CN103040901B - A kind of production method of balloonflower root general glycoside - Google Patents
A kind of production method of balloonflower root general glycoside Download PDFInfo
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- CN103040901B CN103040901B CN201210595584.2A CN201210595584A CN103040901B CN 103040901 B CN103040901 B CN 103040901B CN 201210595584 A CN201210595584 A CN 201210595584A CN 103040901 B CN103040901 B CN 103040901B
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Abstract
The present invention discloses a kind of production method of balloonflower root general glycoside, the method is: after raw material is pulverized, drop into from cast hopper, the rotation of extractor group main frame, material is slowly advanced backward from unit front end, the feed tube that simultaneously extracts solvent slave group end enters in extractor, flowed through mobile material forward end by tank rear end, solid-liquid two-phase material is fully contact in this reverse movement, thereby by extracts active ingredients in medicinal material out. The dregs of a decoction are forced to be pushed to slag notch and are discharged through discharging conveyer, and special Juice squeezer pushes the dregs of a decoction, and dregs of a decoction Shen residual liquor is extruded to medicinal material tissue, reduces dregs of a decoction Shen residual liquor content. Extraction efficiency is higher, extraction is more complete. The present invention selects macroporous absorbent resin binding silica gel column chromatography purification simultaneously, and separating effect is better. Can obtain the highest yield is 3%, and content is more than 92% balloonflower root general glycoside finished product.
Description
Technical field:
The invention belongs to natural organic chemistry field, relate to a kind of production method of balloonflower root general glycoside, particularly relate to one and utilize contraryStream extracts, the production method of macroporous absorbent resin coupling silica gel column chromatography separation and purification balloonflower root general glycoside.
Background technology:
Balloonflower root another name RADIX PLATYCODI, RADIX PLATYCODI, RADIX PLATYCODI, bitter stalk, southern balloonflower root, powder balloonflower root, baiyao, profit as, stalk grass, Lu Ru,Fang Tu, large medicine, burden flower root, small bell flower root, Dao Laji, four leaf vegetables roots, husky rape root, mountain small bell flower root, Buddhist monk Hua Gen,Buddhist monk's headdress flower root, Talinum crassifolium, from Campanulaceae Platycodon grandiflouorum Platycodon grandiflouorum (Platycodongrandiforus). Excavate root in spring, autumn,Remove cauline leaf and fibrous root, pulverize earth, scrape off cork, dry cut into serving pieces. Its chemical composition has platycodoside (platycodin)A, C, D[1], D2, D3, go celery glycosyl platycodoside (deapioplatycodin) D, D3,, 2-O-=acetyl group balloonflower rootSaponin (2-O-acetylplatycodin) D2,3-O-acetyl group platycodoside (3-O-acetylplaty-codin) D2, polygala root soapGlucoside (polyglalacin) D, D2,2-O-acetyl group polygalin (2-O-acetylpolygalacin) D, D2,3-O-acetyl groupPolygalin (3-O-acetylpolygalacin) D, D2, balloonflower root glucoside acid-A methyl esters (methylplatyconate-A), 2-O-firstBase balloonflower root glucoside acid-A methyl esters (methyl-2-O-methyplatyconate-A), balloonflower root glucoside acid-A lactone (platyconicacid-ALactone) [2], wherein principal component is platycodin D, Platycodin A C D is called again 2-O-acetyl group platycodin D, balloonflower root soapGlucoside C is called again 3-O-acetyl group platycodin D. Etc. various saponins.
Platycodoside has and eliminates the phlegm and antitussive effect, suppress gastric secretion and antiulcer action, antiinflammatory action and the promotion circulatory systemEffect. This year is more and more to the research of balloonflower root, the patent application that publication number is CN101084971, and it discloses oneThe preparation method of total saponins of platycodon grandiflorum, comprises the steps: that (1) get balloonflower root medicinal material in order, adds solvent, and solution is adjusted to alkalescenceAfter extract again, obtain extract; (2) macroporous type alkali anion exchange column on extract, first uses buck and pure water rinsing, punchingWashing lotion discards, then uses hydrous ethanol wash-out, and eluent is concentrated, obtains total saponins of platycodon grandiflorum. This technique final products purity is not high,Yield is general, and practical application effect is nothing like the effect of counter-flow extraction, the separation of macroporous absorbent resin coupling silica gel column chromatography.
Summary of the invention
The object of the invention is to provide a kind of production method of balloonflower root general glycoside; The object of the invention be also to provide a kind of convenient and swift,What raw material sources were abundant, extraction efficiency is high, separation and purification successful, DNA purity are high utilizes Continuous Countercurrent Extraction and macropore suctionThe production technology of attached resin concentration purifying balloonflower root general glycoside.
The present invention seeks to be achieved through the following technical solutions.
