CN102816155B - Preparation method of silymarin - Google Patents
Preparation method of silymarin Download PDFInfo
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- CN102816155B CN102816155B CN201210261514.3A CN201210261514A CN102816155B CN 102816155 B CN102816155 B CN 102816155B CN 201210261514 A CN201210261514 A CN 201210261514A CN 102816155 B CN102816155 B CN 102816155B
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Abstract
The invention relates to a preparation method of silymarin, in particular to a preparation method of high-purity silymarin. The preparation method comprises the steps of deoiling raw material; extracting with ethyl acetate by micro-boiling reflux extraction or static soaking extraction to obtain silymarin extractive solution; concentrating; preparing silymarin crude product precipitate; re-dissolving the crude product precipitate with ethanol solution, centrifuging to collect supernatant, and passing the supernatant through neutral alumina column for adsorption; eluting adsorbed silymarin with ethanol solution to obtain eluate; vacuum-concentrating the eluate to recover ethanol, and vacuum-drying to obtain silymarin finished product. The method has the advantages of simple operation, low preparation cost, easy industrialized production, and high product purity.
Description
Technical field
The present invention relates to a kind of preparation method of silymarin, especially relate to a kind of preparation method of high purity silymarin.
Background technology
Silymarin is the mixture of flavanolignanes compound, comprise the compounds such as silibinin (silybin), dehydro-silibinin (dehydrosi-silybin), silybinomer (silybinomer), Isosilybin (isosilybin), Silychristin (silychristin), Silydianin (silydianin), wherein silibinin is its main active ingredient.Silymarin is to be soluble in acetone, methyl alcohol, ethanol, is insoluble in chloroform, water-fast medicine, and silymarin is widely applied in liver disease field, also has in addition antitumor, effect such as treatment diabetes etc.Along with the development of preparation technique, silymarin will have more wide application prospect at field of medicaments.The important source material of silymarin or healthcare products and makeup.
China Patent Publication No. CN1463970A, open day on December 31st, 2003, a kind of preparation method of silymarin is disclosed, taking pulverize silybum marianum seed as raw material, adopt supercritical carbon dioxide extraction method to extract silybum marianum seed oil, with organic solvent extraction silymarin, extracting solution is under supercritical co environment, separate and obtain high purity silymarin, the method has been simplified sepn process, shorten extraction time, weak point is: the method adopts supercritical carbon dioxide extraction method, complicated operation, preparation cost is high, be difficult to form commercial scale production.
Summary of the invention
The object of the invention is to solve the deficiency that existing silymarin preparation method complicated operation, preparation cost are high, be difficult to form commercial scale production, provide a kind of simple to operate, preparation cost is low, the preparation method of easy commercial scale production, silymarin that product purity is high.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for silymarin, described preparation method comprises the following steps:
1) raw material oil removing: Silymarin medicinal material squeezing oil removing, oil pump capacity is controlled at 28 ~ 33%, obtains a Silymarin medicinal material blob of slag after squeezing;
2) extract: a Silymarin medicinal material blob of slag is placed in ethyl acetate solvent and extracts to obtain silymarin extracting solution, and the volume of ethyl acetate is 4 ~ 6 times of Silymarin medicinal material blob of slag quality, extract 65 ~ 75 DEG C of temperature, extraction time 1 ~ 2h, extraction time 2 times or 3 times;
3) concentrated: silymarin extracting solution vacuum concentration is obtained to concentrated solution to proportion 0.94 ~ 0.96g/ml, and the vacuum tightness of vacuum concentration is-0.08 ~-0.09Mpa, and temperature is 50 ~ 80 DEG C;
4) rough: in concentrated solution, to add the purified water of 18 ~ 22 times of concentrated solution volumes to disperse, jitter time 1 ~ 1.5h, 50 ~ 85 DEG C of temperature, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 4000 ~ 6000rpm, centrifugation time 20 ~ 30min;
5) absorption: 94 ~ 96% dissolve with ethanol solution for silymarin crude product is precipitated, ethanolic soln consumption is 2 ~ 4 times of silymarin crude product precipitation quality, 45 ~ 55 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, centrifugal rotational speed is 4000 ~ 6000rpm, centrifugation time 20 ~ 30min, supernatant liquor is crossed neutral alumina column absorption;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 94 ~ 96% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 4 ~ 6 times of retention volume, and ethanolic soln flow velocity is 0.8 ~ 4.5ml/min, and ethanolic soln temperature is 25 ~ 50 DEG C;
7) concentrate drying: silymarin elutriant vacuum concentration to alcoholic strength≤5 ° concentrated solution, then concentrated solution vacuum-drying obtains silymarin finished product, the vacuum tightness of described vacuum concentration is-0.08 ~ 0.-09Mpa, temperature is 50 ~ 80 DEG C, described vacuum drying vacuum tightness is-0.08 ~-0.09Mpa, temperature is 50 ~ 80 DEG C, and be 1 ~ 3h time of drying.
