CN108148107A - The method for extraction and purification of Dioscin - Google Patents
The method for extraction and purification of Dioscin Download PDFInfo
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- CN108148107A CN108148107A CN201711418678.1A CN201711418678A CN108148107A CN 108148107 A CN108148107 A CN 108148107A CN 201711418678 A CN201711418678 A CN 201711418678A CN 108148107 A CN108148107 A CN 108148107A
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- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
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Abstract
The invention discloses a kind of method for extraction and purification of Dioscin, include the following steps：By the mixture of Dioscoreaceae plant roots and stems powder and organic solvent, filtering obtains Dioscin extracting solution after repeatedly cycle extraction process, wherein, each extraction process includes the microwave treatment carried out successively and circumfluence method processing；And obtain Dioscin after Dioscin extracting solution is purified.The technical operation of the method for the present invention is simple, largely reduces the dosage of organic solvent, and the process time shortens more than 50%, and without using soda acid, primary organic solvent with recycling, can greatly reduce the yield of " three wastes " after industrialized production.
Description
Technical field
The present invention relates to biomedicine technical field, more particularly to a kind of method for extraction and purification of Dioscin.
Background technology
Dioscin (Dioscin) is by the diosgenin of spirostan type and a sugar chain being connected on 3 hydroxyls
It is connected with glycosidic bond and is formed, is a kind of typical active natural soap glycosides compound, is present in Dioscoreaceae, Liliaceae, Caryophyllaceae
In the medicinal plants such as the rose family, the rich content especially in Dioscoreaceae plant, such as dioscorea nipponica, dioscorea zingiberensis wright and Dioscorea Panthcica
Deng.Traditional Chinese medicine thinks that Dioscin has the effects that eliminating the phlegm, relaxing tendons and activating collaterals, help digestion sharp water.Modern pharmacology research shows Chinese yam
Saponin(e also has the effects that desensitization, anti-inflammatory, lipid-loweringing, antitumor, liver protection, antiviral.It is readily soluble since Dioscin is connected with saccharide residue
In methanol, ethyl alcohol, acetic acid isopolarity solvent, the nonpolar solvents such as chloroform, petroleum ether, ether are not readily dissolved in, are slightly soluble in acetone, penta
Alcohol.The hydrolysate of Dioscin is diosgenin (diosgenin), has research to think, in human body, Dioscin takes orally
The diosgenin generated by intestinal flora metabolism is the active ingredient to play a role；With Dioscin after Dioscin hydrolysis
The form of member plays a role, and diosgenin can be used as synthesizing the raw material of a variety of steroid hormone class drugs, and application prospect is very
It is wide.
Existing Dioscin extracting method has ultrasonic extraction, reflux extraction and cold soaking extraction method etc., mainly uses
Methanol or Diluted Alcohol are as solvent.Such as：Ultrasonic extraction：To in the extraction of Dioscin in Dioscorea Zingiberensis, using
80% ethyl alcohol is Extraction solvent, solid-liquid ratio 1: 25, the ultrasonic extraction 40min under conditions of 700W and 40kHz；Alcohol reflux carries
It follows the example of：The Dioscin in Dioscoreaceae plant roots and stems is extracted with ethanol refluxing process, extraction conditions are with 6 times of 70% alcohol refluxs of amount
Extraction 3 times, each 2h；The purification process of Dioscin is using macroreticular resin, polyamide, neutral alumina and water saturation just more
Butanol etc. carries out enriching and purifying to herbal extract and obtains thick saponin(e, then through silica gel column chromatography, preparative liquid chromatography, high-speed counter-current
The technologies such as chromatography are detached, to obtain the higher Dioscin of purity.More than Dioscin extracts and purification process exists
The shortcomings that production time is long, organic solvent usage amount is larger.
Invention content
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of method for extraction and purification of Dioscin, with Dioscoreaceae plant roots and stems
For raw material, purify to obtain purity using ultramicro grinding, Microwave-Assisted Ethanol reflux, alcohol precipitation and reversed-phase silica gel column chromatography method and be higher than
98% Dioscin；To sum up, the technical operation of the method for the present invention is simple, largely reduces the dosage of organic solvent, process time
Shorten more than 50%, without using soda acid, primary organic solvent can be with recycling, after greatly reducing industrialized production
The yield of " three wastes ".
In order to realize these purposes and other advantages according to the present invention, a kind of extraction purification side of Dioscin is provided
Method includes the following steps：
The mixture I of Dioscoreaceae plant roots and stems powder and organic solvent is obtained into mixture II through repeatedly cycle extraction process,
Wherein, Dioscoreaceae plant roots and stems powder and the volume ratio of organic solvent mixing are 1 in the mixture:11-20, at any secondary extraction
Reason includes the microwave treatment carried out successively and circumfluence method processing；And
Dioscin sterling is obtained after the mixture II is purified.
