CN1736533A - Supercritical CO2 process for extracting effective medicinal components from Chinese angelica - Google Patents
Supercritical CO2 process for extracting effective medicinal components from Chinese angelica Download PDFInfo
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- CN1736533A CN1736533A CN 200510014555 CN200510014555A CN1736533A CN 1736533 A CN1736533 A CN 1736533A CN 200510014555 CN200510014555 CN 200510014555 CN 200510014555 A CN200510014555 A CN 200510014555A CN 1736533 A CN1736533 A CN 1736533A
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Abstract
The invention discloses a method for extraction of medicinal available composition from Chinese angelica with a supercritical carbon dioxide, belonging to the technique of extracting the medicinal available composition from Chinese angelica. The method contains the following process: adding the root of Chinese angelica into extraction kettle after disintegrating or cutting, and adding CO2 into extraction kettle after condensation and booster, the operation pressure of extraction being 10- 50MPa and the temperature being 32- 90 Deg. C, the mass ratio of entrainer ethanol to material being 0.5: 1- 3: 1, the entrainer being mixed and soaked with raw material or pumped by the entrainer pump and separated from solute and CO2 in separator after extraction, the pressure of the first stage separator being 3- 15MPa and temperature being 25- 40Deg. C, and the pressure of second stage separator being 3- 15MPa and temperature being 20- 30Deg. C, the product or solvent dissolved product being received from receiver, the solvent being evaporated and dried to prepare the final product, CO2 used circularly, and the whole extraction time being 0.5- 5 hours. The method has merits as the following: the energy consumption small, the operation simple, the extraction condition mild, the extraction time short, and so on.
Description
Technical field
The present invention relates to a kind of method of supercritical carbon dioxide extracting effective medicinal components from Chinese angelica, belong to the effective medicinal components from Chinese angelica extractive technique.
Background technology
Radix Angelicae Sinensis derives from the dry rhizome of umbelliferae angelica Angelica sinensis (Oliv) Diels, contains effective medicinal components such as forulic acid, has to activate blood circulation and disperse blood clots, and the effect of menstruation regulating blood nourishing medicinal has the title of " women's panacea "; It is sallow to can be used for the deficiency of blood, dizzy palpitaition, irregular menstruation, dysmenorrhoea amenorrhoea, asthenia cold abdominalgia, the dry constipation of intestines, the treatment of diseases such as arthralgia due to wind-dampness.The method that proposes forulic acid at present from Chinese medicine mainly is a percolation, and supercritical carbon dioxide extracting and ultrasonic extraction also have report.
Ji Chunru etc. have compared percolation and ultrasonic extraction prepares danggui extract, danggui liujin gao, and the result shows that ultrasonic extraction not only can improve total solids content in the danggui extract, danggui liujin gao, and ferulaic acid content has improved 59.7% than pharmacopeia percolation in the medicinal extract.
Zhang Hong etc. have investigated and have utilized supercritical CO
2The process conditions of extracting forulic acid from Ligusticum wallichii are 70 ℃ of extraction temperature, extracting pressure 35MPa, CO
2Flow 25kg/h and extraction time 2.5h; With this understanding, the yield of forulic acid can reach 0.04%, and ultrasonic method receipts cream rate only is 0.015%.
The percolation solvent load is big, the post processing complexity; Though ultrasonic extraction has also carried out some researchs at present, only is confined to carry out simple process condition experiment on the breadboard small-scale, does not appear in the newspapers and utilize supercritical carbon dioxide extraction method to extract forulic acid from Radix Angelicae Sinensis.
Summary of the invention
The object of the invention is to provide a kind of method of supercritical carbon dioxide extracting effective medicinal components from Chinese angelica.This method has low energy consumption, simple to operate, advantages such as extraction conditions is gentle, the easy control of parameter.
The present invention is realized that by following technical proposals its feature comprises following process: with the extraction kettle of packing into after pulverizing of Radix Angelicae Sinensis rhizome or the pelletizing, CO
2After boosting, condensation enters extraction kettle, extracting operation pressure is 10-50MPa, extraction temperature is 32-90 ℃, the quality of entrainer ethanol and raw material mass ratio are 0.5: 1-3: 1, entrainer can mix immersion with raw material, also can directly adopt the entrainer pump to be continuously pumped into, solute and CO are realized in the extraction back in separating still
2Separation, one-level separating still pressure is that 3-15MPa, temperature are 25-40 ℃, secondary separating still pressure is that 3-15MPa, temperature are 20-30 ℃, in receiver, obtain product or dissolved the solvent of product, after the solvent evaporation drying final products, CO
2Recycle.The whole extraction time is 0.5-5 hour.
Compare with percolation, this method has low energy consumption, simple to operate, advantage such as extraction conditions is gentle, operating parameter is easily controlled and extraction time is short, and solvent load is little, is easy to subsequent treatment.
The specific embodiment
Example 1 is soaked the Radix Angelicae Sinensis raw material 1000g that pulverizes 2 hours in 500g ethanol, and extracting pressure is 10MPa, and extraction temperature is 35 ℃; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 25 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 20 ℃, collects product, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 2 hours.Extract gets medicinal extract 23.5g behind rotary evaporation in vacuo, ferulaic acid content is 0.908% in the medicinal extract.
Example 2 is soaked the Radix Angelicae Sinensis raw material 1000g that pulverizes 8 hours in 1500g ethanol, and extracting pressure is 50MPa, and extraction temperature is 65 ℃; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 40 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 30 ℃, collects product, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 3 hours, and extract gets medicinal extract 33.5g behind rotary evaporation in vacuo, and ferulaic acid content is 0.848% in the medicinal extract.