The present invention is by Silymarin medicinal material squeezing oil removing, and oil yield is controlled at 28-33%, prevents from that oil yield is too high to cause in Silymarin medicinal material silymarin to follow oil running off together, and the medicinal raw material silymarin content that is used for extracting silymarin is low, is unfavorable for subsequent extracted; Employing ethyl acetate is extracted, and extraction efficiency is high, and cost is low; By first silymarin extracting solution concentration and recovery ethyl acetate, reduce preparation cost, then in concentrated solution, add purified water that silymarin is uniformly dispersed, a large amount of water-soluble impurities are fully dissolved in purified water, then centrifugal that silymarin crude product precipitates; Silymarin crude product precipitation is dissolved with dissolve with ethanol, then the centrifugal supernatant liquor that obtains, supernatant liquor, by neutral alumina column chromatography, is then used ethanolic soln wash-out, collect silymarin elutriant, then silymarin elutriant obtains high purity silymarin finished product through vacuum concentration and vacuum-drying.
As preferably, step 2) extract and adopt micro-refluxing extraction of boiling, extract 70 ~ 75 DEG C of temperature, extraction time 1 ~ 1.5h, extraction time is 2 times.Adopt the micro-refluxing extraction of boiling of comparatively high temps, extraction time is short, and extraction time can reduce, and extraction efficiency is high.
As preferably, step 2) extract and adopt static dipping to extract, extract 65 DEG C ~ 70 DEG C of temperature, extraction time 1.5 ~ 2h, extraction time is 3 times.Adopt the static dipping of lower temperature to extract, Energy Intensity Reduction in leaching process, can save preparation cost.
As preferably, in step 4), dispersion process adopts mechanical stirring auxiliary, mixing speed 40 ~ 100rpm, churning time 8 ~ 15min.Employing mechanical stirring is auxiliary, and silymarin is fully disperseed, and prevents the polymerization of uniting, and removal of impurity is high, and the purity of the product of follow-up preparation is high.
As preferably, in step 5), the particle diameter of neutral alumina is 20 ~ 200 orders, and applied sample amount and neutral alumina mass ratio are 1:2 ~ 8, and the aspect ratio of post is 3 ~ 8:1, and the temperature control of chromatography process center pillar is at 20 ~ 40 DEG C.Neutral alumina particle diameter is controlled at 20 ~ 200 orders, and specific surface area is large, high adsorption capacity, and the amount of applied sample amount and neutral alumina is controlled at 1:2 ~ 8, and pillar aspect ratio is controlled at 3 ~ 8:1, advantages of good adsorption effect, silymarin adsorption rate is high, and product yield is high.
