CN101973849A - Method for extracting crude solanesol product from potato stalk by microwave-assisted reversed-phase supercritical CO2 extraction - Google Patents
Method for extracting crude solanesol product from potato stalk by microwave-assisted reversed-phase supercritical CO2 extraction Download PDFInfo
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- CN101973849A CN101973849A CN2010105112749A CN201010511274A CN101973849A CN 101973849 A CN101973849 A CN 101973849A CN 2010105112749 A CN2010105112749 A CN 2010105112749A CN 201010511274 A CN201010511274 A CN 201010511274A CN 101973849 A CN101973849 A CN 101973849A
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Abstract
The invention discloses a method for extracting a crude solanesol product from potato stalks by microwave-assisted reversed-phase supercritical CO2 extraction, which uses potato stalks as the raw material and adopts a microwave-assisted reversed-phase supercritical CO2 extraction technology to fast and efficiently extract the crude solanesol product. The invention overcomes the disadvantage that the yield of the solanesol is reduced as a result of the unavoidable degradation and isomerization of the solanesol in the traditional alkaline saponification process. By using the method, the yield of the solanesol can be up to 75-85%.
Description
Technical field
The present invention relates to a kind of is raw material with the potato haulm, adopts microwave-assisted in conjunction with anti-phase supercritical CO
2Abstraction technique extracts the method for eggplant Buddhist nun alcohol crude product.
Background technology
Eggplant Buddhist nun alcohol is a kind of undersaturated nine polyisoprene primary alconols, belongs to four sesquiterpene alcoholses, mainly is present in the plant of Solanaceae, as eggplant leaf, tobacco leaf, tomato leaf etc.Eggplant Buddhist nun alcohol has unique chain and isolates polyene structure, can be as a lot of medicine synthetic important source material.Key intermediate-ubiquinone that ubiquinone class medicine can not generation in this way also can be used as the synthesis material intermediate of anti-allergy agent, anti-ulcerative drug, hypolipidemic and cancer therapy drug.
Potato (Solanlum tuberosum L.) is the annual herb tuberous plant, is to be only second to wheat, paddy rice, corn the fourth-largest food crop afterwards in the world.China is that world potato produces first state, but behind the potato harvest, and cauline leaf generally all is used as waste and burns or give free rein to rottenly, makes a part " resource " become " source of pollution ", and ecotope has been caused great influence.Therefore, extract eggplant Buddhist nun alcohol in the cauline leaf, turn waste into wealth, not only can reduce pollution, and help improving the added value of agriculture production environment, thus the recycling economy development pattern of realization Sustainable development.
The raw material that extracts eggplant Buddhist nun alcohol both at home and abroad mostly is plant of Solanaceae tobacco, eggplant, tomato etc., and extracting method mostly is organic solvent heating extractings such as normal hexane, ethyl acetate, sherwood oil, but this method solvent-oil ratio is big, and extraction yield is low.Also there is report to adopt ultrasonic wave and microwave-assisted technology to extract in recent years, but more rare to the extraction of eggplant Buddhist nun alcohol in the plant-potato that belongs to Solanaceae together.