Preferably, by the mixture I, filtering obtains mixture II after 4-5 times recycles extraction process.
Preferably, the actual conditions of the microwave treatment are：Microwave power is 300-500W, extraction time 10-
20min, 40-50 DEG C of Extracting temperature；The time of the circumfluence method is 30-60min, and temperature is 35-45 DEG C.
Preferably, the actual conditions of the microwave treatment are：Microwave power is 300-400W, extraction time 12-
15min, 48-50 DEG C of Extracting temperature；The time of the circumfluence method is 50-60min, and temperature is 40-45 DEG C.
Preferably, Dioscoreaceae plant roots and stems powder and organic solvent in Dioscoreaceae plant roots and stems powder and organic solvent mixed liquor
The volume ratio of mixing is 1:12-14.
Preferably, the purification is further comprising the steps of：
Medicinal extract is obtained after the Dioscin extracting solution is recovered under reduced pressure organic solvent；
Vacuum distillation processing obtains distillation after the deionized water dilution of 3-5 times of volume is added in into the medicinal extract；
After the distillation is precipitated at least 6h, discard supernatant liquid and obtain sediment, the sediment centrifugal treating is obtained
A centrifugation, by a centrifugation be dissolved in ethyl alcohol after centrifugal treating obtain secondary centrifuging precipitation and it is secondary on
Clear liquid；
Dioscin crude powder is obtained after secondary supernatant is dried under reduced pressure；
The Dioscin crude powder is obtained into eluent after the processing of reversed silica gel column chromatography；
The eluent is dried under reduced pressure acquisition Dioscin.
Preferably, the reversed filler of the reverse-phase chromatographic column in the reversed silica gel column chromatography is C18, grain size 75-
150 μm, it is 9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2 and 7: 2.5 that the mobile phase of gradient elution, which is followed successively by according to volume ratio:
N-butanol-methanol-water of 0.5 ratio mixing, elution flow rate 1.0-2.0mL/min retain the eluent of 20-30min.
Preferably, the temperature for being evaporated under reduced pressure processing is 45-50 DEG C, and pressure is -0.1~-0.2MPA.
Preferably, it is 85-90% ethyl alcohol or methanol that organic solvent, which is mass percentage,.
Preferably, the preparation method for wearing imperial powder is further comprising the steps of：
Dioscoreaceae plant roots and stems are cleaned, after epidermis air-dries, it is spare；
It opens motor driving support shaft and drives multilayer drying net low speed rotation；
Dioscoreaceae plant roots and stems are delivered to through feed hopper after a pair of of compression roller pulverizes processing, fall into the multilayer of low speed rotation
Drying is dried to water content≤6% step by step on the net, and the specific steps dried step by step include：
Open heating pressure fan by the temperature of Dioscoreaceae plant roots and stems in 30-50min uniform heating to permanent after 80-82 DEG C
Temperature
Drying and processing 30-50min；Constant temperature drying handles 40- after Dioscoreaceae plant roots and stems are warming up to 84-86 DEG C again
60min；
Constant temperature drying to water content is less than 6% after Dioscoreaceae plant roots and stems are warming up to 88-90 DEG C again；
Drying gas is passed through in the ethyl alcohol in lautertuns and filtered simultaneously by drying step by step, it is to be dried terminate by ethyl alcohol remove with
Dioscin is obtained after the mixing purification of Dioscin extracting solution；
A pair of of telescopic rod of startup trails and the bristle of the brush body is driven to contradict to stop after multilayer drying is online
Only, it is again turned on the circle of motor low speed rotation at least 5 later, the Dioscoreaceae plant roots and stems after drying step by step are swept with bristle drops down onto receipts
Collect slot, then the discharge port discharging through collecting tank；
The Dioscoreaceae plant roots and stems that discharging goes out after the drying step by step of barrel-shaped casing are ground into the superfine of 300-500 mesh
Dioscoreaceae plant roots and stems powder；
Wherein, drying unit is pulverized to include：
Barrel-shaped casing, interior the first accommodating space and the second accommodating sky that the setting that is arranged above and below is divided by horizontal baffle
Between；
Rotary furnace drying component including motor, is arranged on the middle part of the horizontal baffle；Support shaft, with motor
Drive shaft is coaxially disposed, and the support shaft is set after the horizontal baffle along the axially extending of the second accommodating space
It puts；Multilayer dries net, is spaced apart and is arranged in the support shaft, and from up to down successively in concentric circles, multilayer drying net
Diameter gradually increase；Pressure fan is heated, is arranged on the lower section of the rotary furnace drying component；Air outlet is arranged on described
The side wall of barrel-shaped casing or top；Lautertuns is connected to by delivery pipe at air outlet, and matter is filled in the lautertuns
The ethyl alcohol that percentage composition is more than 70% is measured, one end of the delivery pipe is stretched in ethyl alcohol, and the upper end of the lautertuns is provide with