The invention has the beneficial effects as follows: 1) operational condition gentleness, simple to operate, be easy to commercial scale production; 2) extract solvent recovery cycle utilization, utilization ratio is high, and preparation cost is low; 3) preparation method's good reliability, constant product quality, foreign matter content is low, and silymarin purity is high.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
embodiment 1:
A preparation method for silymarin, described preparation method comprises the following steps:
1) raw material oil removing: Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at the manufacturer of 28%(oil press zhai: Zhejiang Pan Feng Machinery Manufacturing Co., Ltd.; Model: 6YL-78; Rotating speed: 69-208rpm; Power: 5.5 kilowatts);
2) extract: a Silymarin medicinal material blob of slag is placed in the static dipping of ethyl acetate solvent and extracts to obtain silymarin extracting solution, and the volume of ethyl acetate is 6 times of Silymarin medicinal material blob of slag quality, extracts 65 DEG C of temperature, extraction time 1.5h, extraction time is 3 times;
3) concentrated: to be-0.09Mpa that temperature is under the condition of 50 DEG C, to be concentrated into proportion 0.94g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 18 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.5h, temperature is 50 DEG C, adopts mechanical stirring auxiliary in dispersion process, and mixing speed is 100rpm, churning time 8min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 6000rpm, centrifugation time 20min;
5) absorption: by silymarin crude product precipitation 96% dissolve with ethanol solution, ethanolic soln consumption is 2 times of silymarin crude product precipitation quality, 45 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 6000rpm, centrifugation time 20min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 20 orders, and applied sample amount and neutral alumina mass ratio are 1:2, the aspect ratio of post is 3:1, and the temperature control of adsorption process center pillar is at 20 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 94% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 4 times of retention volume, and ethanolic soln flow velocity is 0.8ml/min, and ethanolic soln temperature is 20 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.09Mpa, temperature is under 50 DEG C of conditions, to be concentrated into 5 ° of alcoholic strengths (alcoholic strength adopts Ebullioscope in 20 DEG C of measurements), then in vacuum tightness be-0.09Mpa, temperature is that under the condition of 50 DEG C, dry 3h obtains silymarin finished product, detect silymarin finished product content according to the HPLC measuring method of the silymarin content of 7.0 editions regulations of European Pharmacopoeia, mobile phase A is phosphoric acid: methyl alcohol: water=0.5:35:65 (v/v/v); Mobile phase B is phosphoric acid: methyl alcohol: water=0.5:50:50 (v/v/v), and detection wavelength is 288nm, 20 ~ 30 DEG C of column temperatures, chromatographic column is 125mm × 4mm, taking octadecyl silane, (5 μ are m) as weighting agent, and flow velocity is 0.8ml/min, and the yield of silymarin finished product and purity are in table 1.
embodiment 2:
A preparation method for silymarin, described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at the manufacturer of 33%(oil press zhai: Zhejiang Pan Feng Machinery Manufacturing Co., Ltd.; Model: 6YL-78, rotating speed: 69-208rpm; Power: 5.5 kilowatts);
2) extract: a Silymarin medicinal material blob of slag is placed in the micro-refluxing extraction of boiling of ethyl acetate solvent and obtains silymarin extracting solution, and the volume of ethyl acetate is 4 times of Silymarin medicinal material blob of slag quality, extract 75 DEG C of temperature, extraction time 1h, extraction time is 2 times;
3) concentrated: to be-0.08Mpa that temperature is under 80 DEG C of conditions, to be concentrated into proportion 0.96g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 22 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1h, temperature is 85 DEG C, and dispersion process mid-early stage adopts mechanical stirring auxiliary, and mixing speed is 40rpm, churning time 15min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 4000rpm, centrifugation time 30min;
5) absorption: by silymarin crude product precipitation 94% dissolve with ethanol solution, ethanolic soln consumption is 4 times of silymarin crude product precipitation quality, 55 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 4000rpm, centrifugation time 30min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 200 orders, and applied sample amount and neutral alumina mass ratio are 1:8, the aspect ratio of post is 8:1, and the temperature control of chromatography process center pillar is at 30 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 96% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 6 times of retention volume, and ethanolic soln flow velocity is 4.5ml/min, and ethanolic soln temperature is 40 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.08Mpa, temperature is under 80 DEG C of conditions, to be concentrated into 4 ° of alcoholic strengths (alcoholic strength adopts Ebullioscope in 20 DEG C of measurements), then at vacuum tightness-0.08Mpa, temperature is that under 80 DEG C of conditions, dry 1h obtains silymarin finished product, detect silymarin finished product content according to the HPLC measuring method of the silymarin content of 7.0 editions regulations of European Pharmacopoeia, mobile phase A is phosphoric acid: methyl alcohol: water=0.5:35:65 (v/v/v); Mobile phase B is phosphoric acid: methyl alcohol: water=0.5:50:50 (v/v/v), and detection wavelength is 288nm, 20 ~ 30 DEG C of column temperatures, chromatographic column is 125mm × 4mm, taking octadecyl silane, (5 μ are m) as weighting agent, and flow velocity is 0.8ml/min, and the yield of silymarin finished product and purity are in table 1.