More to the report that extracts eggplant Buddhist nun alcohol in the tobacco leaf, especially separation, purifying of seeing medicinal extract after extracting more.Patent CN 101298410A has reported a kind of " adopting centrifugal method and the equipment thereof that extracts eggplant Buddhist nun alcohol that combines of saponification, extraction and low temperature crystallization ", and this method is 70.02% with the eggplant Buddhist nun alcohol content that the pure crude product of 30% eggplant Buddhist nun makes; Patent ZL200610048708.X has reported " a kind of method of effective raising solanesol content in crude product ", and this invention is to be the alkane dissolving washing of 7～12% eggplant Buddhist nun alcohol crude product with C1-C8 with content, makes content greater than 25% eggplant Buddhist nun alcohol crude product; Patent CN 101139274B has authorized a kind of " with the method for synthesizing coenzyme Q 10 by olefin metathetical reaction ", and this method is raw material adopted of synthesizing coenzyme Q 10 with eggplant Buddhist nun alcohol; Patent ZL200610041915.2 has authorized " a kind of method of extraction of high purity solanesol alcohol ", and this method adopts supercritical CO
2The high efficiency separation and purification method of fluid extraction and column chromatography associating extracts eggplant Buddhist nun alcohol from inferior tobacco, and the purity of gained eggplant Buddhist nun alcohol is 96%; Patent CN 1345711 " a kind of method of purifying solanesol ", reported utilize adsorption chromatography and gel permeation chromatography to be not less than 70% eggplant Buddhist nun alcohol extract purifying from purity to obtain purity be elaboration more than 95%; Patent ZL200610038249.7 has authorized a kind of " extracting the method for high-purity solanesol from the low levels solanesol extract ", this method is to adopt purity to be raw material greater than 8% eggplant Buddhist nun alcohol, surpass 95% high-purity solanesol with obtaining content after solvent extraction, the crystallization, the rate of recovery is greater than 85%, but it is many to invent the solvent species that adopts, the process complexity; Patent ZL200410067949.X has authorized " a kind of purification process of eggplant Buddhist nun alcohol ", and this method is to make sorbent material with macroporous resin, adopts the method for column chromatography purification eggplant Buddhist nun alcohol; Patent ZL200610038069.9 has authorized a kind of " underpressure distillation combines the method for extracting eggplant Buddhist nun alcohol with liquid-liquid extraction and crystallization phases ", this method is that the pure crude product of 15～20% eggplant Buddhist nun is purified to 53-56% through the solubilizing agent underpressure distillation, bring up to 82～84% through liquid-liquid extraction purity, eggplant Buddhist nun alcohol content is more than 90% behind the secondary crystal; Patent ZL99117334.1 has authorized a place " extraction process of eggplant Buddhist nun alcohol ", and this method is the method that adopts supercritical liquid extraction technique to come eggplant Buddhist nun alcohol in the extraction separation tobacco leaf, and the percentage extraction of this eggplant Buddhist nun of method institute alcohol is 90%; Patent ZL200510021746.1 has authorized a kind of " liquid liquid two-phase is extracted the method for high-content solanesol extract ", and the content that this method gained soaks eggplant Buddhist nun alcohol is 17～24%.
At present, bibliographical information to the middle eggplant Buddhist nun ethanol-extracted of potato is more rare, patent CN 1712392A discloses " a kind of method of extracting eggplant Buddhist nun alcohol from leaf of potato ", and the content of the eggplant Buddhist nun alcohol straight product that this method obtains can reach more than 90%, calculates by the potato cured leaf to reach 0.78%; Patent CN 1762940A has reported " a kind of extract method for purifying solanesol from leaf of potato and waste tobacco leaf ", and this method is to cook extraction agent with oil, and finally can obtain purity by saponification, extraction, crystallization is 90% eggplant Buddhist nun alcohol product; Patent CN101284765A has reported " a kind of microwave-assisted extracts the method for eggplant Buddhist nun alcohol in the waste of white potato haulm ", and the content of eggplant Buddhist nun alcohol is more than 10% in the eggplant Buddhist nun alcohol crude product of this method gained; Patent CN 1932022B has authorized " a kind of is the method for feedstock production high-purity solanesol with the leaf of potato ", this method adopts lipase auxiliary, adopt the correlation cavitation to extract, to extraction liquid polyamide resin Solid-Phase Extraction, leaf of potato medicinal extract to gained dissolves post crystallization through refluxing then, purity is eggplant Buddhist nun alcohol product 90% or more, the method for this method extraction leaf of potato medicinal extract is loaded down with trivial details, and in a large number with an organic solvent; Patent CN 101497557A " extracts method for purifying solanesol " from leaf of potato, reported that a kind of is raw material with the leaf of potato, by technologies such as microwave auxiliary extraction, saponification, column chromatography, crystallization, recrystallizations, make purity and be the eggplant Buddhist nun alcohol goods more than 95%.