Example 3 drops into the Radix Angelicae Sinensis raw material 1000g that pulverizes in the extraction kettle, and extracting pressure is 10MPa, and extraction temperature is 35 ℃, and 500g ethanol is continuously pumped into by the entrainer pump simultaneously; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 25 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 20 ℃, collects extract, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 2 hours, and extract gets medicinal extract 22.3g behind rotary evaporation in vacuo, and ferulaic acid content is 0.915% in the medicinal extract.Example 4 drops into the Radix Angelicae Sinensis raw material 1000g that pulverizes in the extraction kettle, and extracting pressure is 50MPa, and extraction temperature is 65 ℃, and 1200g ethanol is continuously pumped into by the entrainer pump simultaneously; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 40 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 30 ℃, collects extract, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 3 hours, and extract gets medicinal extract 30.8g behind rotary evaporation in vacuo, and ferulaic acid content is 0.852% in the medicinal extract.
Example 5 is immersed in the Radix Angelicae Sinensis raw material 1000g that pulverizes in the 500g ethanol after 4 hours, and extracting pressure is 10MPa, and extraction temperature is 35 ℃, is continuously pumped into 500g ethanol by the entrainer pump simultaneously; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 25 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 20 ℃, collects extract, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 2 hours, and extract gets medicinal extract 30.0g behind rotary evaporation in vacuo, and ferulaic acid content is 0.963% in the medicinal extract.
Example 6 is immersed in the Radix Angelicae Sinensis raw material 1000g that pulverizes in the 500g ethanol after 4 hours, and extracting pressure is 10MPa, and extraction temperature is 35 ℃, is continuously pumped into 1000g ethanol by the entrainer pump simultaneously; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 25 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 20 ℃, collects extract, CO by receiver
2Flow velocity 10Kg/h, the extraction time is 3 hours, and extract gets medicinal extract 40.2g behind rotary evaporation in vacuo, and ferulaic acid content is 0.926% in the medicinal extract.
Example 7 drops into the Radix Angelicae Sinensis raw material 1000g that pulverizes in the extraction kettle, and extracting pressure is 30MPa, and extraction temperature is 45 ℃; Separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 25 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 20 ℃, collects product by receiver, obtains Chinese angelica volatile oil 23.6g.Extract remainder was immersed in the 500g ethanol after 4 hours, and extracting pressure is 30MPa, and extraction temperature is 45 ℃, and separation condition is constant, collects product by receiver, extract behind rotary evaporation in vacuo medicinal extract 20.5g, ferulaic acid content is 1.05% in the medicinal extract.
Example 8 drops into the Radix Angelicae Sinensis raw material 1000g that pulverizes in the extraction kettle, and extracting pressure is 50MPa, and extraction temperature is 65 ℃, separation condition: separating still 1: separating pressure is 6MPa, and separation temperature is 40 ℃; Separating still 2: separating pressure 4MPa, separation temperature is 30 ℃, collects product by receiver, obtains Chinese angelica volatile oil 25.8g.With extract remainder be immersed in the 800g ethanol soak 4 hours after, extracting pressure is 50MPa, extraction temperature is 65 ℃; Collect product by receiver, separation condition is constant, and extract gets medicinal extract 30.0g behind rotary evaporation in vacuo, and ferulaic acid content is 0.956% in the medicinal extract.
Claims (1)
1. the method for a supercritical carbon dioxide extracting effective medicinal components from Chinese angelica, its feature comprises following process: the Radix Angelicae Sinensis rhizome is pulverized or pelletizing after the extraction kettle of packing into, CO
2After boosting, condensation enters extraction kettle, extracting operation pressure is 10-50MPa, extraction temperature is 32-90 ℃, the quality of entrainer ethanol and raw material mass ratio are 0.5: 1-3: 1, entrainer can mix immersion with raw material, also can directly adopt the entrainer pump to be continuously pumped into, solute and CO are realized in the extraction back in separating still
2Separation, one-level separating still pressure is that 3-15MPa, temperature are 25-40 ℃, secondary separating still pressure is that 3-15MPa, temperature are 20-30 ℃, in receiver, obtain product or dissolved the solvent of product, after the solvent evaporation drying final products, CO
2Recycle, the whole extraction time is 0.5-5 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510014555 CN1736533A (en) | 2005-07-18 | 2005-07-18 | Supercritical CO2 process for extracting effective medicinal components from Chinese angelica |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921186A (en) * | 2012-09-18 | 2013-02-13 | 长春工业大学 | Method for extracting and separating Chinese medicinal components by subcritical fluid |
| CN103386215A (en) * | 2013-07-29 | 2013-11-13 | 嘉文丽（福建）化妆品有限公司 | Method for continuously extracting active components of Hibiscus taiwanensis by utilizing supercritical carbon dioxide |
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2005
- 2005-07-18 CN CN 200510014555 patent/CN1736533A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921186A (en) * | 2012-09-18 | 2013-02-13 | 长春工业大学 | Method for extracting and separating Chinese medicinal components by subcritical fluid |
| CN103386215A (en) * | 2013-07-29 | 2013-11-13 | 嘉文丽（福建）化妆品有限公司 | Method for continuously extracting active components of Hibiscus taiwanensis by utilizing supercritical carbon dioxide |
| CN103386215B (en) * | 2013-07-29 | 2015-11-18 | 嘉文丽（福建）化妆品有限公司 | The method of supercritical continuous carbon dioxide extraction Taiwan Cortex seu Flos Hibisci taiwanenss active ingredient |
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