CN102079745B - Production method of silymarin - Google Patents
Production method of silymarin Download PDFInfo
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- CN102079745B CN102079745B CN 200910238368 CN200910238368A CN102079745B CN 102079745 B CN102079745 B CN 102079745B CN 200910238368 CN200910238368 CN 200910238368 CN 200910238368 A CN200910238368 A CN 200910238368A CN 102079745 B CN102079745 B CN 102079745B
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- silymarin
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- silybum marianum
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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 51
- 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 51
- 235000017700 silymarin Nutrition 0.000 title claims abstract description 48
- 229960004245 silymarin Drugs 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 21
- 244000272459 Silybum marianum Species 0.000 claims abstract description 12
- 235000010841 Silybum marianum Nutrition 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 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 abstract description 9
- 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 abstract description 8
- 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 abstract description 8
- 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 abstract description 8
- 235000014899 silybin Nutrition 0.000 abstract description 8
- 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 abstract description 7
- 229930003944 flavone Natural products 0.000 abstract description 7
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 7
- 235000011949 flavones Nutrition 0.000 abstract description 7
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 238000000825 ultraviolet detection Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 3
- 238000011049 filling Methods 0.000 abstract 2
- VLGROHBNWZUINI-UHFFFAOYSA-N Silybin Natural products COc1cc(ccc1O)C2OC3C=C(C=CC3OC2CO)C4Oc5cc(O)cc(O)c5C(=O)C4O VLGROHBNWZUINI-UHFFFAOYSA-N 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 229940043175 silybin Drugs 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 229950000628 silibinin Drugs 0.000 description 8
- 238000007599 discharging Methods 0.000 description 5
- 231100001261 hazardous Toxicity 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 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 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 201000006474 Brain Ischemia Diseases 0.000 description 1
- 206010008120 Cerebral ischaemia Diseases 0.000 description 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 1
- 241000320380 Silybum Species 0.000 description 1
- 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 1
- 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 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000003811 acetone extraction Methods 0.000 description 1
- 230000003035 anti-peroxidant effect Effects 0.000 description 1
- 230000000702 anti-platelet effect Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 206010008118 cerebral infarction Diseases 0.000 description 1
- 230000002279 cholagogic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- -1 dehydro-silibinin Chemical compound 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 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
- 239000012530 fluid Substances 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 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 1
- 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 1
- 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 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Abstract
The invention provides a production method of silymarin, which comprises the following steps: shelling silybum marianum seeds; filling the silybum marianum shells into a softening tank, and softening the silybum marianum shells with vapor; filling the softened silybum marianum shells into a flat-turn extractor, and adding ethanol to carry out extraction, thereby obtaining an extracting solution; concentrating the extracting solution to a certain degree to obtain a concentrated solution; adding aqueous alkali into the concentrated solution, stirring and standing to precipitate; and filtering the precipitate, drying, pulverizing and screening. In the extraction process, no toxic or harmful reagent is adopted, and no solvent residue which is harmful to the product can be produced; the ultraviolet detection indicates that the total flavone content in the product can be higher than 70%, the contents of silybin and isosilybin can be higher than 30%, and the product yield is 3-4% of the silybum marianum seeds; and therefore, the invention has the advantages of high extraction efficiency, simple technique and low solvent consumption.
Description
Technical field
The embodiment of the invention relates to a kind of production method, relates in particular to a kind of production method of silymarin.
Background technology
Silymarin is the mixture of flavanolignan's compounds, originates to be the seed of composite family Silybum plant Silymarin (Silybum marianum).Its main component comprises Flavonoid substances such as silibinin, Isosilybin, dehydro-silibinin, Silychristin and Silydianin.Silymarin has the hepatic cholagogic effect, is mainly used in the treatment of hepatopathy.Secondly, it also has effects such as tangible anti peroxidation of lipid, radioprotective, removing free radical, anti-gastric-ulcer.In reducing blood-fat, prevent and treat atherosclerosis, there is good effect aspects such as prevention cerebral ischemia, anti-platelet aggregation.Nontoxic, no teratogenesis and mutagenesis.
In realizing process of the present invention, the contriver finds that there are the following problems at least in the prior art:
Patent publication No. CN1317486A discloses a kind of process for preparing sematron by aceton method, and it is raw material that this method adopts the Herba Silybi mariani meal pressed oil, forms through acetone extraction, concentrated, drying, petroleum ether degreasing, redrying and pulverizing six procedures.Owing to adopted acetone and sherwood oil in this technology, the residual of hazardous solvent reduces the security of product application in the product.