Venetian blind type cover；
A pair of of compression roller is arranged on the horizontal baffle, and the pair of compression roller is along the half of the horizontal baffle
Diameter direction is extended；Feed hopper is arranged on the upper end of the barrel-shaped casing, and the lower ending opening of the feed hopper is connected to
Face a pair of compression roller is set after first accommodating space of barrel-shaped casing；
Discharge component, it is telescopic to be arranged on the lower surface of the horizontal baffle including a pair of of telescopic rod, and one
Telescopic rod relatively short in telescopic rod is set close to the support shaft；Brush body, connection are arranged under a pair of of telescopic rod
End, the brush body are in staged multi-link structure, are provided with continuous bristle on the lower face of multi link, and the brush body
The quantity of multi link and multilayer drying net quantity be adapted, in staged multi-link structure the drop of two neighboring connecting rod and its
The drop of the two neighboring drying net of underface is adapted；Wherein, the collapsing length of a pair of of telescopic rod and the bristle with it just
The distance of the multilayer drying net of lower section is adapted；Material collecting tank is the annular for the periphery for being circumferentially positioned at the heating pressure fan
Accommodating groove, and the annular diameters of the material collecting tank are less than the diameter of the drying net of relative maximum in multilayer drying net, it is described to gather materials
The outer annular diameter of slot and the interior diameter of barrel-shaped casing are adapted, and the bottom of the material collecting tank is set from a lateral opposite side inclination
It puts, the barrel-shaped casing is extended in the bottom of the relatively low material collecting tank by discharge port；
Temperature sensor and humidity sensor are arranged in second accommodating space；And
Temperature and humidity controller is arranged on the side wall of the barrel-shaped casing, and the Temperature and Humidity Control its pass with temperature
Sensor and humidity sensor electrical connection.
The present invention includes at least following advantageous effect：
(1) Dioscoreaceae plant roots and stems are subjected to ultramicro grinding processing, relative to the prior art, avoid the pre- place of soda acid
Reason；
(2) it is handled in repeatedly cycle extraction process using microwave auxiliary reflux method, makes active ingredient in raw material more abundant
It is more easily extracted, expends quantity of solvent is only single circumfluence method extraction 1/5, required time is carried for single circumfluence method
1/10 taken has the characteristics that extracting method quick, efficient, energy saving；
(3) Dioscin crude product is obtained using alcohol precipitation, the Dioscin made full use of is soluble in the poles such as methanol, ethyl alcohol, acetic acid
Property solvent, is insoluble in the physical characteristic of water, avoids the use of soda acid；
(4) reversed-phase silica gel column chromatography method purifies, and reduces the dosage of organic solvent, improves the purity of Dioscin.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Description of the drawings
Fig. 1 is the process flow chart of the method for extraction and purification of the Dioscin described in one embodiment of the present of invention；
Fig. 2 is the cross-sectional view for pulverizing drying unit described in one embodiment of the present of invention.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, to enable those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein are not precluded one or more
The presence or addition of a other element or combinations.
As shown in Figure 1, the present invention provides a kind of method for extraction and purification of Dioscin, include the following steps：
The mixture I of Dioscoreaceae plant roots and stems powder and organic solvent is obtained into mixture II through repeatedly cycle extraction process,
Wherein, Dioscoreaceae plant roots and stems powder and the volume ratio of organic solvent mixing are 1 in the mixture:11-20, at any secondary extraction
Reason includes the microwave treatment carried out successively and circumfluence method processing；And
Dioscin sterling is obtained after the mixture II is purified.
In one preferred embodiment, by the mixture I, filtering obtains mixture II after 4-5 times recycles extraction process.
In one preferred embodiment, the actual conditions of the microwave treatment are：Microwave power is 300-500W, and extraction time is
10-20min, 40-50 DEG C of Extracting temperature；The time of the circumfluence method is 30-60min, and temperature is 35-45 DEG C.
In one preferred embodiment, the actual conditions of the microwave treatment are：Microwave power is 300-400W, and extraction time is
12-15min, 48-50 DEG C of Extracting temperature；The time of the circumfluence method is 50-60min, and temperature is 40-45 DEG C.
Dioscoreaceae plant roots and stems powder and have in one preferred embodiment, in Dioscoreaceae plant roots and stems powder and organic solvent mixed liquor
The volume ratio of solvent mixing is 1:12-14.
