CN102731486A - New method for purifying silymarin - Google Patents
New method for purifying silymarin Download PDFInfo
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- CN102731486A CN102731486A CN2012101448957A CN201210144895A CN102731486A CN 102731486 A CN102731486 A CN 102731486A CN 2012101448957 A CN2012101448957 A CN 2012101448957A CN 201210144895 A CN201210144895 A CN 201210144895A CN 102731486 A CN102731486 A CN 102731486A
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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 the natural organic chemistry field, relate to that a kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, extract and the macroporous resin purification technology through microwave counter current again, obtain the method for high purity SLB.
Background technology:
Silybum marianum seeds contains crude fat 25.05%, and its lipid acid is mainly unsaturated oleic acid (47.46%) and linolic acid (31.79%).The spent meal protein content is 19.58%, is higher than general cereal.Wherein maximum with albumin content, account for 62.60% of total protein.Silymarin protein with in, lower molecular weight is main owing to be rich in acidic amino acid, the white matter iso-electric point mainly is distributed in the neutral meta-acid scope.
SLB is the plant milk extract that from the kind skin of composite family medicinal plant Silymarin seed, extracts, and is yellow powder or knot article sprills, bitter.Be soluble in buck, acetone, ETHYLE ACETATE, ethanol and methyl alcohol, be insoluble in chloroform, water insoluble, staple has Flavonoid substances such as silibinin, Isosilybin, Silydianin and Silychristin.This material has following effect: the protection liver cell is avoided the toxicant infringement, and especially alcohol and environmental pollutant (agricultural chemicals, heavy metal etc.) invasion infringement is with dirty; Have powerful anti-oxidant function, can protect liver cell to avoid radical and destroy, render a service and outclass vitamin E; Promote proteinic synthesizing, accelerate to make the new dirty cell of using, or make liver cell in damaged condition repair voluntarily.Therefore be called as " the big right medicine of guaranteeing ".In addition SLB have radioprotective, anti-ageing, prevent and treat effects such as arteriosclerosis, delay skin aging.This product is widely used in the production of products such as medicine, healthcare products, makeup, food.
The SLB industrial production has several different methods, is cold compression to degrease basically, uses solvent extraction again.In the cold press process, some the pigment wax strippings in the cot are in oil, and SLB has loss.The grouts of oil removing are at first with petroleum ether degreasing, dewaxing, and then are that solvent carries out diacolation or thermal backflow is extracted with ETHYLE ACETATE or alcohol, reclaim solvent then and get the SLB bullion and sell, and seldom have producer that it is proceeded purifying; And ETHYLE ACETATE is in recycling process, and hydrolysis produces acetate, has influence on the yield and the quality of product.
Summary of the invention:
The present invention adopts the biological wall breaking method; Anticipating substitute is rolled in Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae of seed skin shell; Make the oil cells that is wrapped dissociate out; Combine the microwave treatment method again, remove the fat in the seed fast, and degreasing more thoroughly obtains deciding the oily novel method of Silymarin of content.
Silybum marianum seed after the de-oiling is made solvent through microwave reflux extracting device with ethanol, removes albumen in iso-electric point, after macroporous resin adsorption, concentrates, dryly obtains highly purified SLB.The inventive method can obtain Silymarin oil and two products of SLB simultaneously.Be different from traditional cold press oil removing, ethyl acetate extraction is had to the method for single SLB.Shortcomings such as SLB routine techniques extraction yield is relatively low, the running time is long, extracting substance is single have been overcome.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.Its step is following:
(1) biological wall breaking: dry silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution, insulation enzymolysis 60min removes the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell; Make the oil cells that is wrapped dissociate out, improve the grease extraction yield.
(2) Microwave Pretreatment: silybum marianum seed was pulverized the 30-60 mesh sieve; Add 1-6 times of sherwood oil (boiling range 60-90 ℃) solution, carry out Microwave Pretreatment, microwave power is at 300～600W; Frequency 4000～8000MHz; Extraction time 300～400s, extraction temperature is 50～60 ℃ and reclaims sherwood oil, obtains Silymarin oil.