embodiment 3:
A preparation method for silymarin, described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at the manufacturer of 30%(oil press zhai: Zhejiang Pan Feng Machinery Manufacturing Co., Ltd., model: 6YL-78, rotating speed: 69-208rpm.Power: 5.5 kilowatts);
2) extract: a Silymarin medicinal material blob of slag is placed in ethyl acetate solvent and adopts static dipping to extract to obtain silymarin extracting solution, and the volume of ethyl acetate is 5 times of Silymarin medicinal material blob of slag quality, extracts temperature 70 C, extraction time 2h, extraction time is 3 times;
3) concentrated: to be-0.085Mpa that temperature is under 65 DEG C of conditions, to be concentrated into proportion 0.95g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 20 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.25h, temperature is 65 DEG C, and the employing mechanical stirring of dispersion process mid-early stage is auxiliary, and mixing speed is 70rpm, churning time 10min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 5000rpm, centrifugation time 25min;
5) absorption: by silymarin crude product precipitation 95% dissolve with ethanol solution, ethanolic soln consumption is 3 times of silymarin crude product precipitation quality, 50 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 5000rpm, centrifugation time 25min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 100 orders, and applied sample amount and neutral alumina mass ratio are 1:5, the aspect ratio of post is 5:1, and the temperature control of chromatography process center pillar is at 30 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 95% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 5 times of retention volume, and ethanolic soln flow velocity is 3ml/min, and ethanolic soln temperature is 25 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.085Mpa, temperature is under 65 DEG C of conditions, to be concentrated into 3 ° of alcoholic strengths (alcoholic strength adopts Ebullioscope in 20 DEG C of measurements), then in vacuum tightness be-0.085Mpa, temperature is that under 65 DEG C of conditions, dry 2h obtains silymarin finished product, detect silymarin finished product content according to the HPLC measuring method of the silymarin content of 7.0 editions regulations of European Pharmacopoeia, mobile phase A is phosphoric acid: methyl alcohol: water=0.5:35:65 (v/v/v); Mobile phase B is phosphoric acid: methyl alcohol: water=0.5:50:50 (v/v/v), and detection wavelength is 288nm, 20 ~ 30 DEG C of column temperatures, chromatographic column is 125mm × 4mm, taking octadecyl silane, (5 μ are m) as weighting agent, and flow velocity is 0.8ml/min, and the yield of silymarin finished product and purity are in table 1.
embodiment 4:
A preparation method for silymarin, described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at the manufacturer of 30%(oil press zhai: Zhejiang Pan Feng Machinery Manufacturing Co., Ltd., model: 6YL-78, rotating speed: 69-208rpm.Power: 5.5 kilowatts);
2) extract: a Silymarin medicinal material blob of slag is placed in the micro-refluxing extraction of boiling of ethyl acetate solvent and obtains silymarin extracting solution, and the volume of ethyl acetate is 5 times of Silymarin medicinal material blob of slag quality, extract temperature 70 C, extraction time 1.5h, extraction time is 2 times;
3) concentrated: to be-0.085Mpa that temperature is under 65 DEG C of conditions, to be concentrated into proportion 0.95g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 20 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.25h, temperature is 65 DEG C, and the employing mechanical stirring of dispersion process mid-early stage is auxiliary, and mixing speed is 70rpm, churning time 10min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 5000rpm, centrifugation time 25min;
5) absorption: by silymarin crude product precipitation 95% dissolve with ethanol solution, ethanolic soln consumption is 3 times of silymarin crude product precipitation quality, 50 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 5000rpm, centrifugation time 25min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 100 orders, and applied sample amount and neutral alumina mass ratio are 1:5, the aspect ratio of post is 5:1, and the temperature control of chromatography process center pillar is at 25 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 95% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 5 times of retention volume, and ethanolic soln flow velocity is 3ml/min, and ethanolic soln temperature is 30 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.085Mpa, temperature is under 65 DEG C of conditions, to be concentrated into 3 ° of alcoholic strengths (alcoholic strength adopts Ebullioscope in 20 DEG C of measurements), then in vacuum tightness be-0.085Mpa, temperature is that under 65 DEG C of conditions, dry 2h obtains silymarin finished product, detect silymarin finished product content according to the HPLC measuring method of the silymarin content of 7.0 editions regulations of European Pharmacopoeia, mobile phase A is phosphoric acid: methyl alcohol: water=0.5:35:65 (v/v/v); Mobile phase B is phosphoric acid: methyl alcohol: water=0.5:50:50 (v/v/v), and detection wavelength is 288nm, 20 ~ 30 DEG C of column temperatures, chromatographic column is 125mm × 4mm, taking octadecyl silane, (5 μ are m) as weighting agent, and flow velocity is 0.8ml/min, and the yield of silymarin finished product and purity are in table 1.