In sum, the extraction object to eggplant Buddhist nun alcohol mostly is tobacco as can be seen, and is mostly by purifying its purity to be increased for the eggplant Buddhist nun alcohol in the tobacco.But actually rare for the extraction bibliographical information of the plant potato that belongs to Solanaceae together, for the eggplant Buddhist nun in medicinal extract alcohol content increase except that adopting microwave-assisted, all do not occur both at home and abroad being that raw material adopts microwave-assisted in conjunction with anti-phase supercritical CO to potato haulm
2Abstraction technique extracts the report of eggplant Buddhist nun alcohol.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of microwave-assisted in conjunction with anti-phase supercritical CO
2The method of eggplant Buddhist nun alcohol crude product is extracted in extraction from potato haulm.This method is to be raw material with the potato haulm, utilizes microwave-assisted in conjunction with anti-phase supercritical CO
2Abstraction technique extracts the novel method of eggplant Buddhist nun alcohol crude product fast and efficiently.And overcome the traditional technology alkali soapization and inevitably made degraded of eggplant Buddhist nun alcohol or isomerization, thereby the shortcoming that eggplant Buddhist nun alcohol yield is reduced, and reduced the reagent loss that saponification in the leaching process brought, greatly reduce energy consumption, and turn waste into wealth, minimizing improves the added value of agriculture production to the pollution of environment, thereby realizes the recycling economy development pattern of Sustainable development.
For solving the problems of the technologies described above, a kind of microwave-assisted of the present invention is in conjunction with anti-phase supercritical CO
2The method of eggplant Buddhist nun alcohol crude product is extracted in extraction from potato haulm, comprise the steps:
(1) getting potato haulm pulverizes, cross 40 mesh sieves, mix with ethyl acetate then, the potato haulm in the described mixture and the weight of ethyl acetate and volume ratio are 10g: 50～200ml, in temperature is that 40～70 ℃, microwave frequency are that 2450MHz, power are under the condition of 200～700W, stir with 150 rev/mins speed, microwave-assisted extracted 1 hour, suction filtration under 0.08MPa then, united extraction liquid, under 55～60 ℃, 0.08MPa, concentrate substance A, the content of eggplant Buddhist nun alcohol is 5%～6.5%;
(2) substance A is used 95% dissolve with ethanol, substance A and 95% alcoholic acid weight and volume ratio are 10g: 100～200mL, utilize the reversed phase extraction technology, and substance A is a 20L/h entrainment agent system by flow, enters CO
2Supercritical extraction unit, 40～60 ℃ of extraction temperature, separating still pressure is 10～20MPa, the separating still temperature is 30～60 ℃; Static extracting pressure is 100-300bar, extraction 30～60min; Dynamic extraction pressure is 100～300bar, extraction 1～5h, CO
2Flow is an abstraction purification under the condition of 5Kg/h, in extraction process, reclaims supercritical CO
2Extract, merge the back concentrate substance B, promptly get eggplant Buddhist nun alcohol crude product, the content of eggplant Buddhist nun alcohol is 35%～45% in this crude product, the pure yield of eggplant Buddhist nun reaches 75～85%, compares substance A, removal of impurity reaches 70～80%.
Described entrainment agent system is 85% ethanol.
Utilize the eggplant Buddhist nun alcohol content of the various eggplant Buddhist nun alcohol goods that relate among high effective liquid chromatography for measuring the present invention, condition determination is as follows:
The high performance liquid chromatography parameter:
Chromatographic column: C
18
Eluent: methyl alcohol: alcoholic acid volume ratio=40%: 60%
Elution rate: 1ml/min,
Detect wavelength: 211nm.
The beneficial effect of characteristics of the present invention and generation:
The present invention is to be raw material with the potato haulm, adopts microwave-assisted in conjunction with anti-phase supercritical CO
2Abstraction technique extracts eggplant Buddhist nun alcohol, step is easy, easy handling, and extraction yield is up to 85%, overcome the traditional technology alkali soapization and inevitably made degraded of eggplant Buddhist nun alcohol or isomerization, thereby the shortcoming that eggplant Buddhist nun alcohol yield is reduced, and reduced the reagent loss that saponification in the leaching process brought, greatly reduce energy consumption, and turn waste into wealth, minimizing improves the added value of agriculture production to the pollution of environment, thereby realizes the recycling economy development pattern of Sustainable development.The present invention makes full use of the good resources advantage of Gansu potato, utilizes microwave-assisted in conjunction with anti-phase supercritical CO
2Abstraction technique is developed this product, and market outlook are good, and economic benefit is wide.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail
The HPLC figure of the eggplant Buddhist nun alcohol that Fig. 1 prepares for method of the present invention;
The yield figure of the eggplant Buddhist nun alcohol product that Fig. 2 prepares for method of the present invention.
