CN102731486B - New method for purifying silymarin - Google Patents
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Abstract
The invention belongs to the field of natural organic chemistry, and relates to a method for preparing high purity silymarin by the following steps: adopting biological wall breaking and microwave pretreatment to obtain oil, carrying out microwave countercurrent extraction and macroporous resin purification to obtain the high purity silymarin. The method has the following advantages that: 1, a step-by-step method is adopted to carry out degreasing, seeds are pretreated, microwave countercurrent extraction is performed, and isoelectric point precipitation is performed to remove proteins, such that complete dissolution of effective components of the silymarin is prompted; 2, with the microwave extraction, the extraction time is reduced to 60-80 minutes so as to improve extraction speed and increase effective component content, and reduce herb consumption and energy consumption; 3, the macroporous resin adsorption technology is adopted so as to reduce the amount of the solvent, and the macroporous resin can be conveniently and rapidly regenerated, such that the cost is substantially reduced; and 4, two products of silybum marianum oil and silymarin can be obtained. With the method, the biological wall breaking treatment is performed on the silybum marianum seeds at the early stage so as to shorten the microwave pretreatment time, such that the seed oil can be extracted in just a few minutes; with the two-step microwave extraction, the extraction time is shortened; and the disadvantages of long conventional extraction time, low extract purity and single extract are overcome.
Description
Technical field:
The invention belongs to field of natural organic chemistry, relate to that one utilizes biological wall breaking, Microwave Pretreatment obtains oily, then extract and macroporous resin purification technology through microwave counter current, obtain the method for high purity silymarin.
Background technology:
Silybum marianum seeds is containing crude fat 25.05%, and its lipid acid is mainly unsaturated oleic acid (47.46%) and linolic acid (31.79%).Spent meal protein content is 19.58%, higher than general cereal.Wherein maximum with albumin content, account for 62.60% of total protein.Silybum marianum protein matter based in, lower molecular weight, owing to being rich in acidic amino acid, white matter iso-electric point is mainly distributed within the scope of neutral meta-acid.
Silymarin is the plant milk extract extracted from the seed coat of the medicinal plants of Compositae Silymarin seed, in yellow powder or knot product sprills, and bitter.Be soluble in buck, acetone, ethyl acetate, ethanol and methyl alcohol, be insoluble in chloroform, water insoluble, main component has the Flavonoid substances such as silibinin, Isosilybin, Silydianin and Silychristin.This material has following effect: protection liver cell is encroached on from toxicant, and especially alcohol and environmental pollutant (agricultural chemicals, heavy metal etc.) invasion infringement are with dirty; Have powerful anti-oxidant function, liver cell can be protected to destroy from free radical, and effect outclass vitamin-E; Promote the synthesis of protein, what quickening manufacture was new uses dirty cell, or makes liver cell self-healing in damaged condition.Therefore be called as " warranty medicine right greatly ".In addition silymarin have radioprotective, anti-ageing, prevent and treat the effect such as arteriosclerosis, delay skin aging.This product is widely used in the production of the products such as medicine, healthcare products, makeup, food.
Silymarin industrial production has multiple method, is cold compression to degrease substantially, then uses solvent extraction.In cold pressing process, some the pigment wax strippings in cot are in oil, and silymarin has loss.The grouts of oil removing are first with petroleum ether degreasing, dewaxing, and then with ethyl acetate or alcohol for solvent carries out diacolation or circumfluence distillation, then recycling design obtains silymarin crude product and sells, and seldom has producer to proceed purifying to it; And ethyl acetate is recycling in process, hydrolysis is producing acetic acid, has influence on yield and the quality of product.
Summary of the invention:
The present invention adopts biological wall breaking method, anticipating substitute is rolled in the Mierocrystalline cellulose of seed skin shell, hemicellulose, pectin segment and albuminous membranae, make wrapped oil cells free out, again in conjunction with microwave treatment method, fat in fast eliminating seed, and degreasing more thoroughly obtains the novel method of the Silybum Marianum Gaertn Seed Oil determining content.
Silybum marianum seed ethanol as solvent after de-oiling, through microwave reflux extracting device, removes albumen in iso-electric point, finally by macroporous resin adsorption, and concentrated, the highly purified silymarin of dry acquisition.The inventive method can obtain Silybum Marianum Gaertn Seed Oil and silymarin two products simultaneously.Be different from traditional cold press oil removing, ethyl acetate is extracted, and has to the method for single silymarin.Overcome the shortcomings such as silymarin routine techniques extraction yield is relatively low, the operating time is long, extracting substance is single.
