CN102335316A - Extraction method of raw total saponins from fresh dioscorea plants - Google Patents

Extraction method of raw total saponins from fresh dioscorea plants Download PDF

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CN102335316A
CN102335316A CN2010105859117A CN201010585911A CN102335316A CN 102335316 A CN102335316 A CN 102335316A CN 2010105859117 A CN2010105859117 A CN 2010105859117A CN 201010585911 A CN201010585911 A CN 201010585911A CN 102335316 A CN102335316 A CN 102335316A
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microwave
rhizoma dioscoreae
total saponin
fresh rhizoma
class plant
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CN2010105859117A
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CN102335316B (en
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万绍平
郑小非
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Abstract

The invention relates to an extraction method of raw total saponins and in particular to an extraction method of raw total saponins from fresh dioscorpea plants. The extraction method of the raw total saponins from fresh dioscorpea plants mainly comprises the following steps: crushing, fermenting, radiating with microwave, performing secondary crushing, immerging into a solvent, filtering a mixed solution and recycling the solvent. Compared with the traditional extraction method, the extraction method provided by the invention adopts a method of secondary crushing after microwave radiation, so that cellular content is quickly expanded by virtue of microwave radiation to cause sufficient expansion of cell walls accordingly, and secondary crushing is carried out to wholly disintegrate the cell walls, so that the cellular content is completely released and sufficiently contacted with the solvent, therefore, the extract can be sufficiently dissolved in the solvent, the extraction rate of a target extract is greatly improved, and the content of total saponins in a material can be over 95 percent.