Embodiment
The present invention is further described below in conjunction with drawings and Examples.
Embodiment 1:
1. get potato haulm, pulverize, cross 40 mesh sieves, the powder of getting the potato haulm of 10g mixes with the certain volume ethyl acetate, (solid-to-liquid ratio of mixture is weight (g): volume (ml)=10: 50, in temperature is that 40 ℃, microwave frequency are that 2450MHz, power are under the condition of 700W, stirs with 150 rev/mins speed, and microwave-assisted extracted 1 hour, suction filtration under 0.08MPa then, united extraction liquid, under 60 ℃, 0.08MPa, concentrate substance A, content is 5%;
With substance A with 95% dissolve with ethanol (substance A and 95% alcoholic acid weightmeasurement ratio are 10g/200mL) after, utilize the reversed phase extraction technology, the ethanol with 85% is entrainment agent, flow is 20L/h, substance A enters CO by this entrainment agent system
2Supercritical extraction unit, 50 ℃ of extraction temperature, separating still pressure is 10MPa, the separating still temperature is 60 ℃; Static extracting pressure is 100bar, extraction 60min; Dynamic extraction pressure 300bar, extraction 3h, CO
2Flow is an abstraction purification under the condition of 5Kg/h, in extraction process, reclaims supercritical CO
2Extract, merge the back concentrate substance B.
3.HPLC the content of detection material B is 35%, eggplant Buddhist nun alcohol yield reaches 85%, compares substance A, improves 7 times, and removal of impurity reaches 70%.
1. get potato haulm, pulverize, cross 40 mesh sieves, the powder of getting the potato haulm of 10g mixes with the certain volume ethyl acetate, (solid-to-liquid ratio of mixture is weight (g): volume (ml)=10: 200, in temperature is that 70 ℃, microwave frequency are that 2450MHz, power are under 200 the condition, stirs with 150 rev/mins speed, and microwave-assisted extracted 1 hour, suction filtration under 0.08MPa then, united extraction liquid, under 55 ℃, 0.08MPa, concentrate substance A, content is 6.5%;
With substance A with 95% dissolve with ethanol (substance A and 95% alcoholic acid weightmeasurement ratio are 10g/100mL) after, utilize the reversed phase extraction technology, the ethanol with 85% is entrainment agent, flow is 20L/h, substance A enters CO by this entrainment agent system
2Supercritical extraction unit, 40 ℃ of extraction temperature, separating still pressure is 20MPa, the separating still temperature is 30 ℃; Static extracting pressure is 300bar, extraction 30min; Dynamic extraction pressure 100bar, extraction 1h, CO
2Flow is an abstraction purification under the condition of 5Kg/h, in extraction process, reclaims supercritical CO
2Extract, merge the back concentrate substance B.
3.HPLC the content of detection material B is 45%, eggplant Buddhist nun alcohol yield reaches 75%, compares substance A, improves 7 times, and removal of impurity reaches 80%.
Embodiment 3
1. get potato haulm, pulverize, cross 40 mesh sieves, the powder of getting the potato haulm of 10g mixes with the certain volume ethyl acetate, (solid-to-liquid ratio of mixture is weight (g): volume (ml)=10: 150, in temperature is that 60 ℃, microwave frequency are that 2450MHz, power are under the condition of 500W, stirs with 150 rev/mins speed, and microwave-assisted extracted 1 hour, suction filtration under 0.08MPa then, united extraction liquid, under 57 ℃, 0.08MPa, concentrate substance A, content is 6%;
With substance A with 95% dissolve with ethanol (substance A and 95% alcoholic acid weightmeasurement ratio are 10g/150mL) after, utilize the reversed phase extraction technology, the ethanol with 85% is entrainment agent, flow is 20L/h, substance A enters CO by this entrainment agent system
2Supercritical extraction unit, 60 ℃ of extraction temperature, separating still pressure is 15MPa, the separating still temperature is 50 ℃; Static extracting pressure is 200bar, extraction 45min; Dynamic extraction pressure 200bar, time 5h, CO
2Flow is an abstraction purification under the condition of 5Kg/h, in extraction process, reclaims supercritical CO
2Extract, merge the back concentrate substance B.