For achieving the above object, the technical solution used in the present invention is:
One utilizes biological wall breaking, Microwave Pretreatment obtains oily, then extracts and macroporous resin purification technology through microwave counter current, obtains the method for high purity silymarin.Its step is as follows:
(1) biological wall breaking: dry silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, insulation enzymolysis 60min, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make wrapped oil cells free out, improve grease extraction efficiency.
(2) Microwave Pretreatment: silybum marianum seed was pulverized 30-60 mesh sieve, add 1-6 times of sherwood oil (boiling range 60-90 DEG C) solution, carry out Microwave Pretreatment, microwave power is at 300 ~ 600W, frequency 4000 ~ 8000MHz, extraction time 300 ~ 400s, extraction temperature is 50 ~ 60 DEG C and reclaims sherwood oil, obtains Silybum Marianum Gaertn Seed Oil.
(3) microwave counter current extracts: the ethanol of the silybum marianum seed powder 80-85% after de-oiling extracts in conjunction with microwave counter current, forward feeding. and the flowing of backspace water inlet material and water is reverse continuous dynamic flow.Extracting temperature 50 ~ 60 DEG C, time 60-80min, 400 ~ 600W, frequency 5000 ~ 8000MHz, slag is forced to be pushed to slag notch through spiral conveyer of slagging tap and discharges, and spiral of slagging tap extrudes slag simultaneously, debris in slag is extruded, improve extracting solution yield, centrifuging, reclaim ethanol.
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, regulates PH to 6-6.5 with hydrochloric acid, separates out protein precipitation, isolated protein, then regulates pH value between 9-10 with NaOH:
(5) macroporous resin adsorption: by Silymarin alkaline solution through pretreated macroporous resin adsorption, make adsorptive single, resin model is S-8, AB-8, DA-201, NKA-9 resin, and the aspect ratio of resin column is 8: 1-15: 1:
(6) sour water wash-out: at normal temperatures and pressures, with 0.5-1BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with PH, elution volume is 1 6BV;
(7) ethanol elution: at normal temperatures and pressures, with 2-4BV/h flow velocity, with the ethanol aqueous wash deresination of 70%-95%, wash-out body is protected as 3-4BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure, reclaim ethanol, vacuum-drying, micronization, obtains silymarin
Embodiment: one utilizes biological wall breaking, twice microwave extraction, and macroporous resin purification technology, obtains the method for high purity silymarin.
Embodiment 1: one utilizes biological wall breaking, Microwave Pretreatment obtains oily, then through microwave counter current and macroporous resin purification technology, obtain the method for high purity silymarin, its step is as follows:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, the solution 60min of insulation, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, the oil cells that bale broken is wrapped up in is free out, improves grease extraction efficiency;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 30 mesh sieves, add 4-6 times of sherwood oil (boiling range 60-90 DEG C) solution, carry out Microwave Pretreatment, microwave power at 300 W, frequency 1000MHz, extraction time 300s, extraction temperature is 60 DEG C, reclaim sherwood oil, obtain Silybum Marianum Gaertn Seed Oil 195.3g, de-oiling Herba Silybi mariani powder 793g;
(3) microwave counter current extracts: the de-oiling Herba Silybi mariani powder ethanol of 80% extracts in conjunction with microwave counter current, and forward feeding, oppositely intakes, and the flowing of material and water is reverse continuous dynamic flow.Extracting temperature 50 DEG C, time 60min, 400W, frequency 5000MHz, extrude debris in slag, the partial protein of precipitation separation, reclaims ethanol;
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, regulates PH to 6 with hydrochloric acid, separates out protein precipitation, isolated protein, then regulates pH value to be 9 with NaOH:
(5) macroporous resin adsorption: by nonprotein Silymarin solution through pretreated macroporous resin adsorption, make adsorptive list, resin model is S-8 resin, and the aspect ratio of resin column is 8: 1;
(6) sour water wash-out: at normal temperatures and pressures, with 0.5BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with PH, elution volume is 1BV;
(7) ethanol elution: at normal temperatures and pressures, with 2BV/h flow velocity, with the ethanol aqueous wash deresination of 70%, elution volume is 3BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure, reclaim ethanol, vacuum-drying, micronization, obtains silymarin 51g, purity 80.8%.