A production method for balloonflower root general glycoside, its step is as follows:
(1) will after balloonflower root pulverizing, add continuous countercurrent extracting tank ethanol water refluxing extraction;
(2) extracting liquid filtering that will process through (1), obtains balloonflower root general glycoside crude extract;
(3) gained balloonflower root general glycoside crude extract is concentrated, obtain the thick concentrate of balloonflower root general glycoside;
(4) the thick concentrate of gained balloonflower root general glycoside is diluted with water, and filters, obtain filtrate;
(5) by upper gained filtrate broad spectrum type macroporous resin adsorption post, adsorb the complete impurity that washes with water, then use the ethanol water of low powered posterior chamberSolution is washed impurity, then uses the ethanol water wash-out of the high number of degrees, obtains balloonflower root general glycoside eluent;
(6) gained eluent is condensed into cream, obtains balloonflower root general glycoside condensed cream;
(7) balloonflower root general glycoside condensed cream is mixed to silica gel, and by the mixture of mixing as for silicagel column top, through ethyl acetate and oilEther mixed liquor wash-out, obtains eluent;
(8) eluent is reclaimed to solvent after concentrate drying obtain balloonflower root general glycoside semi-finished product;
(9) balloonflower root general glycoside semi-finished product are dissolved with ethanol water, filter, reclaim ethanol, concentrated, place crystallize out, take outFilter to obtain balloonflower root general glycoside finished product.
In described step (1), balloonflower root is crossed 30～80 mesh sieves after pulverizing and is carried out ethanol water refluxing extraction again, extracts solvent and is50%～85% ethanol water.
In described step (1), the equipment of extraction is counter-flow extraction production line, comprises elevator, charging transmission, countercurrent extraction tankOrganize main frame 1, draw glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draw glassware 2, Juice squeezer 2, discharging transmission, centrePump, Pump for giving-out, temporary tank, heat exchanger, liquid flowing valve etc. The rear raw material that pulverizes and sieves is at the uniform velocity added by elevator charge door place,Extract pumps via Pump for giving-out continuously from flowing to temporary storage tank.
In described step (1), adverse current production line parameter is, elevator frequency 15～30Hz, and main frame 1 frequency 18～20Hz,Juice squeezer 1 frequency 45～50Hz, main frame 2 frequency 20～22Hz, Juice squeezer 2 frequency 40～45Hz, Pump for giving-out flow 0.5～2T/h,Charging 100～400kg/h.
In described step (4), the dilution water yield is 5 times of concentrate volume, filters to such an extent that impurity discards.
In described step (5), macroporous resin adsorption step adopts wet method dress post, retains liquid level, and filtrate, by adsorption column, is flowedSpeed 0.05ml/g resin per minute, resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous absorptionResin.
In described step (5), large pore resin absorption column ratio of height to diameter is 10～5: 1, and the ethanol water of low powered posterior chamber is 5%～20%Ethanol water, the ethanol water of the high number of degrees is 50%～80% ethanol water, washing the impurity water yield is 3～5BV, washes impurity lowThe ethanol water amount of the number of degrees is 1～2BV, and the ethanol water amount of the high number of degrees of wash-out is 4BV.
In described step (7), silica gel column chromatography step adopts wet method dress post, retains liquid level, and condensed cream is mixed to work by weight at 1: 1Silica gel after changing, and the mixture of mixing is placed in to silicagel column top, eluent is ethyl acetate: benzinum volume ratio is 50～85: 15Ethyl acetate and benzinum mixture, elution flow rate 0.1ml/g silica gel per minute, elution volume is 5BV. Silica gel activating barPart is, 110 DEG C of 30min.
In described step (9), 60 DEG C of thermosols of 12～16 times of amount 50% ethanol waters for balloonflower root general glycoside semi-finished product. Concentrated densityFor d=1.03～1.05.
The present invention discloses a kind of production method of balloonflower root general glycoside, and the method is: after raw material is pulverized, drop into from cast hopper, extractThe rotation of tank group main frame, slowly advances material backward from unit front end, and the feed tube that simultaneously extracts solvent slave group end entersEnter in extractor, flowed through mobile material forward end by tank rear end, solid-liquid two-phase material fills in this reverse movementDivide contact, thereby by extracts active ingredients in medicinal material out. The dregs of a decoction are forced to be pushed to slag notch and are discharged through discharging conveyer,Special Juice squeezer pushes the dregs of a decoction, and dregs of a decoction Shen residual liquor is extruded to medicinal material tissue, reduces dregs of a decoction Shen residual liquorContent. Extraction efficiency is higher, extraction is more complete.
The present invention selects macroporous absorbent resin binding silica gel column chromatography purification simultaneously, and separating effect is better.
