CN102335316B - Extraction method of raw total saponins from fresh dioscorea plants - Google Patents
Extraction method of raw total saponins from fresh dioscorea plants Download PDFInfo
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- CN102335316B CN102335316B CN 201010585911 CN201010585911A CN102335316B CN 102335316 B CN102335316 B CN 102335316B CN 201010585911 CN201010585911 CN 201010585911 CN 201010585911 A CN201010585911 A CN 201010585911A CN 102335316 B CN102335316 B CN 102335316B
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- total saponin
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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
Technical field
The present invention relates to a kind of extracting method of thick total saponin, be specifically related to a kind of method of from fresh Chinese yam class plant, extracting thick total saponin.
Background technology
Saponin is the glycoside compound that exists a botanic class relatively more complicated, and saponin is made up of sapogenin and sugared two portions, can be water-soluble, dissolve in ethanol, methyl alcohol, and be insoluble in ether or the benzene.The abstraction technique of saponin commonly used has at present: the cold soaking of water or water-containing solvent extracts, adds extraction heat, ultrasonic extraction, overcritical collection etc.They have a common characteristic to be extracted plant and byproduct thereof segmentation back and solvent exactly in a container after for some time, and saponin diffuses in the solvent.Conventional extracting method enters cell interior because employing sees through cell walls with solvent, thing to be extracted dissolves into and brings out from cell interior through cell walls together behind the solvent again, the common disadvantage of this extracting method is that the defecation rate of energy consumption height, extraction time length, extracted products foreign matter content height, 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 walls is broken, utilize saponin polarity height, the principle big to the microwave absorbing amount, can make that saponin is extracted out rapidly, reduce the extraction time and improved the purity of extract.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 height of fresh plant, cell walls elasticity is abundant, and how entocyte expands again, and cell walls also is difficult to be bursting at the collision.Therefore the target extract just can not discharge in cell, thereby can not fully contact with solvent, has influenced extraction yield and the extraction time of target extract greatly.
Summary of the invention
The objective of the invention is at top described problem, a kind of method of extracting thick total saponin from fresh Chinese yam class plant is provided, can improve the extraction yield that from fresh Chinese yam class plant, extracts thick total saponin greatly and shorten extraction time.
The present invention is achieved by the following technical programs.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome is cut into sheet or is ground into particulate state, deposit then and treat its spontaneous 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 particle of 40 order to 200 order sizes.
(4) particle that obtains in the step 3 being immersed in concentration is in 65% to 95% the ethanolic soln 1-10 minutes, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 30-120 seconds, is immersed in concentration again and is in 65% to 95% the ethanolic soln 1-10 minutes, leaches mixing solutions then.
(6) process of repeating step 5 repeats 3 to 5 times.
(7) merge the solution that multiple times of filtration obtains, and behind the ethanol in the recovery solution, namely 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 replace with other organic solvents.
Beneficial effect of the present invention is: compare with traditional extracting method, the present invention has adopted and has carried out the method that secondary is pulverized behind the microwave exposure again, make entocyte expand rapidly through microwave exposure, cause cell walls fully to expand thereupon, and then carry out secondary and pulverize, just cell walls integral body can be cracked, entocyte all discharges, and fully contacts with solvent.So also just make extract to be dissolved in fully in the solvent, improved the extraction yield of target extract greatly, can reach more than 95% of total saponin content in this material.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment one.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome 100g is ground into particulate state, deposits then and treat its spontaneous 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 particle of 40-100 order size.
(4) particle that obtains in the step 3 being immersed in concentration is in 65% the ethanolic soln 1 minute, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 30 seconds, is immersed in concentration again and is in 65% the ethanolic soln 1 minute, leaches mixing solutions then.
(6) process of repeating step 5 repeats 3 times.
(7) merge the solution that multiple times of filtration obtains, and behind the ethanol in the recovery solution, namely obtain needed thick total saponin.
