CN102875563A - Method for extracting podophyllotoxin from dysosma versipellis - Google Patents
Method for extracting podophyllotoxin from dysosma versipellis Download PDFInfo
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- CN102875563A CN102875563A CN2012103561846A CN201210356184A CN102875563A CN 102875563 A CN102875563 A CN 102875563A CN 2012103561846 A CN2012103561846 A CN 2012103561846A CN 201210356184 A CN201210356184 A CN 201210356184A CN 102875563 A CN102875563 A CN 102875563A
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Abstract
The invention relates to a method for extracting podophyllotoxin from dysosma versipellis. The method comprises the steps as follows: extracting with waveform to obtain extract; adding the extract to macroreticular resin column to absorb; eluting; recovering alcohol in a pressure reduced way; concentrating; adding the concentrate to polyamide chromatographic column; eluting; carrying out support detection with homogenous polyamide film by utilizing the eluant; collecting; recovering the solvent in a pressure reduced way; adding acetone to crystallize; separating and crystallizing; washing; and drying to obtain the product. The method provided by the invention is simple in operation, less in consumption of solvent, low in production cost, stable in technology, low in energy consumption and pollution, and high in purity of the obtained product (99%), and is suitable for experiment and industrial preparation and preparative production.
Description
Technical field
The present invention relates to a kind of extracting method of podophyllotoxin, particularly a kind of method of from Dysosma versipellis, extracting podophyllotoxin.
Background technology
Dysosma versipellis is the root and rhizome for Berberidaceae plant Dysosma versipellis, Dysosma Pleiantha and dysosma veitchii Fu.Dissipating phlegm and resolving masses; Stasis-dispelling and pain-killing; Clearing heat and detoxicating.Be used for cough; Swelling and pain in the throat; Scrofula; Goiter and tumor; Carbuncle is swollen; Furunculosis; Venomous snake bite; Wound; Bi Zheng.Contain podophyllotoxin in the Dysosma versipellis, structural formula is:
Studies show that: podophyllotoxin for pointed condyloma, superficial epitheliomatosis (such as superficial or wetting property basal cell carcinoma, squamous cell epithelioma and basal squamous cell epithelioma), front upper rind gall keratosis, seborrheic keratosis, day photosensitiveness angling and post-radiation keratosis, childhood papilloma of larynx, wart (verruca vulgaris, verruca filiformis).Podophyllotoxin energy establishment simplexvirus suppresses the cell mitotic division in mid-term, is used for the toxicity venereal disease.98% above podophyllotoxin is made 0.5% tincture, and to be used for pointed condyloma evident in efficacy.Still be not applicable to preparation technology's report of high-purity podophyllotoxin industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of extracting method that is beneficial to large production operation, the high podophyllotoxin of product purity.
The object of the present invention is achieved like this:
A kind of method of from Dysosma versipellis, extracting podophyllotoxin, described method is comprised of the following step: get Dysosma versipellis, pulverize, adding the concentration that its quality 15-20 doubly measures volume is the ethanol of 80-90%, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W, extract 2-4 time, each 5-20 minute, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the macroporous adsorptive resins and adsorbs, the 50-70% ethanol elution, collect 3-8 and doubly measure the column volume elutriant, decompression recycling ethanol is also concentrated, is added on the polymeric amide chromatography post methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain.
Above-mentioned a kind of method of from Dysosma versipellis, extracting podophyllotoxin, the concentration that adds ethanol before the described microwave extracting is 85%, consumption is 18 times of amount volumes of raw materials quality.
Above-mentioned a kind of method of extracting podophyllotoxin from Dysosma versipellis, described microwave extracting power is 500W, extracts each 10 minutes 3 times.
Above-mentioned a kind of method of extracting podophyllotoxin from Dysosma versipellis, described macroporous adsorbent resin are selected from a kind of among D101 type, D102 type, AB-8 type, HPD400, the HPD826.
Above-mentioned a kind of method of extracting podophyllotoxin from Dysosma versipellis, described macroporous adsorbent resin wash-out is 60% with the concentration of ethanol.
Above-mentioned a kind of method of extracting podophyllotoxin from Dysosma versipellis, described macroporous adsorbent resin wash-out is 5 times of amount column volumes with the collecting amount of ethanol.
