CN102824392A - Method for extracting florilenalin from helenium bigelovii leaves - Google Patents
Method for extracting florilenalin from helenium bigelovii leaves Download PDFInfo
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- CN102824392A CN102824392A CN 201210350244 CN201210350244A CN102824392A CN 102824392 A CN102824392 A CN 102824392A CN 201210350244 CN201210350244 CN 201210350244 CN 201210350244 A CN201210350244 A CN 201210350244A CN 102824392 A CN102824392 A CN 102824392A
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Abstract
The invention discloses a method for extracting florilenalin from helenium bigelovii leaves. The method comprises the following steps: grinding helenium bigelovii serving as a raw material into 20-80 meshes, put in a supercritical extraction kettle; introducing liquid CO2 and dynamically extracting for 2-3 hours under the conditions that the pressure is 15-25 MPa and the temperature is 40-50 DEG C; separating the extract at the pressure of 5-10 MPa and the temperature of 50-60 DEG C and dispersed the extract by using hot water; absorbing by macroporous resin; carrying out ethanol solution gradient elution, and concentrating eluant under reduced pressure; extracting the concentrated solution with ethyl acetate; and concentrating and refrigerating and crystallizing the extract solution; and finally drying at a low temperature to obtain the florilenalin. The method is simple to operate, high in extraction efficiency and low in pollution, and is easy for industrial production.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of method of from the Helenium autumnale L. leaf, extracting autumnolide.
Background technology
Helenium autumnale L. is a Compositae Dugaldia plant, cries wing golden pheasant chrysanthemum again, and Helenium autumnale L. originates in the North America, is distributed in the U.S. and Canada.The property happiness warm environment on the sunny side, cold-resistant drought-enduring, fit and give birth to 15 ℃ to 28 ℃ of temperature, do not select soil, vitality is extremely indomitable, under adapt circumstance, the breeding rate of expansion is very fast, except viewing and admiring, Helenium autumnale L. can also be medicinal.Aspect the traditional Chinese medical science, the wounded in the battle all herbal medicine with Helenium autumnale L. is used to treat diseases such as the hepatic and renal YIN deficiency, Light-headedness, soreness of the waist and knees, early whitening of beard and hair, rheumatic arthritis.
Modern study is found to contain the terpene lactone effective ingredient in the Helenium autumnale L., like helenalin, amaralin, spire helenalin, autumnolide etc., has than powerful antitumor, antiinflammatory, effect such as antibiotic.
The method of from Helenium autumnale L., extracting total lactone generally adopts organic reagent to extract, and extraction obtains repeatedly again.Like the foreign literature disclosed method is the Helenium autumnale L. pulverizing, uses chloroform extraction, and extract is collected water layer with hexane, methanol, water mixed solvent dissolving, concentrates back reuse chloroform extraction, separates obtaining autumnolide repeatedly through silica gel column layer.As stated, extract the method for total lactone in the existing Helenium autumnale L., method is complicated, and the organic reagent consumption is big, especially adopts chloroform extraction, is not suitable for suitability for industrialized production.
Summary of the invention
The present invention is intended to overcome the defective and the deficiency of prior art, and a kind of method of from the Helenium autumnale L. leaf, extracting autumnolide is provided.
The objective of the invention is to realize through following technical scheme:
A kind of method of from the Helenium autumnale L. leaf, extracting total lactone is characterized in that: be raw material with the Helenium autumnale L., pulverize the 20-80 order, drop into supercritical extraction reactor, feed liquid CO
2, under pressure 15-25MPa, temperature 40-50 ℃ condition, dynamic extraction 2-3 hour; At pressure 5-10MPa, temperature 50-60 ℃ parsing extract, extract disperses with hot water, adds in the macroporous resin to adsorb; The alcoholic solution gradient elution is collected eluent, concentrating under reduced pressure; Concentrated solution is used ethyl acetate extraction, and extract concentrates back cold preservation crystallization, and cold drying promptly gets total lactone.
Described liquid CO
2Flow velocity is 20-30kg/h.
Optional polar macroporous resin of described macroporous resin or non-polar macroporous resin, a kind of among the optional AB-8 of model, D101, HPD100 or the ADS-21.
Described alcoholic solution gradient elution is: earlier with 3-10 times of column volume 10-30% alcoholic solution eluting impurity, reuse 2-8 times of column volume 40-90% ethanol elution effective ingredient.
Described total lactone content is not less than 90%.
Advantage of the present invention is to have adopted supercritical CO
2Extraction, low-temperature extraction, efficient is high, and energy consumption is low, and solvent is liquid CO
2, cleanliness without any pollution.
Advantage of the present invention also adopts purification by macroporous resin, and is simple to operate, and eluting solvent is single, is beneficial to recovery, is easy to suitability for industrialized production.
To combine the specific embodiment to further specify the present invention below.