Detailed description of the invention:
Embodiment 1:
Take balloonflower root 2T, after pulverizing, cross 40 mesh sieves, at the uniform velocity added 75% ethanol by elevator charge door with the speed of 400kg/hThe aqueous solution is added by feed tube with the flow of 2T/h with tubing pump, and elevator frequency setting is 30Hz, and main frame 1 frequency setting is20Hz, Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz,Obtain balloonflower root general glycoside crude extract 10T; Balloonflower root general glycoside crude extract is concentrated to concentration tank via Pump for giving-out continuous pump from flowing to temporary storage tank,The thick concentrate 600L of balloonflower root general glycoside; Gained concentrate is added to the dilution of 3T water, remove by filter impurity; Filtrate is crossed HPD400 macroporePolymeric adsorbent, resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T5% ethanol aqueous wash impurity, 8T80%Ethanol water wash-out, obtains balloonflower root general glycoside eluent 7.8T; Eluent concentrates to obtain balloonflower root general glycoside condensed cream 400kg; Balloonflower root general glycosideCondensed cream is mixed 400kg activated silica gel, is placed in silicagel column top, and eluent is ethyl acetate: benzinum volume ratio is 85: 15Ethyl acetate and benzinum mixture, elution flow rate 0.1ml/g silica gel per minute, obtains eluent 2000kg; Eluent reclaims moltenAfter agent, concentrate drying obtains balloonflower root general glycoside semi-finished product 120kg; 60 DEG C of thermosols of 1500L50% ethanol water for balloonflower root general glycoside semi-finished product,Filter, reclaim ethanol, be concentrated into d=1.05, place crystallize out, suction filtration obtains balloonflower root general glycoside finished product 40kg, content 92%.
Embodiment 2:
Take balloonflower root 800kg, after pulverizing, cross 60 mesh sieves, at the uniform velocity added 65% by elevator charge door with the speed of 200kg/hEthanol water is added by feed tube with the flow of 1T/h with tubing pump, and elevator frequency setting is 25Hz, and main frame 1 frequency is establishedBe decided to be 18Hz, Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz, obtains balloonflower root general glycoside crude extract 4T; Balloonflower root general glycoside crude extract is concentrated to concentration tank via Pump for giving-out continuous pump from flowing to temporary storage tank,Obtain the thick concentrate 250L of balloonflower root general glycoside; Gained concentrate is added to the dilution of 1.25T water, remove by filter impurity; It is large that filtrate is crossed AB-8Macroporous adsorbent resin, resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T20% ethanol aqueous wash impurity, 8T600%Ethanol water wash-out, obtains balloonflower root general glycoside eluent 7.8T; Eluent concentrates to obtain balloonflower root general glycoside condensed cream 150kg; Balloonflower root general glycosideCondensed cream is mixed 150kg activated silica gel, is placed in silicagel column top, and eluent is ethyl acetate: benzinum volume ratio is 65: 15Ethyl acetate and benzinum mixture, elution flow rate 0.1ml/g silica gel per minute, obtains eluent 750kg; Eluent reclaims solventRear concentrate drying obtains balloonflower root general glycoside semi-finished product 50kg; 60 DEG C of thermosols of 600L50% ethanol water for balloonflower root general glycoside semi-finished product, mistakeFilter, reclaims ethanol, is concentrated into d=1.04, places crystallize out, and suction filtration obtains balloonflower root general glycoside finished product 24kg, content 93%.
Embodiment 3:
Take balloonflower root 1.6T, after pulverizing, cross 80 mesh sieves, at the uniform velocity added 75% second by elevator charge door with the speed of 100kg/hAlcohol solution is added by feed tube with the flow of 500kg/h with tubing pump, and elevator frequency setting is 25Hz, and main frame 1 frequency is establishedBe decided to be 18Hz, Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz, obtains balloonflower root general glycoside crude extract 8T; Balloonflower root general glycoside crude extract is concentrated to concentration tank via Pump for giving-out continuous pump from flowing to temporary storage tank,Obtain the thick concentrate 500L of balloonflower root general glycoside; Gained concentrate is added to the dilution of 2.5T water, remove by filter impurity; Filtrate is crossed DM-130Macroporous absorbent resin, resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T15% ethanol aqueous wash impurity,8T70% ethanol water wash-out, obtains balloonflower root general glycoside eluent 7.8T; Eluent concentrates to obtain balloonflower root general glycoside condensed cream 310kg; TangerineStalk general glycoside condensed cream is mixed 310kg activated silica gel, is placed in silicagel column top, and eluent is ethyl acetate: benzinum volume ratio is 75: 15Ethyl acetate and benzinum mixture, elution flow rate 0.1ml/g silica gel per minute, obtains eluent 1.5T; Eluent reclaims moltenAfter agent, concentrate drying obtains balloonflower root general glycoside semi-finished product 110kg; 60 DEG C of thermosols of 1.6T50% ethanol water for balloonflower root general glycoside semi-finished product, filter, and reclaim ethanol, are concentrated into d=1.03, place crystallize out, and suction filtration obtains balloonflower root general glycoside finished product 38kg, content 94%.