Patent publication No. CN1463970A discloses a kind of silymarin production method, and this method is at first pulverized silybum marianum seed, and behind supercritical fluid extraction proposition Silymarin oil, again with ethanol or ethyl acetate extraction, extracting solution is through supercritical CO
2Abstraction impurity removal matter.This technology has the ethyl acetate residue problem equally, simultaneously, though used advanced supercritical fluid technology, is subjected to the restriction of production cost, promotes difficult.
Patent publication No. CN101381363A discloses the method that a kind of potass extraction macroporous resin adsorption is separated silymarin, this method be silybum marianum seed after oil expression is pulverized through potass extraction, macroporous resin adsorption, sour water and ethanol elution, drying forms again.
Patent publication No. CN1560046A discloses a kind of with the silymarin extraction process of ethanol as single organic solvent, behind this method extraction using alcohol, repeatedly washs the back drying with ethanol, water, yellow soda ash respectively and forms.More than two technologies avoided hazardous solvent residual, but post-processing step is more, technology is loaded down with trivial details.
Summary of the invention
The embodiment of the invention provides a kind of production method of silymarin, in order to solve the defective that hazardous solvent is residual in the prior art, production cost is high, technology is loaded down with trivial details, production efficiency is low.
The embodiment of the invention provides a kind of production method of silymarin, comprising:
Step 1, silybum marianum seed is shelled;
Step 2, pack the Silymarin shell into softening jar, softening with steam;
Step 3, the Silymarin shell after will the softening flat-turn leacher of packing into adds extraction using alcohol, gets extracting solution;
Step 4, described extracting solution is concentrated into to a certain degree, gets concentrated solution;
Step 5, in described concentrated solution, add alkali aqueous solution, stir, staticly settle;
Step 6, with described sedimentation and filtration, drying, crushing screening.
The production method of above-mentioned silymarin, in the described step 2, the temperature of steam is 105～110 ℃, the softening time is 0.5～1.5h.
The production method of above-mentioned silymarin, the operation of described step 3 is specially:
With pack into the material lattice of described flat-turn leacher of described Silymarin shell after softening, charge amount is 60～70% of described material lattice, described concentration of ethanol is 70%～98%, temperature is 50～60 ℃, solvent ratio is 0.7～1.5: 1, and the temperature of regulating described flat-turn leacher is 50～60 ℃, and rotating speed is 1r/80～160min, spray extracts 5～12h continuously.
The production method of above-mentioned silymarin, in the described step 4, described concentrated solution is 20%～70% of described silybum marianum seed weight.
The production method of above-mentioned silymarin, in the described step 5, the volume of described alkali aqueous solution is 3～10 times of described concentrated solution volume; The kind of described alkali aqueous solution is potassium hydroxide, sodium hydroxide, saleratus and sodium bicarbonate; The concentration of described alkali aqueous solution is 0.3%～1.0%.
The production method of above-mentioned silymarin, in the described step 5, the time of described stirring is 10min～2h, the time of described precipitation is 10min～1h.
The production method of above-mentioned silymarin, the drying temperature in the described step 6 are 50～70 ℃, and be 7～12h time of drying.
The production method of the silymarin of the embodiment of the invention has reached following beneficial effect:
1, the present invention adopts peeler that Silymarin seed hulls, benevolence are separated, and keeps complete kind of benevolence, separates back Silymarin shell as extracting material, reduces the oil quantity in the subsequent disposal.
2, adopt flat-turn leacher as extraction equipment, reduce solvent usage quantity and loss, increase charging capacity, thereby increase work efficiency, reduce production costs.
3, adopt ethanol as unique organic solvent in producing, avoid hazardous solvent use and residual.
4, omit defatting step, post-treating method is simple, has simplified technology.
5, directly oven dry has been saved the energy and space with respect to vacuum-drying.
Embodiment
For the purpose, technical scheme and the advantage that make the embodiment of the invention clearer, to the technical scheme in the embodiment of the invention be clearly and completely described below, obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Embodiment one:
80 tons of Silymarin seeds shell through peeler, get 38 tons on Silymarin shell, through the softening 1h of steam, about 110 ℃ of temperature, discharging moisture 8%.Flat-turn leacher YJP300 extraction, charge amount are to expect 60%, 95% ethanol consumption of lattice 1: 1, temperature 55-60 ℃, and 50 ℃ of leacher temperature, rotating speed 1r/120min sprays continuously, extraction 5h.Leach liquor is concentrated into 20m
3, add 30 ℃ of 0.5% sodium bicarbonate aqueous solution 80m
3, stir 1h fast, sedimentation 1h, centrifugal after washing is to neutrality, 70 ℃ of dry 10h, crushing screening.2.8 tons of silymarins, silibinin and Isosilybin content totally 32.45%, general flavone content 74.5%.