Description

A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin
Technical field
The present invention relates to a kind of method for distilling of thick total Saponin, be specifically related to a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin.
Background technology
Saponin is to have botanic one type of relatively more complicated glycoside compound, and Saponin is made up of ruscogenin and sugared two parts, can be water-soluble, dissolve in ethanol, methanol, and be insoluble in ether or the benzene.The abstraction technique of Saponin commonly used has at present: the merceration of water or aqueous solvent extracts, adds extraction heat, ultrasonic extraction, supercritical collection etc.They have a common characteristic to be extracted plant and side-product thereof segmentation back and solvent exactly in a container after a period of time, and Saponin diffuses in the solvent.Conventional method for distilling is owing to adopt solvent through cell wall entering cell interior; Thing to be extracted dissolves into and brings out from cell interior through cell wall together behind the solvent again; The common disadvantage of this method for distilling is that energy consumption is high, the extraction time is long, the extracted products impurity content is high, the defecation rate target extract is lower, is difficult to reach more than 85%.
(patent No. is Chinese invention patent " the solvent-free method that adds the extraction heat Saponin of a kind of microwave ": 200410046954.2) disclose a kind of method of extracting Saponin; This method has adopted microwave exposure to contain plant tissue after the lower segmentation of moisture in leaching process; Intracellular matter expands rapidly cell wall is broken; Utilize high, the big principle of Saponin polarity, can make that Saponin is extracted out rapidly, reduced the extraction time and improved the purity of extract the microwave absorbtivity.But experiment test, this method only just have than obvious effects the lower dried plant raw material of water content, and for fresh plant material, effect is but also not obvious.Because the water content of fresh plant is high, cell wall elasticity is abundant, and how cellular content expands again, and cell wall also is difficult to burst.Therefore the target extract just can not discharge in cell, thereby can not fully contact with solvent, has influenced the extraction ratio and the extraction time of target extract greatly.
Summary of the invention
Said problem above the objective of the invention is to be directed against provides a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting slightly total Saponin, can improve the extraction ratio that from fresh Rhizoma Dioscoreae class plant, extracts thick total Saponin greatly and shorten extraction time.
The present invention is achieved through following technical scheme.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome is cut into lamellar or is ground into graininess, deposit then and treat its natural fermentation, as raw material.Fermentation time is 10-60 hours.
(2) raw material that ferments is carried out irradiation 10-480 seconds with microwave to it, when material temperature rises to 60 ℃ to 95 ℃, stop microwave exposure.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 40 order to 200 orders size.
(4) granule that obtains in the step 3 being immersed in concentration is in 65% to 95% the alcoholic solution 1-10 minutes, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 30-120 seconds, is immersed in concentration once more and is in 65% to 95% the alcoholic solution 1-10 minutes, leaches mixed solution then.
(6) process of repeating step 5 repeats 3 to 5 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the ethanol in the solution, promptly obtain needed thick total Saponin.
In order to reduce the waste of microwave exposure energy, step 2 can replace with: after the raw material that ferments is dewatered a little, use microwave that it was carried out irradiation 10-480 seconds, when material temperature rises to 60 ℃ to 95 ℃, stop microwave exposure.
Ethanol in the step 4 and 5 can use other organic solvents to replace.
Beneficial effect of the present invention is: compare with conventional method of extraction; The present invention has adopted and has carried out the method that secondary is pulverized behind the microwave exposure again, makes cellular content expand rapidly through microwave exposure, causes cell wall fully to expand thereupon; And then carry out secondary and pulverize; Just can cell wall integral body be cracked, cellular content all discharges, and fully contacts with solvent.So also just make extract to be dissolved in fully in the solvent, improved the extraction ratio of target extract greatly, can reach more than 95% of total saponin content in this material.
The specific embodiment
Further specify the present invention below in conjunction with embodiment.
embodiment one.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome 100g is ground into graininess, deposits then and treat its natural fermentation, as raw material.Fermentation time is 12 hours.
(2) raw material that ferments is inserted in the container, use microwave that it was carried out irradiation 40 seconds, material temperature rises to 60 ℃.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 40-100 order size.
(4) granule that obtains in the step 3 being immersed in concentration is in 65% the alcoholic solution 1 minute, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 30 seconds, is immersed in concentration once more and is in 65% the alcoholic solution 1 minute, leaches mixed solution then.
(6) process of repeating step 5 repeats 3 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the ethanol in the solution, promptly obtain needed thick total Saponin.
embodiment 2.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome 150g is cut into lamellar, deposits then and treat its natural fermentation, as raw material.Fermentation time is 24 hours.
(2) raw material that ferments is dewatered a little after, insert in the container, use microwave that it was carried out irradiation 90 seconds, material temperature rises to 90 ℃.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 60-120 order size.
(4) granule that obtains in the step 3 being immersed in concentration is in 95% the alcoholic solution 3 minutes, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 70 seconds, is immersed in concentration once more and is in 85% the alcoholic solution 3 minutes, leaches mixed solution then.
(6) process of repeating step 5 repeats 3 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the ethanol in the solution, promptly obtain needed thick total Saponin.
embodiment 3.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome 300g is cut into lamellar or is ground into graininess, deposit then and treat its natural fermentation, as raw material.Fermentation time is 36 hours.
(2) raw material that ferments is inserted in the container, use microwave that it was carried out irradiation 150 seconds, when material temperature rises to 85 ℃, stop microwave exposure.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 140 orders size.
(4) granule that obtains in the step 3 being immersed in concentration is in 90% the methanol solution 5 minutes, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 80 seconds, is immersed in concentration once more and is in 75% the methanol solution 5 minutes, leaches mixed solution then.
(6) process of repeating step 5 repeats 4 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the alcohol in the solution, promptly obtain needed thick total Saponin.
embodiment 4.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome 300g is cut into lamellar or is ground into graininess, deposit then and treat its natural fermentation, as raw material.Fermentation time is 48 hours.
(2) raw material that ferments is dewatered a little after, insert in the container, use microwave that it was carried out irradiation 200 seconds, when material temperature rises to 93 ℃, stop microwave exposure.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 200 orders size.
(4) granule that obtains in the step 3 being immersed in concentration is in 85% the butanol solution 7 minutes, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 100 seconds, is immersed in concentration once more and is in 80% the butanol solution 7 minutes, leaches mixed solution then.
(6) process of repeating step 5 repeats 4 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the n-butyl alcohol in the solution, promptly obtain needed thick total Saponin.
embodiment 5.
A kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin comprises the steps.
(1) fresh Rhizoma Dioscoreae class plant rhizome 1Kg is cut into lamellar or is ground into graininess, deposit then and treat its natural fermentation, as raw material.Fermentation time is 60 hours.
(2) raw material that ferments is inserted in the container, use microwave that it was carried out irradiation 480 seconds, and intermittently stir, when material temperature rises to 95 ℃, stop microwave exposure.
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 200 orders size.
(4) granule that obtains in the step 3 being immersed in concentration is in 90% the alcoholic solution 10 minutes, leaches mixed solution then.
(5) remaining filtering residue is through microwave radiation after 120 seconds, is immersed in concentration once more and is in 95% the alcoholic solution 10 minutes, leaches mixed solution then.
(6) process of repeating step 5 repeats 5 times.
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the ethanol in the solution, promptly obtain needed thick total Saponin.