(3) microwave counter current extracts: the silybum marianum seed powder after the de-oiling combines microwave counter current to extract the forward charging with the ethanol of 80-85%. and flowing of backspace water inlet material and water is reverse continuous dynamic flow.Extract 50～60 ℃ of temperature, time 60-80min, 400～600W, frequency 5000～8000MHz; Slag is forced to be pushed to slag notch and is discharged through the spiral conveyer of slagging tap, and the spiral of slagging tap pushes slag simultaneously, and debris in the slag is extruded; Improve the extracting solution yield, ethanol is reclaimed in centrifuging.
(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6-6.5 with hydrochloric acid, separates out protein precipitation, and separating protein is regulated pH value between 9-10 with NaOH again:
(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the Silymarin alkaline solution, make adsorptive single, the 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 the 0.5-1BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 1 6BV;
(7) ethanol elution: at normal temperatures and pressures, with the 2-4BV/h flow velocity, with the ethanol aqueous wash deresination of 70%-95%, the wash-out body is protected and is 3-4BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure reclaims ethanol, vacuum-drying, and micronization obtains SLB
Embodiment: a kind ofly utilize biological wall breaking, twice microwave extraction, and the macroporous resin purification technology, obtain the method for high purity SLB.
Embodiment 1: a kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, again through microwave counter current and macroporous resin purification technology, obtains the method for high purity SLB, and its step is following:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution; Insulation separate 60min; Remove the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, the oil cells that bale broken is wrapped up in dissociates out, improves the grease extraction yield;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 30 mesh sieves, add 4-6 times of sherwood oil (boiling range 60-90 ℃) solution, and carried out Microwave Pretreatment; Microwave power is at 300 W, and frequency 1000MHz extracts time 300s; Extraction temperature is 60 ℃; Reclaim sherwood oil, obtain Silymarin oil 195.3g, de-oiling Herba Silybi mariani powder 793g;
(3) microwave counter current extracts: the de-oiling Herba Silybi mariani powder combines microwave counter current to extract with 80% ethanol, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow.Extract 50 ℃ of temperature, time 60min, 400W, frequency 5000MHz extrudes debris in the slag, and the protein moiety of precipitation separation reclaims ethanol;
(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6 with hydrochloric acid, separates out protein precipitation, separating protein, and using NaOH to regulate pH value again is 9:
(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the nonprotein Silymarin solution, make the adsorptive list, the resin model is the S-8 resin, and the aspect ratio of resin column is 8: 1;
(6) sour water wash-out: at normal temperatures and pressures, with the 0.5BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 1BV;
(7) ethanol elution: at normal temperatures and pressures, with the 2BV/h flow velocity, the ethanol aqueous wash deresination with 70%, elution volume is 3BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure reclaims ethanol, vacuum-drying, and micronization obtains SLB 51g, purity 80.8%.
Case study on implementation 2: a kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, again through microwave counter current and macroporous resin purification technology, obtains the method for high purity SLB, and its step is following:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution; Insulation enzymolysis 60min; Remove the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make the oil cells that is wrapped dissociate out, improve the grease extraction yield;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 40 mesh sieves, add 1-6 times of sherwood oil (boiling range 60-90 ℃) solution, and carried out Microwave Pretreatment; Microwave power is at 400W, and frequency 6000MHz extracts time 400s; Extraction temperature is 60 ℃; 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 combines microwave counter current to extract with 85% ethanol, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow.Extract 60 ℃ of temperature, time 70min, 500W, frequency 6000MHz extrudes debris in the slag, and the protein moiety of precipitation separation reclaims ethanol:
(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, and it is 10 that separating protein uses NaOH to regulate pH value again;
(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the nonprotein Silymarin solution, make adsorptive single, the resin model is the AB-8 resin, and the aspect ratio of resin column is 10: 1;
(6) sour water wash-out: at normal temperatures and pressures, with the 1BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with the 3BV/h flow velocity, the ethanol aqueous wash deresination with 80%, elution volume is 4BV:
(8) drying under reduced pressure: collect ethanol eluate, concentrating under reduced pressure reclaims ethanol, and the vacuum-drying micronization obtains SLB 51.7g, purity 81.2%.