Above-mentioned a kind of method of extracting podophyllotoxin from Dysosma versipellis, described polymeric amide are selected from a kind of in polyamide 6, polyamide 66, polymeric amide 11, polymeric amide 12, the polyamide 610.
Preparation gained podophyllotoxin adopts following method to detect.
Embodiment 1HPLC method is measured podophyllotoxin purity
The chromatographic condition chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: methanol-water (90:10); Flow velocity: 1m1/min; Detect wavelength: 224nm; Column temperature: 30 ℃.
The measuring method precision takes by weighing podophyllotoxin 2mg, places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10uL to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.
Adopt the present invention to prepare podophyllotoxin, compared with prior art, method of the present invention has simple to operate, and solvent consumption is few, production cost is low, process stabilizing, and energy consumption is little, pollute littlely, products obtained therefrom purity high (99%) is applicable to laboratory and industrialization half preparation and the production of preparation property.
Specific embodiment
Form by the following examples is described in further detail foregoing of the present invention again, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example, all technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1 gets Dysosma versipellis 10kg, pulverize, the concentration that adds 15 times of amounts of its quality volume is 80% ethanol, drops in the microwave extracting apparatus and carries out microwave extracting, extraction power 300W, extract 2 times, each 5 minutes, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the D101 type macroporous adsorptive resins and adsorbs 50% ethanol elution, collect 3 times of amount column volume elutriants, decompression recycling ethanol is also concentrated, is added on polymeric amide (polyamide 6) chromatography column methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain podophyllotoxin 1.25g, detect through HPLC, purity is 99.5%.
Embodiment 2 gets Dysosma versipellis 10kg, pulverize, the concentration that adds 18 times of amounts of its quality volume is 85% ethanol, drops in the microwave extracting apparatus and carries out microwave extracting, extraction power 400W, extract 3 times, each 10 minutes, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the D102 type macroporous adsorptive resins and adsorbs 60% ethanol elution, collect 5 times of amount column volume elutriants, decompression recycling ethanol is also concentrated, is added on polymeric amide (polyamide 66) chromatography column methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain podophyllotoxin 1.15g, detect through HPLC, purity is 99.8%.
Embodiment 3 gets Dysosma versipellis 10kg, pulverize, the concentration that adds 20 times of amounts of its quality volume is 90% ethanol, drops in the microwave extracting apparatus and carries out microwave extracting, extraction power 600W, extract 4 times, each 20 minutes, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the AB-8 type macroporous adsorptive resins and adsorbs 70% ethanol elution, collect 8 times of amount column volume elutriants, decompression recycling ethanol is also concentrated, is added on polymeric amide (polymeric amide 11) chromatography column methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain podophyllotoxin 1.18g, detect through HPLC, purity is 99.2%.
Embodiment 4 gets Dysosma versipellis 10kg, pulverize, the concentration that adds 18 times of amounts of its quality volume is 85% ethanol, drops in the microwave extracting apparatus and carries out microwave extracting, extraction power 500W, extract 3 times, each 10 minutes, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the HPD400 type macroporous adsorptive resins and adsorbs 70% ethanol elution, collect 8 times of amount column volume elutriants, decompression recycling ethanol is also concentrated, is added on polymeric amide (polymeric amide 12) chromatography column methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain podophyllotoxin 1.28g, detect through HPLC, purity is 99.6%.
Embodiment 5 gets Dysosma versipellis 10kg, pulverize, the concentration that adds 18 times of amounts of its quality volume is 85% ethanol, drops in the microwave extracting apparatus and carries out microwave extracting, extraction power 500W, extract 3 times, each 10 minutes, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the HPD826 type macroporous adsorptive resins and adsorbs 70% ethanol elution, collect 8 times of amount column volume elutriants, decompression recycling ethanol is also concentrated, is added on polymeric amide (polyamide 610) chromatography column methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain podophyllotoxin 1.31g, detect through HPLC, purity is 99.7%.
Claims (7)
1. method of from Dysosma versipellis, extracting podophyllotoxin, it is characterized in that described method is comprised of the following step: get Dysosma versipellis, pulverize, adding the concentration that its quality 15-20 doubly measures volume is the ethanol of 80-90%, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W, extract 2-4 time, each 5-20 minute, combining extraction liquid, filter, decompression recycling ethanol is also concentrated, joins on the macroporous adsorptive resins and adsorbs, the 50-70% ethanol elution, collect 3-8 and doubly measure the column volume elutriant, decompression recycling ethanol is also concentrated, is added on the polymeric amide chromatography post methylene chloride-methanol mixed solvent wash-out take ratio as 4:1, launch as supporting detection with stating eluent more than the class polyamide layer of the same race, collection is corresponding to the stream part of Rf=4-5 on the polyamide layer, and decompression and solvent recovery adds the acetone crystallization, fractional crystallization, washing, be drying to obtain.