Case study on implementation 2: one utilizes biological wall breaking, Microwave Pretreatment obtains oily, then through microwave counter current and macroporous resin purification technology, obtain the method for high purity silymarin, its step is as follows:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, insulation enzymolysis 60min, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make wrapped oil cells free out, improve grease extraction efficiency;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 40 mesh sieves, add 1-6 times of sherwood oil (boiling range 60-90 DEG C) solution, carry out Microwave Pretreatment, microwave power at 400W, frequency 6000MHz, extraction time 400s, extraction temperature is 60 DEG C, reclaim sherwood oil, obtain silybum marianum seed oil 195g, de-oiling Herba Silybi mariani powder 797.3g;
(3) microwave counter current extracts: the de-oiling Herba Silybi mariani powder ethanol of 85% extracts in conjunction with microwave counter current, and forward feeding, oppositely intakes, and the flowing of material and water is reverse continuous dynamic flow.Extracting temperature 60 DEG C, time 70min, 500W, frequency 6000MHz, extrude debris in slag, the partial protein of precipitation separation, reclaims ethanol:
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, and isolated protein regulates pH value to be 10 with NaOH again;
(5) macroporous resin adsorption: by nonprotein Silymarin solution through pretreated macroporous resin adsorption, make adsorptive single, resin model is AB-8 resin, and the aspect ratio of resin column is 10: 1;
(6) sour water wash-out: at normal temperatures and pressures, with 1BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with PH, elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with 3BV/h flow velocity, with the ethanol aqueous wash deresination of 80%, elution volume is 4BV:
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure, reclaim ethanol, vacuum-drying micronization, obtains silymarin 51.7g, purity 81.2%.
Case study on implementation 3: one utilizes biological wall breaking, Microwave Pretreatment obtains oily, then through microwave counter current and macroporous resin purification technology, obtain the method for high purity silymarin.Its step is as follows:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, insulation enzymolysis 60min, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make wrapped oil cells free out, improve grease extraction efficiency;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 50 mesh sieves, add 4-6 times of sherwood oil (boiling range 60-90 DEG C) solution, carry out Microwave Pretreatment, microwave power at 500W, frequency 7000MHz, extraction time 400s, extraction temperature is 60 DEG C, reclaim sherwood oil, obtain silybum marianum seed oil 197g, de-oiling Herba Silybi mariani powder 795g;
(3) microwave counter current extracts: the de-oiling Herba Silybi mariani powder ethanol of 80% extracts in conjunction with microwave counter current, and forward feeding, oppositely intakes, and the flowing of material and water is reverse continuous dynamic flow.Extracting temperature 50 DEG C, time 80min, 600W, frequency 7000MHz, extrude debris in slag, the partial protein of precipitation separation, reclaims ethanol;
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, protein isolate, then regulates pH value to be 9 with NaOH;
(5) macroporous resin adsorption: by nonprotein Silymarin solution through pretreated macroporous resin adsorption, make adsorptive list, resin model is DA-201 resin, and the aspect ratio of resin column is 12: 1;
(6) sour water wash-out: at normal temperatures and pressures with 1BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with PH, elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with 3BV/h flow velocity, with the ethanol aqueous wash deresination of 80%, elution volume is 4BV;
(8) drying under reduced pressure: collect ethanol eluate, alkali pressure is concentrated, and reclaim ethanol, vacuum-drying micronization, obtains silymarin 50.5g, purity 82%.
Case study on implementation 4: one utilizes biological wall breaking, Microwave Pretreatment obtains oily, then through microwave counter current and macroporous resin purification technology, obtain the method for high-purity skin silymarin.Its step is as follows:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, insulation enzymolysis 60min, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make wrapped oil cells free out, improve grease extraction efficiency;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 60 mesh sieves, add 1-6 times of sherwood oil (boiling range 60-90 DEG C) solution, carry out Microwave Pretreatment, microwave power at 600W, frequency 8000MHz, extraction time 360s, extraction temperature is 50 DEG C, reclaim sherwood oil, obtain silybum marianum seed oil 189g, de-oiling Herba Silybi mariani powder 790.6g;
(3) microwave counter current extracts: the de-oiling Herba Silybi mariani powder ethanol of 80% extracts in conjunction with microwave counter current, and forward feeding, oppositely intakes, and the flowing of material and water is reverse continuous dynamic flow.Extracting temperature 60 DEG C, time 80min, 600W, frequency 8000MHz, extrude debris in slag, the partial protein of precipitation separation, reclaims ethanol;
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, isolated protein, then regulates pH value to be 9 with NaOH;
(5) macroporous resin adsorption: by nonprotein Silymarin solution through pretreated macroporous resin adsorption, make adsorptive single, resin model is NKA-9 resin, and the aspect ratio of resin column is 15: 1;
(6) sour water wash-out: at normal temperatures and pressures, with 1BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with PH, elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with 4BV/h flow velocity, with the ethanol aqueous wash deresination of 95%, elution volume is 4BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrated, reclaim ethanol, drying under reduced pressure, micronization, obtains silymarin 49.7g, purity 83.1%.