In one preferred embodiment, the purification is further comprising the steps of：
Medicinal extract is obtained after the Dioscin extracting solution is recovered under reduced pressure organic solvent；
Vacuum distillation processing obtains distillation after the deionized water dilution of 3-5 times of volume is added in into the medicinal extract；
After the distillation is precipitated at least 6h, discard supernatant liquid and obtain sediment, the sediment centrifugal treating is obtained
A centrifugation, by a centrifugation be dissolved in ethyl alcohol after centrifugal treating obtain secondary centrifuging precipitation and it is secondary on
Clear liquid；
Dioscin crude powder is obtained after secondary supernatant is dried under reduced pressure；
The Dioscin crude powder is obtained into eluent after the processing of reversed silica gel column chromatography；
The eluent is dried under reduced pressure acquisition Dioscin.
Preferably, the reversed filler of the reverse-phase chromatographic column in the reversed silica gel column chromatography is C18, grain size 75-
150 μm, it is 9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2 and 7: 2.5 that the mobile phase of gradient elution, which is followed successively by according to volume ratio:
N-butanol-methanol-water of 0.5 ratio mixing, elution flow rate 1.0-2.0mL/min retain the eluent of 20-30min.
In one preferred embodiment, the temperature for being evaporated under reduced pressure processing is 45-50 DEG C, and pressure is -0.1~-0.2MPA.
In one preferred embodiment, organic solvent is that mass percentage is 85-90% ethyl alcohol or methanol.
In one preferred embodiment, the preparation method for wearing imperial powder is further comprising the steps of：
Dioscoreaceae plant roots and stems are cleaned, after epidermis air-dries, it is spare；
It opens motor driving support shaft and drives multilayer drying net low speed rotation；
Dioscoreaceae plant roots and stems are delivered to through feed hopper after a pair of of compression roller pulverizes processing, fall into the multilayer of low speed rotation
Drying is dried to water content≤6% step by step on the net, and the specific steps dried step by step include：
Open heating pressure fan by the temperature of Dioscoreaceae plant roots and stems in 30-50min uniform heating to permanent after 80-82 DEG C
Warm drying and processing 30-50min；Constant temperature drying handles 40-60min after Dioscoreaceae plant roots and stems are warming up to 84-86 DEG C again；
Constant temperature drying to water content is less than 6% after Dioscoreaceae plant roots and stems are warming up to 88-90 DEG C again；
Dioscoreaceae plant roots and stems are pulverized into processing, can extrude out large quantity of moisture therein, and will not excessively damage Chinese yam
The epidermis of section's plant roots and stems, it is as much as possible to retain Dioscin not soluble in water；
Drying and processing step by step, and slowly at the uniform velocity heating treatment early period, it is ensured that moisture gradually dissipates in Dioscoreaceae plant roots and stems
Mistake comes out, and does not interfere with the compactness of the institutional framework in Dioscoreaceae plant roots and stems, avoids further loss Dioscin, and then
Retain the Dioscin in Dioscoreaceae plant roots and stems to greatest extent；
Drying gas is passed through in the ethyl alcohol in lautertuns and filtered simultaneously by drying step by step, it is to be dried terminate by ethyl alcohol remove with
Dioscin is obtained after the mixing purification of Dioscin extracting solution；It, will be where it is possible to taking out of after drying gas is filtered by ethyl alcohol
Dioscin is separated, and improves the final recovery rate of Dioscin；
A pair of of telescopic rod of startup trails and the bristle of the brush body is driven to contradict to stop after multilayer drying is online
Only, it is again turned on the circle of motor low speed rotation at least 5 later, the Dioscoreaceae plant roots and stems after drying step by step are swept with bristle drops down onto receipts
Collect slot, then the discharge port discharging through collecting tank；
The Dioscoreaceae plant roots and stems that discharging goes out after the drying step by step of barrel-shaped casing are ground into the superfine of 300-500 mesh
Dioscoreaceae plant roots and stems powder；
Wherein, include as shown in Fig. 2, pulverizing drying unit：
Barrel-shaped casing 10, it is interior the first accommodating space 11 and second of the setting that is arranged above and below to be divided into hold by horizontal baffle 13
12 between emptying；
Rotary furnace drying component 20 including motor 21, is arranged on the middle part of the horizontal baffle；Support shaft 22, with
The drive shaft coaxial arrangement of motor, and the support shaft is prolonged after the horizontal baffle along the axial direction of second accommodating space
Stretch setting；Multilayer dries net 23, is spaced apart and is arranged in the support shaft, and from up to down successively in concentric circles, multilayer
The diameter of drying net gradually increases；Pressure fan 24 is heated, is arranged on the lower section of the rotary furnace drying component；Air outlet 25,
It is arranged on side wall or the top of the barrel-shaped casing；Lautertuns 26 is connected to by delivery pipe 261 at air outlet, and described
Filled with the ethyl alcohol that mass percentage is more than 70% in lautertuns, one end of the delivery pipe is stretched in ethyl alcohol, described