2. described a kind of method of from Dysosma versipellis, extracting podophyllotoxin according to claim 1, the concentration that it is characterized in that adding before the described microwave extracting ethanol is 85%, consumption is 18 times of amount volumes of raw materials quality.
3. described a kind of method of extracting podophyllotoxin from Dysosma versipellis according to claim 1 is characterized in that described microwave extracting power is 500W, extracts each 10 minutes 3 times.
4. described a kind of method of extracting podophyllotoxin from Dysosma versipellis according to claim 1 is characterized in that described macroporous adsorbent resin is selected from a kind of among D101 type, D102 type, AB-8 type, HPD400, the HPD826.
5. described a kind of method of extracting podophyllotoxin from Dysosma versipellis according to claim 1 is characterized in that described macroporous adsorbent resin wash-out is 60% with the concentration of ethanol.
6. described a kind of method of extracting podophyllotoxin from Dysosma versipellis according to claim 1 is characterized in that described macroporous adsorbent resin wash-out is 5 times with the collecting amount of ethanol and measures column volumes.
7. described a kind of method of extracting podophyllotoxin from Dysosma versipellis according to claim 1 is characterized in that described polymeric amide is selected from a kind of in polyamide 6, polyamide 66, polymeric amide 11, polymeric amide 12, the polyamide 610.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098583A (en) * | 2013-04-09 | 2014-10-15 | 中国医学科学院药物研究所 | Podophyllotoxin crystal X material, preparation method, pharmaceutical composition and use |
| CN104666383A (en) * | 2014-12-30 | 2015-06-03 | 铜仁学院 | Technology for microwave-assisted extraction of dysosma versipellis flavonoids compound |
| CN106800508A (en) * | 2017-01-14 | 2017-06-06 | 华北理工大学 | New benzoic acid derivative and preparation method thereof in wild anise, using and pharmaceutical composition |
| CN107383041A (en) * | 2017-07-17 | 2017-11-24 | 长沙爱扬医药科技有限公司 | A kind of method that podophyllotoxin and Hyperoside are extracted from Dysosma versipellis |
| CN112125917A (en) * | 2020-11-04 | 2020-12-25 | 中国科学院西北高原生物研究所 | Extraction method of podophyllotoxin |
-
2012
- 2012-09-24 CN CN2012103561846A patent/CN102875563A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098583A (en) * | 2013-04-09 | 2014-10-15 | 中国医学科学院药物研究所 | Podophyllotoxin crystal X material, preparation method, pharmaceutical composition and use |
| CN104098583B (en) * | 2013-04-09 | 2018-02-02 | 中国医学科学院药物研究所 | Podophyllotoxin crystalline substance X-type material and preparation method and its pharmaceutical composition and purposes |
| CN104666383A (en) * | 2014-12-30 | 2015-06-03 | 铜仁学院 | Technology for microwave-assisted extraction of dysosma versipellis flavonoids compound |
| CN104666383B (en) * | 2014-12-30 | 2018-01-23 | 铜仁学院 | A kind of technique of microwave radiation exaraction Dysosma versipellis flavone compound |
| CN106800508A (en) * | 2017-01-14 | 2017-06-06 | 华北理工大学 | New benzoic acid derivative and preparation method thereof in wild anise, using and pharmaceutical composition |
| CN106800508B (en) * | 2017-01-14 | 2019-03-12 | 华北理工大学 | New benzoic acid derivative and preparation method thereof, application and pharmaceutical composition in wild illiciumverum |
| CN107383041A (en) * | 2017-07-17 | 2017-11-24 | 长沙爱扬医药科技有限公司 | A kind of method that podophyllotoxin and Hyperoside are extracted from Dysosma versipellis |
| CN112125917A (en) * | 2020-11-04 | 2020-12-25 | 中国科学院西北高原生物研究所 | Extraction method of podophyllotoxin |
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Application publication date: 20130116 |