Claims (1)
1. one kind utilizes biological wall breaking, Microwave Pretreatment obtains oily, then extracts and macroporous resin purification technology through microwave counter current, and obtain the method for high purity silymarin, its step is as follows:
(1) biological wall breaking: dry silybum marianum seed soaks, add appropriate cellulase, hemicellulase solution, insulation enzymolysis 60min, remove the Mierocrystalline cellulose, hemicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make wrapped oil cells free out, improve grease extraction efficiency;
(2) pre-treatment de-oiling: silybum marianum seed was pulverized 30-60 mesh sieve, add 4-6 times of sherwood oil boiling range 60-90 DEG C solution, carry out Microwave Pretreatment, microwave power is at 300 ~ 600W, frequency 4000 ~ 8000MHz, extraction time 300 ~ 400s, extraction temperature is 50 ~ 60 DEG C, reclaim sherwood oil, obtain Silybum Marianum Gaertn Seed Oil;
(3) microwave counter current extracts: the ethanol of the silybum marianum seed powder 80-85% after de-oiling extracts in conjunction with microwave counter current, and forward feeding, oppositely intakes; The flowing of material and water is reverse continuous dynamic flow, Extracting temperature 50 ~ 60 DEG C, time 60-80min, 400 ~ 600W, frequency 5000 ~ 8000MHz, slag is forced to be pushed to slag notch through spiral conveyer of slagging tap and discharges, spiral of slagging tap extrudes slag simultaneously, debris in slag is extruded, and improves extracting solution yield, centrifuging, reclaims ethanol;
(4) isoelectric precipitation: owing to being rich in acidic amino acid, isoelectric points of proteins is mainly distributed within the scope of neutral meta-acid, with salt acid for adjusting pH to 6-6.5, separates out protein precipitation, isolated protein, then uses NaOH adjust ph between 9-10;
(5) macroporous resin adsorption: by Silymarin alkaline solution through pretreated macroporous resin adsorption, make adsorptive single, resin model is S-8, AB-8, DA-201, NKA-9 resin, and the aspect ratio of resin column is 8: 1-15: 1;
(6) sour water wash-out: at normal temperatures and pressures, with 0.5-1BV/h flow velocity, be the phosphoric acid solution wash-out resin of 2 with pH, elution volume is 4-6BV/h;
(7) ethanol elution: at normal temperatures and pressures, with 2-4BV/h flow velocity, with the ethanol aqueous wash deresination of 70%-95%, elution volume is 3-4BV/h;
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure, reclaim ethanol, vacuum-drying, micronization, obtains silymarin.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242423A (en) * | 2013-05-13 | 2013-08-14 | 江苏大学 | Method for extracting silybum marianum protein |
| CN103509647B (en) * | 2013-09-27 | 2014-11-05 | 宁波市北仑玉健医药科技有限公司 | Method for preparing silybum marianum oil rich in silymarin |
| CN105693708A (en) * | 2014-11-25 | 2016-06-22 | 河南智晶生物科技股份有限公司 | Silymarin extraction method |
| CN104450172B (en) * | 2014-12-10 | 2018-02-16 | 江苏中兴药业有限公司 | A kind of extracting method of Silybum Marianum Gaertn Seed Oil |
| CN104621339A (en) * | 2015-01-23 | 2015-05-20 | 沈阳化工大学 | Method for extracting silybum marianum protein isolate |
| CN106511421B (en) * | 2016-08-30 | 2019-05-17 | 江苏中兴药业有限公司 | A method of purification milk thistle Flavone class compound |
| CN107354000B (en) * | 2017-08-03 | 2020-10-13 | 金寨县益农农业科技开发有限公司 | Peony seed shell rotting spray liquid and using method thereof |
| CN108936652A (en) * | 2018-05-29 | 2018-12-07 | 广西中医药大学 | A kind of health-care fruit jelly and preparation method thereof of hypoglycemic decompression |
| CN108822094A (en) * | 2018-09-17 | 2018-11-16 | 西安利君精华药业有限责任公司 | A kind of silymarin extraction process |
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| CN101381363A (en) * | 2007-09-06 | 2009-03-11 | 天津大学 | Method for extracting macroporous adsorption resin and separating hepadestal from alkaline water |
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