Two: 100 tons of Silymarin seeds of embodiment shell through peeler, get 49.2 tons on Silymarin shell, and are softening through steam, time 0.5h, about 105 ℃ of temperature, discharging moisture 9.5%.Flat-turn leacher YJP300 extraction, charge amount are to expect 70%, 85% ethanol consumption of lattice 1: 1.5, temperature 55-60 ℃, and 50 ℃ of leacher temperature, rotating speed 1r/80min sprays continuously, extraction 9h.Leach liquor is concentrated into 50m
3, add 50 ℃ of 0.3% potassium hydroxide aqueous solution 300m
3, stirring 0.5h fast, the centrifugal after washing of sedimentation 0.5h is to neutrality, 70 ℃ of dry 10h, crushing screening.3.7 tons of silymarins, silibinin and Isosilybin content totally 34.2%, general flavone content 75.6%.
Three: 80 tons of Silymarin seeds of embodiment shell through peeler, get 39.8 tons on Silymarin shell, and are softening through steam, time 1h, about 105 ℃ of temperature, discharging moisture 7.2%.Flat-turn leacher YJP300 extraction, charge amount are to expect 65%, 75% ethanol consumption of lattice 1: 0.8, temperature 55-60 ℃, and 60 ℃ of leacher temperature, rotating speed 1r/120min sprays continuously, extraction 12h.Leach liquor is concentrated into 48.7m
3, add 20 ℃ of 0.8% potassium bicarbonate aqueous solution 480m
3, stirring 0.5h fast, the centrifugal after washing of sedimentation 10min is to neutrality, 70 ℃ of dry 10h, crushing screening.2.7 tons of silymarins, silibinin and Isosilybin content totally 35.4%, general flavone content 77.8%.
Four: 100 tons of Silymarin seeds of embodiment shell through peeler, get 48 tons on Silymarin shell, through the softening 0.5h of steam, about 110 ℃ of temperature, discharging moisture 9%.Flat-turn leacher YJP300 extraction, charge amount are to expect 60%, 70% ethanol consumption of lattice 1: 1.2, temperature 50-55 ℃, and 55 ℃ of leacher temperature, rotating speed 1r/160min sprays continuously, extraction 9h.Leach liquor is concentrated into 35m
3, add 40 ℃ of 1.0% aqueous sodium hydroxide solution 280m
3, stir 2h fast, sedimentation 45min, centrifugal after washing is to neutrality, 50 ℃ of dry 12h, crushing screening.3.8 tons of silymarins, silibinin and Isosilybin content totally 33.56%, general flavone content 75.5%.
Five: 80 tons of Silymarin seeds of embodiment shell through peeler, get 38 tons on Silymarin shell, through the softening 0.5h of steam, about 110 ℃ of temperature, discharging moisture 9%.Flat-turn leacher YJP300 extraction, charge amount are to expect 65%, 98% ethanol consumption of lattice 1: 0.7, temperature 50-55 ℃, and 55 ℃ of leacher temperature, rotating speed 1r/100min sprays continuously, extraction 7h.Leach liquor is concentrated into 16m
3, add 40 ℃ of 1.0% aqueous sodium hydroxide solution 48m
3, stir 10min fast, sedimentation 0.5h, centrifugal after washing is to neutrality, 70 ℃ of dry 7h, crushing screening.2.7 tons of silymarins, silibinin and Isosilybin content totally 34.56%, general flavone content 76.5%.
Above-described embodiment among the present invention, owing in leaching process, do not adopt poisonous or harmful reagent, can not produce the residual problem of hazardous solvent to product as can be known yet.In addition, the general flavone content of the product that the present invention obtains can reach more than 70% through ultraviolet detection, and silibinin and Isosilybin content can reach more than 30%, and product yield is the 3%-4% of Silymarin seed, the extraction efficiency height, and technology is simple, and solvent load is few.