Claims (4)
1. a preparation method for silymarin, is characterized in that described preparation method comprises the following steps:
1) raw material oil removing: Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at 28%;
2) extract: a Silymarin medicinal material blob of slag is placed in the static dipping of ethyl acetate solvent and extracts to obtain silymarin extracting solution, and the volume of ethyl acetate is 6 times of Silymarin medicinal material blob of slag quality, extracts 65 DEG C of temperature, extraction time 1.5h, extraction time is 3 times;
3) concentrated: to be-0.09Mpa that temperature is under the condition of 50 DEG C, to be concentrated into proportion 0.94g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 18 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.5h, temperature is 50 DEG C, adopts mechanical stirring auxiliary in dispersion process, and mixing speed is 100rpm, churning time 8min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 6000rpm, centrifugation time 20min;
5) absorption: by silymarin crude product precipitation 96% dissolve with ethanol solution, ethanolic soln consumption is 2 times of silymarin crude product precipitation quality, 45 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 6000rpm, centrifugation time 20min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 20 orders, and applied sample amount and neutral alumina mass ratio are 1:2, the aspect ratio of post is 3:1, and the temperature control of adsorption process center pillar is at 20 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 94% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 4 times of retention volume, and ethanolic soln flow velocity is 0.8ml/min, and ethanolic soln temperature is 20 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.09Mpa, temperature is under 50 DEG C of conditions, to be concentrated into 5 ° of alcoholic strengths, in vacuum tightness is-0.09Mpa then, temperature is that under the condition of 50 DEG C, dry 3h obtains silymarin finished product.
2. a preparation method for silymarin, is characterized in that described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at 33%;
2) extract: a Silymarin medicinal material blob of slag is placed in the micro-refluxing extraction of boiling of ethyl acetate solvent and obtains silymarin extracting solution, and the volume of ethyl acetate is 4 times of Silymarin medicinal material blob of slag quality, extract 75 DEG C of temperature, extraction time 1h, extraction time is 2 times;
3) concentrated: to be-0.08Mpa that temperature is under 80 DEG C of conditions, to be concentrated into proportion 0.96g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 22 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1h, temperature is 85 DEG C, and dispersion process mid-early stage adopts mechanical stirring auxiliary, and mixing speed is 40rpm, churning time 15min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 4000rpm, centrifugation time 30min;
5) absorption: by silymarin crude product precipitation 94% dissolve with ethanol solution, ethanolic soln consumption is 4 times of silymarin crude product precipitation quality, 55 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 4000rpm, centrifugation time 30min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 200 orders, and applied sample amount and neutral alumina mass ratio are 1:8, the aspect ratio of post is 8:1, and the temperature control of chromatography process center pillar is at 30 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 96% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 6 times of retention volume, and ethanolic soln flow velocity is 4.5ml/min, and ethanolic soln temperature is 40 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.08Mpa, temperature is under 80 DEG C of conditions, to be concentrated into 4 ° of alcoholic strengths, then at vacuum tightness-0.08Mpa, temperature is that under 80 DEG C of conditions, dry 1h obtains silymarin finished product.
3. a preparation method for silymarin, is characterized in that described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at 30%;
2) extract: a Silymarin medicinal material blob of slag is placed in ethyl acetate solvent and adopts static dipping to extract to obtain silymarin extracting solution, and the volume of ethyl acetate is 5 times of Silymarin medicinal material blob of slag quality, extracts temperature 70 C, extraction time 2h, extraction time is 3 times;
3) concentrated: to be-0.085Mpa that temperature is under 65 DEG C of conditions, to be concentrated into proportion 0.95g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 20 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.25h, temperature is 65 DEG C, and the employing mechanical stirring of dispersion process mid-early stage is auxiliary, and mixing speed is 70rpm, churning time 10min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 5000rpm, centrifugation time 25min;
5) absorption: by silymarin crude product precipitation 95% dissolve with ethanol solution, ethanolic soln consumption is 3 times of silymarin crude product precipitation quality, 50 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 5000rpm, centrifugation time 25min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 100 orders, and applied sample amount and neutral alumina mass ratio are 1:5, the aspect ratio of post is 5:1, and the temperature control of chromatography process center pillar is at 30 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 95% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 5 times of retention volume, and ethanolic soln flow velocity is 3ml/min, and ethanolic soln temperature is 25 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.085Mpa, temperature is under 65 DEG C of conditions, to be concentrated into 3 ° of alcoholic strengths, in vacuum tightness is-0.085Mpa then, temperature is that under 65 DEG C of conditions, dry 2h obtains silymarin finished product.