Embodiment 2.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome 150g is cut into sheet, deposits then and treat its spontaneous 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 particle of 60-120 order size.
(4) particle that obtains in the step 3 being immersed in concentration is in 95% the ethanolic soln 3 minutes, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 70 seconds, is immersed in concentration again and is in 85% the ethanolic soln 3 minutes, leaches mixing solutions then.
(6) process of repeating step 5 repeats 3 times.
(7) merge the solution that multiple times of filtration obtains, and behind the ethanol in the recovery solution, namely obtain needed thick total saponin.
Embodiment 3.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome 300g is cut into sheet or is ground into particulate state, deposit then and treat its spontaneous 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 particle of 140 order sizes.
(4) particle that obtains in the step 3 being immersed in concentration is in 90% the methanol solution 5 minutes, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 80 seconds, is immersed in concentration again and is in 75% the methanol solution 5 minutes, leaches mixing solutions then.
(6) process of repeating step 5 repeats 4 times.
(7) merge the solution that multiple times of filtration obtains, and behind the alcohol in the recovery solution, namely obtain needed thick total saponin.
Embodiment 4.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome 300g is cut into sheet or is ground into particulate state, deposit then and treat its spontaneous 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 particle of 200 order sizes.
(4) particle that obtains in the step 3 being immersed in concentration is in 85% the butanol solution 7 minutes, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 100 seconds, is immersed in concentration again and is in 80% the butanol solution 7 minutes, leaches mixing solutions then.
(6) process of repeating step 5 repeats 4 times.
(7) merge the solution that multiple times of filtration obtains, and behind the propyl carbinol in the recovery solution, namely obtain needed thick total saponin.
Embodiment 5.
A kind of method of extracting thick total saponin from fresh Chinese yam class plant comprises the steps.
(1) fresh Chinese yam class plant rhizome 1Kg is cut into sheet or is ground into particulate state, deposit then and treat its spontaneous 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 particle of 200 order sizes.
(4) particle that obtains in the step 3 being immersed in concentration is in 90% the ethanolic soln 10 minutes, leaches mixing solutions then.
(5) Sheng Xia filter residue is through microwave radiation after 120 seconds, is immersed in concentration again and is in 95% the ethanolic soln 10 minutes, leaches mixing solutions then.
(6) process of repeating step 5 repeats 5 times.
(7) merge the solution that multiple times of filtration obtains, and behind the ethanol in the recovery solution, namely obtain needed thick total saponin.
Claims (5)
1. a method of extracting thick total saponin from fresh Chinese yam class plant is characterized in that: comprise the steps:
(1) fresh Chinese yam class plant rhizome is cut into sheet or is ground into particulate state, deposit then and treat its spontaneous 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 particle of 40 order to 200 order sizes;
(4) particle that obtains in the step 3 being immersed in concentration is in 65% to 95% the ethanolic soln 1-10 minutes, leaches mixing solutions then;
(5) Sheng Xia filter residue is after microwave radiation, is immersed in concentration again and is in 65% to 95% the ethanolic soln 1-10 minutes, leaches mixing solutions then;
(6) process of repeating step 5 repeats 3 to 5 times;
(7) merge the solution that multiple times of filtration obtains, and behind the ethanol in the recovery solution, namely obtain needed thick total saponin.
2. a kind of method of from fresh Chinese yam 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 extracting thick total saponin from fresh Chinese yam class plant 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 Chinese yam 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 extracting thick total saponin from fresh Chinese yam class plant according to claim 1 is characterized in that: the ethanol in the step 4 and 5 can be with other organic solvents replacements.
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CN101012474B (en) * | 2007-02-05 | 2010-09-15 | 大连理工大学 | Method for preparing Chinese yam saponin by microorganism transformation process |
CN101885750B (en) * | 2010-03-08 | 2012-08-22 | 李绍通 | Method for circularly processing and utilizing rhizome in dioscorea |
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