Claims (9)
1. a production method for balloonflower root general glycoside, is characterized in that the method comprises the steps:
(1) will after balloonflower root pulverizing, add continuous countercurrent extracting tank ethanol water refluxing extraction;
(2) extracting liquid filtering that will process through (1), obtains balloonflower root general glycoside crude extract;
(3) gained balloonflower root general glycoside crude extract is concentrated, obtain the thick concentrate of balloonflower root general glycoside;
(4) the thick concentrate of gained balloonflower root general glycoside is diluted with water, and filters, obtain filtrate;
(5) by upper gained filtrate broad spectrum type macroporous resin adsorption post, adsorb the complete impurity that washes with water, then use the ethanol water of low powered posterior chamberSolution is washed impurity, then uses the ethanol water wash-out of the high number of degrees, obtains balloonflower root general glycoside eluent;
(6) gained eluent is condensed into cream, obtains balloonflower root general glycoside condensed cream;
(7) balloonflower root general glycoside condensed cream is mixed to silica gel, and by the mixture of mixing as for silicagel column top, through ethyl acetate and oilEther mixed liquor wash-out, obtains eluent;
(8) eluent is reclaimed to solvent after concentrate drying obtain balloonflower root general glycoside semi-finished product;
(9) balloonflower root general glycoside semi-finished product are dissolved with ethanol water, filter, reclaim ethanol, concentrated, place crystallize out, take outFilter to obtain balloonflower root general glycoside finished product.
2. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (1), and tangerineStalk is crossed 30～80 mesh sieves after pulverizing and is carried out ethanol water refluxing extraction again, the ethanol water that extraction solvent is 50%～85%.
3. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (1), carryThe equipment of getting is counter-flow extraction production line, comprises elevator, charging transmission, countercurrent extraction tank group main frame 1, draws glassware 1, squeezes juiceMachine 1, countercurrent extraction tank group main frame 2, draw glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary tank, changeHot device, liquid flowing valve, the rear raw material that pulverizes and sieves is at the uniform velocity added by elevator charge door place, and extract is from flowing to temporary tank via going outLiquid pump pumps continuously.
4. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (1), contraryFlowing production line parameter is, elevator frequency 15～30Hz, and main frame 1 frequency 18～20Hz, Juice squeezer 1 frequency 45～50Hz, mainMachine 2 frequency 20～22Hz, Juice squeezer 2 frequency 40～45Hz, Pump for giving-out flow 0.5～2T/h, charging 100～400kg/h.
5. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (4), rareRelease the water yield and be concentrate volume 5 times, filter to such an extent that impurity discards.
6. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (5), largeHole resin adsorption step adopts wet method dress post, retains liquid level, and filtrate is passed through to adsorption column, flow velocity 0.05ml/g resin per minute,Resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous absorbent resin.
7. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (5), largeMacroporous adsorbent resin post ratio of height to diameter is 10～5: 1, and the ethanol water of low powered posterior chamber is 5%～20% ethanol water, the second of the high number of degreesAlcohol solution is 50%～80% ethanol water, and washing the impurity water yield is 3～5BV, and the ethanol water amount of washing impurity low powered posterior chamber is1～2BV, the ethanol water amount of the high number of degrees of wash-out is 4BV.
8. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (7), and siliconGlue chromatographic step adopts wet method dress post, retains liquid level, and condensed cream is mixed to the rear silica gel of activation by weight at 1: 1, and by the mixing of mixingThing is placed in silicagel column top, and eluent is ethyl acetate: benzinum volume ratio is that 50～85: 15 ethyl acetate mixes with benzinumThing, elution flow rate 0.1ml/g silica gel per minute, elution volume is 5BV, silica gel activating condition is 110 DEG C of 30min.
9. the production method of balloonflower root general glycoside according to claim 1, is characterized in that: in described step (9), and tangerine60 DEG C of thermosols of 12～16 times of amount 50% ethanol waters for stalk general glycoside semi-finished product, concentrated density is d=1.03～1.05.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084971A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Method for preparing total saponins of platycodon grandiflorum |
| CN101240005A (en) * | 2007-10-29 | 2008-08-13 | 吉林农业大学 | Method for preparing platycodin D from balloon-flower root and application thereof in anti-cancer medicament |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101084971A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Method for preparing total saponins of platycodon grandiflorum |
| CN101240005A (en) * | 2007-10-29 | 2008-08-13 | 吉林农业大学 | Method for preparing platycodin D from balloon-flower root and application thereof in anti-cancer medicament |
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