The upper end of lautertuns is provide with venetian blind type cover 262；
A pair of of compression roller 30, is arranged on the horizontal baffle, and the pair of compression roller is along the horizontal baffle
Radial direction is extended；Feed hopper 40 is arranged on the upper end of the barrel-shaped casing, and the lower ending opening of the feed hopper connects
Face a pair of compression roller is set after passing to the first accommodating space of barrel-shaped casing；The bottom of feed hopper is non-woven fabrics material, so as to
Stop that drying gas is open blowout since then as possible when Dioscoreaceae plant roots and stems are added；After the completion of adding Dioscoreaceae plant roots and stems,
Feed hopper is closed；
Discharge component 50, it is telescopic to be arranged on the lower surface of the horizontal baffle including a pair of of telescopic rod 51,
And relatively short telescopic rod is set close to the support shaft in a pair of of telescopic rod；Brush body 52, connection are arranged on a pair of flexible
The lower end of bar, the brush body are in staged multi-link structure, and continuous bristle 521 is provided on the lower face of multi link, and
The quantity of the multi link of the brush body and the quantity of multilayer drying net are adapted, two neighboring connecting rod in staged multi-link structure
The drop of drop and the two neighboring drying net immediately below it be adapted；Wherein, the collapsing length of a pair of of telescopic rod with it is described
The distance of bristle and the multilayer drying net immediately below it is adapted；Material collecting tank 53, to be circumferentially positioned at the heating pressure fan
Periphery ring-shaped accommodating slot, and the annular diameters of the material collecting tank be less than multilayer drying net in relative maximum drying net it is straight
Diameter, the outer annular diameter of the material collecting tank and the interior diameter of barrel-shaped casing are adapted, and the bottom of the material collecting tank from side 531 to
Opposite side 532 is obliquely installed, and the barrel-shaped casing is extended in the bottom of the relatively low material collecting tank by discharge port 533；
In practical applications, long-term heat treatment in barrel-shaped casing, the material of bristle can select heat safe palm flabellum or nylon
Material, in addition to bristle, the material of other structures is stainless steel or alloy material in barrel-shaped casing；
Temperature sensor 60 and humidity sensor 70 are arranged in second accommodating space；And
Temperature and humidity controller 80 is arranged on the side wall of the barrel-shaped casing, and the Temperature and Humidity Control itself and temperature
Sensor and humidity sensor electrical connection.Make a reservation for drying temperature step by step, and according to Temperature and Humidity data through temperature and humidity controller
Carry out drying temperature and the adjustment of time；In addition, a pair of of compression roller is driven by squeezing roller motor, a pair of of telescopic rod can be electricity
Dynamic telescopic rod or Pneumatic extension bar, above each electric and pneumatic device including heating pressure fan are also electrically connected with control panel
It connects, to be uniformly controlled.
Embodiment 1
1.1 ultramicro grinding：Rhizoma dioscoreae nipponicae 1kg is taken, drying unit pulverizes and 80-90 DEG C is dried to water content and is step by step through pulverizing
6%, after ultramicro grinding, powder crosses 300 mesh sieve, obtains ultra-micro powder；The condition dried step by step is followed successively by Dioscoreaceae plant roots
The temperature of stem uniform heating to constant temperature drying after 80 DEG C in 40min handles 50min；Dioscoreaceae plant roots and stems are warming up to 84 again
Constant temperature drying handles 40min after DEG C；Constant temperature drying to water content is 6% after Dioscoreaceae plant roots and stems are warming up to 90 DEG C again；
1.2 Microwave-Assisted Ethanol refluxing extraction Dioscins：Take the ultra-micro powder in 1.1, solid-liquid ratio 1:12, ethyl alcohol is dense
It is 90% to spend, microwave power 300W, extraction time 12min, 50 DEG C of Extracting temperature, is extracted 5 times, and flow back 60min every time, is returned
Flow temperature 45 C；
1.3 alcohol precipitations obtain Dioscin crude product：50 DEG C, pressure soaked for vacuum distillation recycling organic solvent under -0.1MPA
Cream after adding in the deionized water dilution vacuum distillation of 3 times of volumes, staticly settles 6h；It is centrifuged after discarding supernatant liquid, takes precipitation, used
Ethyl alcohol, which will precipitate, to be dissolved, and supernatant is gone to obtain Dioscin crude powder after being dried under reduced pressure after centrifugation；
1.4 reversed-phase silica gel column chromatography methods purify：Dioscin crude powder, into inverted silica gel column chromatography (C18, grain size
75 μ μm), it is washed with n-butanol-methanol-water system (9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2,7: 2.5: 0.5) gradient
It takes off, flow velocity 1.0-2.0mL/min, retains the eluent of 20-30min；
After eluent vacuum distillation drying, using efficient liquid phase chromatographic analysis, the purity of Dioscin sterling is
98.7%.The recovery rate for wearing the Dioscin in Longshan is 70%.