Claims (5)

1. a method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin is characterized in that: comprise the steps:
(1) fresh Rhizoma Dioscoreae class plant rhizome is cut into lamellar or is ground into graininess, deposit then and treat its natural fermentation, as raw material;
(2) raw material that ferments is carried out irradiation with microwave to it, when material temperature rises to 60 ℃ to 95 ℃, stop microwave exposure;
(3) raw material behind the microwave exposure is further pulverized, be ground into the granule of 40 order to 200 orders size;
(4) granule that obtains in the step 3 being immersed in concentration is in 65% to 95% the alcoholic solution 1-10 minutes, leaches mixed solution then;
(5) remaining filtering residue is immersed in concentration and is in 65% to 95% the alcoholic solution 1-10 minutes once more behind microwave radiation, leach mixed solution then;
(6) process of repeating step 5 repeats 3 to 5 times;
(7) merge the solution that multiple times of filtration obtains, and after reclaiming the ethanol in the solution, promptly obtain needed thick total Saponin.
2. a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin according to claim 1; It is characterized in that: step 2 can replace with: after the raw material that ferments is dewatered a little; With microwave it is carried out irradiation; And intermittently stir, when material temperature rises to 60 ℃ to 90 ℃, stop microwave exposure.
3. a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin according to claim 1 and 2, it is characterized in that: the fermentation time described in the step 1 is 12-60 hours.
4. a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin according to claim 1, it is characterized in that: the time of the microwave exposure described in the step 2 is 40-480 seconds, the time of the microwave exposure described in the step 5 is 30-120 seconds.
5. a kind of method of from fresh Rhizoma Dioscoreae class plant, extracting thick total Saponin according to claim 1 is characterized in that: the ethanol in the step 4 and 5 can use other organic solvents to replace.
CN 201010585911 2010-12-14 2010-12-14 Extraction method of raw total saponins from fresh dioscorea plants Expired - Fee Related CN102335316B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106831933A (en) * 2017-01-22 2017-06-13 嵊州市派特普科技开发有限公司 The method that thick Total saponin is extracted from Chinese yam class plant
CN112021441A (en) * 2020-08-21 2020-12-04 湖南汇富康达健康管理研究院 Low-GI (glycemic index) full-nutrition bar and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1778811A (en) * 2004-11-22 2006-05-31 王煊 Extraction of saponin by non-solvent microwave heat
CN101012474A (en) * 2007-02-05 2007-08-08 大连理工大学 Method for preparing Chinese yam saponin by microorganism transformation process
CN101885750A (en) * 2010-03-08 2010-11-17 李绍通 Method for circularly processing and utilizing rhizome in dioscorea

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1778811A (en) * 2004-11-22 2006-05-31 王煊 Extraction of saponin by non-solvent microwave heat
CN101012474A (en) * 2007-02-05 2007-08-08 大连理工大学 Method for preparing Chinese yam saponin by microorganism transformation process
CN101885750A (en) * 2010-03-08 2010-11-17 李绍通 Method for circularly processing and utilizing rhizome in dioscorea

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106831933A (en) * 2017-01-22 2017-06-13 嵊州市派特普科技开发有限公司 The method that thick Total saponin is extracted from Chinese yam class plant
CN112021441A (en) * 2020-08-21 2020-12-04 湖南汇富康达健康管理研究院 Low-GI (glycemic index) full-nutrition bar and preparation method thereof

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