The specific embodiment:
Embodiment 1:
Helenium autumnale L. is dry, pulverizes 60 orders, gets 1kg and drops into supercritical extraction reactor, feeds liquid CO with the 20kg/h flow velocity
2, 40 ℃ of extracting pressure 18MPa, temperature are set, reach above-mentioned parameter after, dynamic extraction 3 hours; Resolve extract for 50 ℃ in pressure 6MPa, temperature, extract disperses with hot water, adds in the AB-8 macroporous resin column to adsorb; With 3 times of column volumes, 30% alcoholic solution eluting impurity, 5 times of column volumes of reuse, 70% ethanol elution effective ingredient is about eluent concentrating under reduced pressure 100ml earlier; Reuse equal-volume ethyl acetate extraction 3 times, extract concentrate about 50ml, the cold preservation crystallization; Leach cold drying, get total lactone 4g, content 93%.
Embodiment 2:
Helenium autumnale L. is dry, pulverizes 80 orders, gets 1kg and drops into supercritical extraction reactor, feeds liquid CO with the 25kg/h flow velocity
2, 50 ℃ of extracting pressure 25MPa, temperature are set, reach above-mentioned parameter after, dynamic extraction 3 hours; Resolve extract for 60 ℃ in pressure 8MPa, temperature, extract disperses with hot water, adds in the ADS-21 macroporous resin column to adsorb; With 10 times of column volumes, 10% alcoholic solution eluting impurity, 3 times of column volumes of reuse, 90% ethanol elution effective ingredient is about eluent concentrating under reduced pressure 200ml earlier; Reuse equal-volume ethyl acetate extraction 2 times, extract concentrate about 80ml, the cold preservation crystallization; Leach cold drying, get total lactone 3.1g, content 95.1%.
Embodiment 3:
Helenium autumnale L. is dry, pulverizes 20 orders, gets 1kg and drops into supercritical extraction reactor, feeds liquid CO with the 22kg/h flow velocity
2, 45 ℃ of extracting pressure 20MPa, temperature are set, reach above-mentioned parameter after, dynamic extraction 3 hours; Resolve extract for 60 ℃ in pressure 7MPa, temperature, extract disperses with hot water, adds in the D101 macroporous resin column to adsorb; With 4 times of column volumes, 20% alcoholic solution eluting impurity, 4 times of column volumes of reuse, 60% ethanol elution effective ingredient is about eluent concentrating under reduced pressure 100ml earlier; Reuse equal-volume ethyl acetate extraction 3 times, extract concentrate about 50ml, the cold preservation crystallization; Leach cold drying, get total lactone 4.6g, content 91.3%.
Claims (5)
1. a method of from the Helenium autumnale L. leaf, extracting total lactone is characterized in that: be raw material with the Helenium autumnale L., pulverize the 20-80 order, drop into supercritical extraction reactor, feed liquid CO
2, under pressure 15-25MPa, temperature 40-50 ℃ condition, dynamic extraction 2-3 hour; At pressure 5-10MPa, temperature 50-60 ℃ parsing extract, extract disperses with hot water, adds in the macroporous resin to adsorb; The alcoholic solution gradient elution is collected eluent, concentrating under reduced pressure; Concentrated solution is used ethyl acetate extraction, and extract concentrates back cold preservation crystallization, and cold drying promptly gets total lactone.
2. the method for from the Helenium autumnale L. leaf, extracting total lactone according to claim 1 is characterized in that described liquid CO
2Flow velocity is 20-30kg/h.
3. the method for from the Helenium autumnale L. leaf, extracting total lactone according to claim 1 is characterized in that optional polar macroporous resin of described macroporous resin or non-polar macroporous resin, a kind of among the optional AB-8 of model, D101, HPD100 or the ADS-21.
4. the method for from the Helenium autumnale L. leaf, extracting total lactone according to claim 1; It is characterized in that described alcoholic solution gradient elution is: earlier with 3-10 times of column volume 10-30% alcoholic solution eluting impurity, reuse 2-8 times of column volume 40-90% ethanol elution effective ingredient.
5. the method for from the Helenium autumnale L. leaf, extracting total lactone according to claim 1 is characterized in that described total lactone content is not less than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210350244 CN102824392A (en) | 2012-09-20 | 2012-09-20 | Method for extracting florilenalin from helenium bigelovii leaves |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210350244 CN102824392A (en) | 2012-09-20 | 2012-09-20 | Method for extracting florilenalin from helenium bigelovii leaves |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110179790A (en) * | 2019-07-02 | 2019-08-30 | 广西医科大学 | A kind of preparation and application inhibiting Hepatic Stellate Cell Activation drug |
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2012
- 2012-09-20 CN CN 201210350244 patent/CN102824392A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110179790A (en) * | 2019-07-02 | 2019-08-30 | 广西医科大学 | A kind of preparation and application inhibiting Hepatic Stellate Cell Activation drug |
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Application publication date: 20121219 |