Embodiment 2
1.1 ultramicro grinding：Plate brick Chinese yam 1kg (herein just according to your suggestion) is taken, is pulverized simultaneously through pulverizing drying unit
It is 5% that 80-90 DEG C is dried to water content step by step, and after ultramicro grinding, powder crosses 300 mesh sieve, obtains ultra-micro powder；It dries step by step
Condition be followed successively by by the temperature of Dioscoreaceae plant roots and stems in 30min uniform heating to after 82 DEG C constant temperature drying handle 40min；It will
Constant temperature drying handles 60min after Dioscoreaceae plant roots and stems are warming up to 86 DEG C again；After Dioscoreaceae plant roots and stems are warming up to 88 DEG C again
Constant temperature drying to water content is 5%；
1.2 Microwave-Assisted Ethanol refluxing extraction Dioscins：Take the ultra-micro powder in 1.1, solid-liquid ratio 1:14, ethyl alcohol is dense
It is 85% to spend, microwave power 400W, extraction time 15min, 45 DEG C of Extracting temperature, is extracted 4 times, and flow back 45min every time, is returned
Flow 35 DEG C of temperature；
1.3 alcohol precipitations obtain Dioscin crude product：48 DEG C, pressure is that organic solvent is recovered under reduced pressure under -0.2MPA to obtain medicinal extract, is added
After the deionized water dilution vacuum distillation for entering 4 times of volumes, 7h is staticly settled；It is centrifuged after discarding supernatant liquid, takes precipitation, it will with ethyl alcohol
Precipitation dissolving goes supernatant to obtain Dioscin crude powder after being dried under reduced pressure after centrifugation；
1.4 reversed-phase silica gel column chromatography methods purify：Dioscin crude powder, into inverted silica gel column chromatography (C18, grain size
75 μ μm), it is washed with n-butanol-methanol-water system (9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2,7: 2.5: 0.5) gradient
It takes off, flow velocity 1.0-2.0mL/min, retains the eluent of 20-30min；
After eluent vacuum distillation drying, using efficient liquid phase chromatographic analysis, the purity of Dioscin sterling is
98.5%, the recovery rate of the Dioscin of plate brick Chinese yam is 68%.
Embodiment 3
1.1 ultramicro grinding：Willow leaf Chinese yam 1kg is taken, drying unit pulverizes and 80-90 DEG C is dried to water content step by step through pulverizing
It is 4%, after ultramicro grinding, powder crosses 300 mesh sieve, obtains ultra-micro powder；The condition dried step by step is followed successively by Dioscoreaceae plant
The temperature of rhizome uniform heating to constant temperature drying after 81 DEG C in 50min handles 30min；Dioscoreaceae plant roots and stems are warming up to again
Constant temperature drying handles 50min after 85 DEG C；Constant temperature drying to water content is less than after Dioscoreaceae plant roots and stems are warming up to 89 DEG C again
4%；
1.2 Microwave-Assisted Ethanol refluxing extraction Dioscins：Take the ultra-micro powder in 1.1, solid-liquid ratio 1:12, ethyl alcohol is dense
It is 90% to spend, microwave power 300W, extraction time 20min, 40 DEG C of Extracting temperature, is extracted 5 times, and flow back 30min every time, is returned
Flow 40 DEG C of temperature；
1.3 alcohol precipitations obtain Dioscin crude product：45 DEG C, pressure is that organic solvent is recovered under reduced pressure under -0.2MPA to obtain medicinal extract, is added
After the deionized water dilution vacuum distillation for entering 5 times of volumes, 8h is staticly settled；It is centrifuged after discarding supernatant liquid, takes precipitation, it will with ethyl alcohol
Precipitation dissolving goes supernatant to obtain Dioscin crude powder after being dried under reduced pressure after centrifugation；
1.4 reversed-phase silica gel column chromatography methods purify：Dioscin crude powder, into inverted silica gel column chromatography (C18, grain size
75 μ μm), it is washed with n-butanol-methanol-water system (9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2,7: 2.5: 0.5) gradient
It takes off, flow velocity 1.0-2.0mL/min, retains the eluent of 20-30min；
After eluent vacuum distillation drying, using efficient liquid phase chromatographic analysis, the purity of Dioscin sterling is
98.4%, the recovery rate of the Dioscin of willow leaf Chinese yam is 67%.
Wherein, the Dioscin crude powder yield that Microwave-Assisted Ethanol reflow method in embodiment 1 obtains with it is existing
Single alcohol extraction procedure or ultrasonic wave added alcohol reflux method compare, comparison result see the table below 1：
Wherein, the weight and mesh number of the extraction raw material used in alcohol extraction procedure or ultrasonic wave added alcohol reflux method
Same as Example 1, the actual conditions of alcohol extraction procedure are：95% ethyl alcohol, solid-liquid ratio 1:10,50 DEG C of Extracting temperature,
Extraction 5 times, each 4-5h；It is in the actual conditions of ultrasonic wave added alcohol reflux method：95% ethyl alcohol, solid-liquid ratio 1:10, surpass
Sound 30-60min is extracted 3-4 times, each 2-3h.