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (4)
1. the production method of a silymarin is characterized in that, comprising:
Step 1, silybum marianum seed is shelled;
Step 2, pack the Silymarin shell into softening jar, softening with steam;
Step 3, the Silymarin shell after will the softening flat-turn leacher of packing into adds extraction using alcohol and gets extracting solution;
Step 4, described extracting solution is concentrated into to a certain degree, gets concentrated solution;
Step 5, in described concentrated solution, add alkali aqueous solution, stir, staticly settle;
Step 6, with described sedimentation and filtration, drying, crushing screening;
Wherein, the operation of described step 3 is specially: with pack into the material lattice of described flat-turn leacher of described Silymarin shell after softening, charge amount is 60～70% of described material lattice, described concentration of ethanol is 70%～98%, and temperature is 50～60 ℃, and solvent ratio is 0.7～1.5:1, the temperature of regulating described flat-turn leacher is 50～60 ℃, rotating speed is 1r/80～160min, and spray extracts 5～12h continuously;
In the described step 5, the volume of described alkali aqueous solution is 3～10 times of described concentrated solution volume; The kind of described alkali aqueous solution is potassium hydroxide, sodium hydroxide, saleratus and sodium bicarbonate; The concentration of described alkali aqueous solution is 0.3%～1.0%; The time of described stirring is 10min～2h, and the time of described precipitation is 10min～1h.
2. the production method of silymarin according to claim 1 is characterized in that, in the described step 2, the temperature of steam is 105～110 ℃, and the softening time is 0.5～1.5h.
3. the production method of silymarin according to claim 1 is characterized in that, in the described step 4, described concentrated solution is 20%～70% of described silybum marianum seed weight.
4. the production method of silymarin according to claim 1 is characterized in that, the drying temperature in the described step 6 is 50～70 ℃, and be 7～12h time of drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910238368 CN102079745B (en) | 2009-12-01 | 2009-12-01 | Production method of silymarin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910238368 CN102079745B (en) | 2009-12-01 | 2009-12-01 | Production method of silymarin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102079745A CN102079745A (en) | 2011-06-01 |
| CN102079745B true CN102079745B (en) | 2013-09-11 |
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| CN 200910238368 Active CN102079745B (en) | 2009-12-01 | 2009-12-01 | Production method of silymarin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225085B (en) * | 2011-06-20 | 2012-09-05 | 黑龙江大学 | Method for extracting holy thistle total flavonoids from holy thistle stalks |
| CN103408538B (en) * | 2013-08-27 | 2015-06-24 | 白心亮 | Method for extracting silymarin |
| CN103408539B (en) * | 2013-08-28 | 2016-04-06 | 天津泰阳制药有限公司 | The production method of high-purity silymarin |
| CN103446212B (en) * | 2013-09-11 | 2015-11-11 | 白心亮 | A kind of liver protection product |
| EP2959910A1 (en) * | 2014-06-26 | 2015-12-30 | Bionorica Se | Milk thistle extract of fruit shells of Silybum marianum, process of manufacture and use |
| CN105503843B (en) * | 2016-01-23 | 2018-07-10 | 内蒙古昶辉生物科技股份有限公司 | A kind of preparation method of silymarin |
| 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 |
| CN107663200A (en) * | 2016-07-29 | 2018-02-06 | 内蒙古昶辉生物科技股份有限公司 | A kind of silymarin gradient extracting method using ethyl acetate |
| CN107663201A (en) * | 2016-07-29 | 2018-02-06 | 内蒙古昶辉生物科技股份有限公司 | A kind of method that silymarin is extracted using ethanol |
| CN106188020A (en) * | 2016-07-29 | 2016-12-07 | 内蒙古昶辉生物科技股份有限公司 | A kind of silymarin gradient extracting method using ethanol |
| CN106008484B (en) * | 2016-07-29 | 2019-03-12 | 内蒙古昶辉生物科技股份有限公司 | A kind of extracting method of silymarin |
| CN106243095A (en) * | 2016-07-29 | 2016-12-21 | 内蒙古昶辉生物科技股份有限公司 | A kind of method using ethyl acetate to extract silymarin |
| CN107260787B (en) * | 2017-08-09 | 2020-07-21 | 江苏中兴药业有限公司 | Method for improving dissolution of effective components of silybum marianum shells |
| CN110028499B (en) * | 2019-05-10 | 2021-08-03 | 晨光生物科技集团股份有限公司 | Industrial method for producing high-quality silymarin |
| CN117402151B (en) * | 2023-12-15 | 2024-03-08 | 天津玉健生物工程有限公司 | Method for producing high content silybum marianum extract |
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