Case study on implementation 3: a kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, again through microwave counter current and macroporous resin purification technology, obtains the method for high purity SLB.Its step is following:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution; Insulation enzymolysis 60min; Remove the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make the oil cells that is wrapped dissociate out, improve the grease extraction yield;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 50 mesh sieves, add 4-6 times of sherwood oil (boiling range 60-90 ℃) solution, and carried out Microwave Pretreatment; Microwave power is at 500W, and frequency 7000MHz extracts time 400s; Extraction temperature is 60 ℃; 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 combines microwave counter current to extract with 80% ethanol, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow.Extract 50 ℃ of temperature, time 80min, 600W, frequency 7000MHz extrudes debris in the slag, and the protein moiety of precipitation separation reclaims ethanol;
(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, protein isolates, and using NaOH to regulate pH value again is 9;
(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the nonprotein Silymarin solution, make the adsorptive list, the resin model is the DA-201 resin, and the aspect ratio of resin column is 12: 1;
(6) sour water wash-out: at normal temperatures and pressures with the 1BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with the 3BV/h flow velocity, the ethanol aqueous wash deresination with 80%, elution volume is 4BV;
(8) drying under reduced pressure: collect ethanol eluate, alkali is pressed and is concentrated, and reclaims ethanol, and the vacuum-drying micronization obtains SLB 50.5g, purity 82%.
Case study on implementation 4: a kind of to utilize biological wall breaking, Microwave Pretreatment to get oily, through microwave counter current and macroporous resin purification technology, obtains the method that high-purity severe edema due to hypofunction of the spleen flies silibin again.Its step is following:
(1) biological wall breaking: 1000g is dry, and silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution; Insulation enzymolysis 60min; Remove the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell, make the oil cells that is wrapped dissociate out, improve the grease extraction yield;
(2) Microwave Pretreatment: silybum marianum seed was pulverized 60 mesh sieves, add 1-6 times of sherwood oil (boiling range 60-90 ℃) solution, and carried out Microwave Pretreatment; Microwave power is at 600W, and frequency 8000MHz extracts time 360s; Extraction temperature is 50 ℃; 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 combines microwave counter current to extract with 80% ethanol, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow.Extract 60 ℃ of temperature, time 80min, 600W, frequency 8000MHz extrudes debris in the slag, and the protein moiety of precipitation separation reclaims ethanol;
(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6.5 with hydrochloric acid, separates out protein precipitation, separating protein, and using NaOH to regulate pH value again is 9;
(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the nonprotein Silymarin solution, make adsorptive single, the resin model is the NKA-9 resin, and the aspect ratio of resin column is 15: 1;
(6) sour water wash-out: at normal temperatures and pressures, with the 1BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 5BV;
(7) ethanol elution: at normal temperatures and pressures, with the 4BV/h flow velocity, the ethanol aqueous wash deresination with 95%, elution volume is 4BV;
(8) drying under reduced pressure: collect ethanol eluate, concentrate, reclaim ethanol, drying under reduced pressure, micronization obtains SLB 49.7g, purity 83.1%.
Claims (10)
- One kind to utilize biological wall breaking, Microwave Pretreatment to get oily, extract and the macroporous resin purification technology through microwave counter current again, obtain the method for high purity SLB.Its step is following:(1) biological wall breaking: dry silybum marianum seed soaks; Add an amount of cellulase, semicellulose enzyme solution, insulation enzymolysis 60min removes the Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae that are wrapped in seed skin shell; Make the oil cells that is wrapped dissociate out, improve the grease extraction yield.(2) pre-treatment de-oiling: silybum marianum seed was pulverized the 30-60 mesh sieve, add 4-6 times of sherwood oil (boiling range 60-90 ℃) solution, and carried out Microwave Pretreatment; Microwave power is at 300～600W; Frequency 4000～8000MHz, extraction time 300～400s, extraction temperature is 50～60 ℃; Reclaim sherwood oil, obtain Silymarin oil;(3) microwave counter current extracts: the silybum marianum seed powder after the de-oiling combines microwave counter current to extract with the ethanol of 80-85%, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow.Extract 50～60 ℃ of temperature, time 60-80min, 400～600W, frequency 5000～8000MHz; Slag is forced to be pushed to slag notch and is discharged through the spiral conveyer of slagging tap, and the spiral of slagging tap is extruded debris in the slag simultaneously to the capable extruding of slag; Improve the extracting solution yield, ethanol is reclaimed in centrifuging.(4) isoelectric precipitation: owing to be rich in acidic amino acid, isoelectric points of proteins mainly is distributed in the neutral meta-acid scope, regulates PH to 6-6.5 with hydrochloric acid, separates out protein precipitation, and separating protein is regulated pH value between 9-10 with NaO again;(5) macroporous resin adsorption: with the pretreated macroporous resin adsorption of process on the Silymarin alkaline solution, make the adsorptive list, the 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 the 0.5-1BV/h flow velocity, use PH is 2 phosphoric acid solution wash-out resin, and elution volume is 1-6BV;(7) ethanol elution: at normal temperatures and pressures, with the 2-4BV/h flow velocity, with the ethanol aqueous wash deresination of 70%-95%, elution volume is 3-1BV;(8) drying under reduced pressure: collect ethanol eluate, alkali is pressed and is concentrated, and reclaims ethanol, vacuum-drying, and micronization obtains SLB.