Reversed silica gel column purification side in the equal Application Example 1 of Dioscin crude powder that more than extracting method obtains
Method, the final recovery rate of Dioscin see the table below 1.
Table 1
| Extraction conditions | Ethyl alcohol extracts | Ultrasonic wave added alcohol reflux | Embodiment 1 |
| Ethyl alcohol consumption (L/100g) | 5-10L | 4-5L | 1-2L |
| Extraction time (h) | 20.0-30.0 | 8.0-12.0 | 2.0-3.0 |
| Dioscin crude powder yield (g/100g) | 1.33±0.07 | 1.72±0.05 | 1.89±0.03 |
| The final recovery rate (%) of Dioscin | 35±9.4 | 50±6.9 | 70 |
By upper table 1 it is found that having following advantageous effect using the method for the present invention extraction purification Dioscin：
(1) Dioscoreaceae plant roots and stems are subjected to ultramicro grinding processing, relative to the prior art, avoid the pre- place of soda acid
Reason；
(2) it is handled in repeatedly cycle extraction process using microwave auxiliary reflux method, makes active ingredient in raw material more abundant
It is more easily extracted, expends quantity of solvent is only single circumfluence method extraction 1/5, required time is carried for single circumfluence method
1/10 taken has the characteristics that extracting method quick, efficient, energy saving；
(3) Dioscin crude product is obtained using alcohol precipitation, the Dioscin made full use of is soluble in the poles such as methanol, ethyl alcohol, acetic acid
Property solvent, is insoluble in the physical characteristic of water, avoids the use of soda acid；
(4) reversed-phase silica gel column chromatography method purifies, and reduces the dosage of organic solvent, improve Dioscin purity and
Recovery rate reduces the waste of raw material.
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore under the universal limited without departing substantially from specification and equivalency range, the present invention is not limited to
Specific details and legend shown and described herein.
Claims (10)
1. a kind of method for extraction and purification of Dioscin, which is characterized in that include the following steps：
The mixture I of Dioscoreaceae plant roots and stems powder and organic solvent is obtained into mixture II through repeatedly cycle extraction process, wherein,
Dioscoreaceae plant roots and stems powder and the volume ratio of organic solvent mixing are 1 in the mixture:11-20, any secondary extraction process packet
Include the microwave treatment carried out successively and circumfluence method processing；And
Dioscin sterling is obtained after the mixture II is purified.
2. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that by the mixture I through 4-5 times
Filtering obtains mixture II after recycling extraction process.
3. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that the specific item of the microwave treatment
Part is：Microwave power is 300-500W, extraction time 10-20min, 40-50 DEG C of Extracting temperature；The time of the circumfluence method is
30-60min, temperature are 35-45 DEG C.
4. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that the specific item of the microwave treatment
Part is：Microwave power is 300-400W, extraction time 12-15min, 48-50 DEG C of Extracting temperature；The time of the circumfluence method is
50-60min, temperature are 40-45 DEG C.
5. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that Dioscoreaceae plant roots and stems powder and have
Dioscoreaceae plant roots and stems powder and the volume ratio of organic solvent mixing are 1 in solvent mixed liquor:12-14.
6. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that the purification further includes following step
Suddenly：
Medicinal extract is obtained after the Dioscin extracting solution is recovered under reduced pressure organic solvent；
Vacuum distillation processing obtains distillation after the deionized water dilution of 3-5 times of volume is added in into the medicinal extract；
It after the distillation is precipitated at least 6h, discards supernatant liquid and obtains sediment, the sediment centrifugal treating is obtained one
Secondary centrifugation, centrifugal treating obtains secondary centrifuging precipitation and secondary supernatant after a centrifugation is dissolved in ethyl alcohol
Liquid；
Dioscin crude powder is obtained after secondary supernatant is dried under reduced pressure；
The Dioscin crude powder is obtained into eluent after the processing of reversed silica gel column chromatography；
The eluent is dried under reduced pressure acquisition Dioscin.
7. the method for extraction and purification of Dioscin as claimed in claim 6, which is characterized in that the reversed silica gel column chromatography
In reverse-phase chromatographic column reversed filler for C18, grain size is 75-150 μm, and the mobile phase of gradient elution is followed successively by according to volume ratio
For n-butanol-methanol-water of 9: 0.9: 0.1,8: 1.8: 0.2,7: 2.8: 0.2 and 7: 2.5: 0.5 ratio mixing, elution stream
Speed is 1.0-2.0mL/min, retains the eluent of 20-30min.