4. a preparation method for silymarin, is characterized in that described preparation method comprises the following steps:
1) Silymarin medicinal material adopts oil press zhai squeezing oil removing to obtain a Silymarin medicinal material blob of slag, and oil pump capacity is controlled at 30%;
2) extract: a Silymarin medicinal material blob of slag is placed in the micro-refluxing extraction of boiling of ethyl acetate solvent and obtains silymarin extracting solution, and the volume of ethyl acetate is 5 times of Silymarin medicinal material blob of slag quality, extract temperature 70 C, extraction time 1.5h, extraction time is 2 times;
3) concentrated: to be-0.085Mpa that temperature is under 65 DEG C of conditions, to be concentrated into proportion 0.95g/ml to obtain concentrated solution in vacuum tightness by silymarin extracting solution;
4) rough: the purified water that adds 20 times of concentrated solution volumes in concentrated solution, make in concentrated solution silymarin dispersed, jitter time 1.25h, temperature is 65 DEG C, and the employing mechanical stirring of dispersion process mid-early stage is auxiliary, and mixing speed is 70rpm, churning time 10min, disperse to finish rear centrifugation and obtain silymarin crude product precipitation, centrifugal rotational speed is 5000rpm, centrifugation time 25min;
5) absorption: by silymarin crude product precipitation 95% dissolve with ethanol solution, ethanolic soln consumption is 3 times of silymarin crude product precipitation quality, 50 DEG C of solvent temperatures, after dissolving, centrifugal impurity elimination obtains supernatant liquor, and centrifugal rotational speed is 5000rpm, centrifugation time 25min, supernatant liquor is crossed neutral alumina column absorption, and the particle diameter of neutral alumina is 100 orders, and applied sample amount and neutral alumina mass ratio are 1:5, the aspect ratio of post is 5:1, and the temperature control of chromatography process center pillar is at 25 DEG C;
6) wash-out: the silymarin that the ethanolic soln wash-out of employing 95% is adsorbed on neutral alumina column obtains silymarin elutriant, and ethanolic soln consumption is 5 times of retention volume, and ethanolic soln flow velocity is 3ml/min, and ethanolic soln temperature is 30 DEG C;
7) concentrate drying: silymarin elutriant in vacuum tightness is-0.085Mpa, temperature is under 65 DEG C of conditions, to be concentrated into 3 ° of alcoholic strengths, in vacuum tightness is-0.085Mpa then, temperature is that under 65 DEG C of conditions, dry 2h obtains silymarin finished product.
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| CN103012384B (en) * | 2012-12-13 | 2015-06-17 | 三原润禾植化有限公司 | Method for extracting silymarin from silybum marianum |
| CN107087480A (en) * | 2016-02-18 | 2017-08-25 | 四川利君精华制药股份有限公司 | A kind of medicinal milk thistle cultivation technique and silymarin extracting method |
| 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 |
| CN106474194A (en) * | 2016-12-16 | 2017-03-08 | 宁波沪信药物技术有限公司 | Combination of two kinds of plant amedica and application thereof |
| CN106589052B (en) * | 2017-01-16 | 2020-06-23 | 江苏中兴药业有限公司 | Method for degreasing and dehydrating silybum marianum seed kernel protein coarse powder |
| CN108578263A (en) * | 2018-06-20 | 2018-09-28 | 吉林农业科技学院 | Silymarin Skin whitening care cosmetics |
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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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| 任冰如等.水飞蓟素提取和水飞蓟宾纯化的研究.《时珍国医国药》.2012,第23卷(第3期),第655-656页. * |
| 水飞蓟素提取和水飞蓟宾纯化的研究;任冰如等;《时珍国医国药》;20120331;第23卷(第3期);第1段，第3段，2.1,2.5 * |
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