- 2. according to claim 1 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (1), the enzyme of abolishing Mierocrystalline cellulose, semicellulose, pectin segment and the albuminous membranae employing of seed skin shell is cellulase, hemicellulase, insulation enzymolysis time 60min.
- 3. said to utilize biological wall breaking, Microwave Pretreatment to get oily according to claim 2, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (2), silybum marianum seed powder order number is the 30-60 order, and extraction solvent is a sherwood oil, and dosage is 4-6 a times of raw material.
- 4. according to claim 3 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (2), Microwave Pretreatment power 300～600W, frequency 4000～8000MHz, the extraction time is 300～400s, 50～60 ℃ of extraction temperature.
- 5. according to claim 4 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (3), the silybum marianum seed powder extracts with microwave counter current, the forward charging, and reverse water inlet, flowing of material and water is reverse continuous dynamic flow, extracting solvent is the ethanol of 80-85%
- 6. according to claim 5 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (3), 50～60 ℃ of microwave extraction temperature, time 60-80min, power are 400～600W, frequency is 5000～8000MHz.
- 7. according to claim 6 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (4), the isoelectric points of proteins pH value is 6-6.5, and NaOH buck pH value is adjusted in 9-10.
- 8. according to claim 7 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (5), the macroporous resin model is a kind of in S-8, AB-8, DA-201, the NKA-9 resin, and the aspect ratio of resin column is 8: 1-15: 1.
- 9. according to claim 8 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (6), make eluent with phosphoric acid solution, flow velocity is 0.5-1BV/h, and pH value is 2, and elution volume is 4-6BV.
- 10. according to claim 9 to utilize biological wall breaking, Microwave Pretreatment to get oily, extracts and the macroporous resin purification technology through microwave counter current again, obtains the method for high purity SLB.It is characterized in that: in affiliated step (7), use the ethanol of 70%-95% to be eluent, flow velocity 2-4BV/h, elution volume are 3-4BV.
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| CN103242423A (en) * | 2013-05-13 | 2013-08-14 | 江苏大学 | Method for extracting silybum marianum protein |
| CN103509647A (en) * | 2013-09-27 | 2014-01-15 | 宁波市北仑玉健医药科技有限公司 | Method for preparing silybum marianum oil rich in silymarin |
| CN104450172A (en) * | 2014-12-10 | 2015-03-25 | 江苏中兴药业有限公司 | Fructussilybi oil extraction method |
| CN104621339A (en) * | 2015-01-23 | 2015-05-20 | 沈阳化工大学 | Method for extracting silybum marianum protein isolate |
| 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 |
| CN106511421A (en) * | 2016-08-30 | 2017-03-22 | 江苏中兴药业有限公司 | Method for refining flavonoid compounds in stems and leaves of silybum marianum |
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| 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 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242423A (en) * | 2013-05-13 | 2013-08-14 | 江苏大学 | Method for extracting silybum marianum protein |
| CN103509647A (en) * | 2013-09-27 | 2014-01-15 | 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 |
| CN104450172A (en) * | 2014-12-10 | 2015-03-25 | 江苏中兴药业有限公司 | Fructussilybi oil extraction method |
| CN104621339A (en) * | 2015-01-23 | 2015-05-20 | 沈阳化工大学 | Method for extracting silybum marianum protein isolate |
| CN106511421A (en) * | 2016-08-30 | 2017-03-22 | 江苏中兴药业有限公司 | Method for refining flavonoid compounds in stems and leaves of silybum marianum |
| 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 |
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| 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 |
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