8. the method for extraction and purification of Dioscin as claimed in claim 6, which is characterized in that the temperature for being evaporated under reduced pressure processing is
45-50 DEG C, pressure is -0.1~-0.2MPA.
9. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that organic solvent contains for quality percentage
It measures as 85-90% ethyl alcohol or methanol.
10. the method for extraction and purification of Dioscin as described in claim 1, which is characterized in that the preparation side for wearing imperial powder
Method is further comprising the steps of：
Dioscoreaceae plant roots and stems are cleaned, after epidermis air-dries, it is spare；
It opens motor driving support shaft and drives multilayer drying net low speed rotation；
Dioscoreaceae plant roots and stems are delivered to through feed hopper after a pair of of compression roller pulverizes processing, fall into the multilayer drying of low speed rotation
It is dried to water content≤6% step by step on the net, the specific steps dried step by step include：
Open heating pressure fan by the temperature of Dioscoreaceae plant roots and stems in 30-50min uniform heating to constant temperature after 80-82 DEG C
Drying and processing 30-50min；Constant temperature drying handles 40-60min after Dioscoreaceae plant roots and stems are warming up to 84-86 DEG C again；
Constant temperature drying to water content is less than 6% after Dioscoreaceae plant roots and stems are warming up to 88-90 DEG C again；
Drying gas is passed through in the ethyl alcohol in lautertuns filters simultaneously by drying step by step, to be dried to terminate ethyl alcohol removal and Chinese yam
Dioscin is obtained after saponin extract solution mixing purification；
A pair of of telescopic rod of startup trails and the bristle of the brush body is driven to contradict the stopping after multilayer drying is online, it
After be again turned on motor low speed rotation at least 5 circle, the Dioscoreaceae plant roots and stems after drying step by step are swept with bristle drops down onto collecting tank,
Discharge port discharging through collecting tank again；
The Dioscoreaceae plant roots and stems that discharging goes out after the drying step by step of barrel-shaped casing are ground into the Chinese yam of the superfine of 300-500 mesh
Section's plant roots and stems powder；
Wherein, drying unit is pulverized to include：
Barrel-shaped casing, interior the first accommodating space and the second accommodating space that the setting that is arranged above and below is divided by horizontal baffle；
Rotary furnace drying component including motor, is arranged on the middle part of the horizontal baffle；Support shaft, the driving with motor
Axis is coaxially disposed, and the support shaft after the horizontal baffle along the axially extending setting of second accommodating space；It is more
Layer drying net, in concentric circles is spaced apart and is arranged in the support shaft, and from up to down successively, the diameter of multilayer drying net
Gradually increase；Pressure fan is heated, is arranged on the lower section of the rotary furnace drying component；Air outlet is arranged on the barrel-shaped shell
The side wall of body or top；Lautertuns is connected to by delivery pipe at air outlet, and quality percentage is filled in the lautertuns
Content is more than 70% ethyl alcohol, and one end of the delivery pipe is stretched in ethyl alcohol, and the upper end of the lautertuns is provide with shutter
Formula cover；
A pair of of compression roller is arranged on the horizontal baffle, and radius side of the pair of compression roller along the horizontal baffle
To be extended；Feed hopper, is arranged on the upper end of the barrel-shaped casing, and the lower ending opening of the feed hopper be connected to it is barrel-shaped
Face a pair of compression roller is set after first accommodating space of housing；
Discharge component, it is telescopic to be arranged on the lower surface of the horizontal baffle including a pair of of telescopic rod, and a pair is stretched
Relatively short telescopic rod is set close to the support shaft in contracting bar；Brush body, connection are arranged on the lower end of a pair of of telescopic rod, institute
Brush body is stated in staged multi-link structure, continuous bristle is provided on the lower face of multi link, and the brush body connect more
The quantity of bar and multilayer drying net quantity be adapted, in staged multi-link structure the drop of two neighboring connecting rod with its just under
The drop of the two neighboring drying net of side is adapted；Wherein, the collapsing length of a pair of of telescopic rod and the bristle and its underface
Multilayer drying net distance be adapted；Material collecting tank is the ring-shaped accommodating for the periphery for being circumferentially positioned at the heating pressure fan
Slot, and the annular diameters of the material collecting tank are less than the diameter of the drying net of relative maximum in multilayer drying net, the material collecting tank
The interior diameter of outer annular diameter and barrel-shaped casing is adapted, and the bottom of the material collecting tank is obliquely installed from a lateral opposite side, phase
The barrel-shaped casing is extended by discharge port to the bottom of the relatively low material collecting tank；
Temperature sensor and humidity sensor are arranged in second accommodating space；And
Temperature and humidity controller is arranged on the side wall of the barrel-shaped casing, and the Temperature and Humidity Control itself and temperature sensor
It is electrically connected with humidity sensor.
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