3.HPLC the content of detection material B is 40%, eggplant Buddhist nun alcohol yield reaches 80%, compares substance A, improves 6 times, and removal of impurity reaches 75%.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (2)
1. a microwave-assisted is in conjunction with anti-phase supercritical CO
2The method of eggplant Buddhist nun alcohol crude product is extracted in extraction from potato haulm, it is characterized in that this method may further comprise the steps:
(1) getting potato haulm pulverizes, cross 40 mesh sieves, mix with ethyl acetate then, the potato haulm in the described mixture and the weight of ethyl acetate and volume ratio are 10g: 50～200ml, in temperature is that 40～70 ℃, microwave frequency are that 2450MHz, power are under the condition of 200～700W, stir with 150 rev/mins speed, microwave-assisted extracted 1 hour, suction filtration under 0.08MPa then, united extraction liquid, under 55～60 ℃, 0.08MPa, concentrate substance A, the content of eggplant Buddhist nun alcohol is 5%～6.5%;
(2) substance A is used 95% dissolve with ethanol, substance A and 95% alcoholic acid weight and volume ratio are 10g: 100～200mL, utilize the reversed phase extraction technology, and substance A is a 20L/h entrainment agent system by flow, enters CO
2Supercritical extraction unit, 40～60 ℃ of extraction temperature, separating still pressure is 10～20MPa, the separating still temperature is 30～60 ℃; Static extracting pressure is 100-300bar, extraction 30～60min; Dynamic extraction pressure is 100～300bar, extraction 1～5h, CO
2Flow is an abstraction purification under the condition of 5Kg/h, in extraction process, reclaims supercritical CO
2Extract, merge the back concentrate substance B, promptly get eggplant Buddhist nun alcohol crude product, the content of eggplant Buddhist nun alcohol is 35%～45% in this crude product, the pure yield of eggplant Buddhist nun reaches 75～85%.
2. method according to claim 1 is characterized in that, described entrainment agent system is 85% ethanol.
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| CN2010105112749A CN101973849B (en) | 2010-10-19 | 2010-10-19 | Method for extracting crude solanesol product from potato stalk by microwave-assisted reversed-phase supercritical CO2 extraction |
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| CN2010105112749A CN101973849B (en) | 2010-10-19 | 2010-10-19 | Method for extracting crude solanesol product from potato stalk by microwave-assisted reversed-phase supercritical CO2 extraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046375A (en) * | 2014-06-11 | 2014-09-17 | 西安交通大学 | Microwave-assisted supercritical CO2 extraction system and microwave-assisted supercritical CO2 extraction method for crude oil in oil sand |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5160044A (en) * | 1992-02-20 | 1992-11-03 | National Tsing Hua University | Process for separating ethanol from aqueous solution |
| CN101284765A (en) * | 2008-02-20 | 2008-10-15 | 西北师范大学 | Process for abstracting solanesol in waste of white potato haulm auxiliary by microwave |
-
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- 2010-10-19 CN CN2010105112749A patent/CN101973849B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5160044A (en) * | 1992-02-20 | 1992-11-03 | National Tsing Hua University | Process for separating ethanol from aqueous solution |
| CN101284765A (en) * | 2008-02-20 | 2008-10-15 | 西北师范大学 | Process for abstracting solanesol in waste of white potato haulm auxiliary by microwave |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046375A (en) * | 2014-06-11 | 2014-09-17 | 西安交通大学 | Microwave-assisted supercritical CO2 extraction system and microwave-assisted supercritical CO2 extraction method for crude oil in oil sand |
| CN104046375B (en) * | 2014-06-11 | 2016-04-13 | 西安交通大学 | Microwave-assisted supercritical CO 2the system and method for extraction crude oil from oil sand |
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