-content SLB is to be raw material with the Herba Silybi mariani meal, it is characterized in that:
A, with the Herba Silybi mariani meal behind the meal, in 1: 3-1: 4 ratio adds acetone, carries out feed back extraction 8-10 hour with extractor and concentration tank, and temperature of charge is controlled at the 25-30 degree, reclaims acetone solvent with condensing surface simultaneously;
B, with solvent filter, concentrate 2-4 hour, temperature 60-65 degree, vapor pressure 1.5 MPas reclaim acetone solvent with condensing surface simultaneously, obtain pasty state medicinal extract;
C, medicinal extract is put in the chuck pot, adds 1: 5 purification pure water, water temperature is heated to the 80-90 degree, stirs 1-2 hour, bleeds off water, repeats 5-6 time so repeatedly;
D, Silymarin medicinal extract is put in the vacuum drying tank, carries out vacuum-drying, drying temperature 90-120 degree, negative pressure 0.8 MPa was carried out 4-6 hour continuously, obtained the dry powder piece of the SLB of water cut about 5%, and it is ground into the 80-90 order;
E, the SLB after will pulverizing is put into vacuum tank and is carried out secondary vacuum again, and dry 2-4 hour, temperature 80-110 degree, negative pressure 0.8 MPa promptly gets SLB dry powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106000100A CN102558162A (en) | 2010-12-20 | 2010-12-20 | Processing and extraction method for silybin with low soluble residues and high content |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106000100A CN102558162A (en) | 2010-12-20 | 2010-12-20 | Processing and extraction method for silybin with low soluble residues and high content |
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| CN102558162A true CN102558162A (en) | 2012-07-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010106000100A Pending CN102558162A (en) | 2010-12-20 | 2010-12-20 | Processing and extraction method for silybin with low soluble residues and high content |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964342A (en) * | 2012-12-18 | 2013-03-13 | 佳木斯三江水飞蓟素制品有限公司 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
| WO2015100524A1 (en) * | 2013-12-30 | 2015-07-09 | 晨光生物科技集团股份有限公司 | Method for producing silymarin |
| CN109651347A (en) * | 2019-01-29 | 2019-04-19 | 盘锦天源药业有限公司 | A kind of extracting solution removal magnetisable material device and method |
| CN109810102A (en) * | 2019-01-29 | 2019-05-28 | 盘锦天源药业有限公司 | A kind of silymarin removes molten residual method |
| CN110028499A (en) * | 2019-05-10 | 2019-07-19 | 晨光生物科技集团股份有限公司 | A kind of industrial method producing high-quality silymarin |
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2010
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Non-Patent Citations (1)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964342A (en) * | 2012-12-18 | 2013-03-13 | 佳木斯三江水飞蓟素制品有限公司 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
| CN102964342B (en) * | 2012-12-18 | 2015-05-13 | 佳木斯三江水飞蓟素制品有限公司 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
| WO2015100524A1 (en) * | 2013-12-30 | 2015-07-09 | 晨光生物科技集团股份有限公司 | Method for producing silymarin |
| CN105849103A (en) * | 2013-12-30 | 2016-08-10 | 晨光生物科技集团股份有限公司 | Method for producing silymarin |
| US9765062B2 (en) | 2013-12-30 | 2017-09-19 | Chenguang Biotech Group Co., Ltd. | Method for producing silymarin |
| CN105849103B (en) * | 2013-12-30 | 2019-03-12 | 晨光生物科技集团股份有限公司 | A kind of production method of silymarin |
| CN109651347A (en) * | 2019-01-29 | 2019-04-19 | 盘锦天源药业有限公司 | A kind of extracting solution removal magnetisable material device and method |
| CN109810102A (en) * | 2019-01-29 | 2019-05-28 | 盘锦天源药业有限公司 | A kind of silymarin removes molten residual method |
| CN109651347B (en) * | 2019-01-29 | 2022-05-20 | 盘锦天源药业有限公司 | Device and method for removing magnetic substances from extracting solution |
| CN110028499A (en) * | 2019-05-10 | 2019-07-19 | 晨光生物科技集团股份有限公司 | A kind of industrial method producing high-quality silymarin |
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Application publication date: 20120711 |