CN103040901A - Production method of total platycodin - Google Patents
Production method of total platycodin Download PDFInfo
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- CN103040901A CN103040901A CN2012105955842A CN201210595584A CN103040901A CN 103040901 A CN103040901 A CN 103040901A CN 2012105955842 A CN2012105955842 A CN 2012105955842A CN 201210595584 A CN201210595584 A CN 201210595584A CN 103040901 A CN103040901 A CN 103040901A
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- radix platycodonis
- general glycoside
- ethanol water
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Abstract
The invention discloses a production method of total platycodin. The method comprises the steps that raw materials are crushed and put in from a feeding hopper; an extraction tank unit host rotates; the materials are slowly pushed from the front end of a unit backwards; an extracting solvent enters an extracting tank from a liquid inlet tube at the tail end of the unit, passes through the moving materials from the rear end of the tank, and flows to the front end; and solid and liquid substances are sufficiently contacted in a reverse motion, so that active ingredients in medicinal materials are extracted. Dregs are forcibly pushed to a dreg outlet by a discharge transport and then discharged, a special juice squeezer extrudes the dregs and extrudes residual liquor in the dregs out of a medicinal material tissue, the residual liquor content in the dregs is reduced, the extraction efficiency is higher, and the extraction is more complete. The production method adopts macroporous resin, and is combined with silicagel column chromatography for purification, the separation effect is better, and the finished total platycodin with a maximum yield of 3% and content of above 92% can be obtained.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of production method of Radix Platycodonis general glycoside, particularly relate to a kind of production method of utilizing countercurrent extraction, macroporous adsorbent resin coupling silica gel column chromatography separation and purification Radix Platycodonis general glycoside.
Background technology:
Radix Platycodonis another name RADIX PLATYCODI, RADIX PLATYCODI, RADIX PLATYCODI, Radix Platycodi, south Radix Platycodonis, powder Radix Platycodonis, BAIYAO, sharp as, stalk grass, reed as, room figure, large medicine, burden flower root, Radix Platycodonis root, Dao Laji, Radix Pesudostellariae root, husky Brassica campestris L root, mountain Radix Platycodonis root, Buddhist monk Hua Gen, Buddhist monk's headdress flower root, the Radix Talini Paniculati is from campanulaceae Platycodon grandiflouorum Platycodon grandiflouorum (Platycodon grandiforus).Spring, autumn are excavated root, remove stem and leaf and fibrous root, pulverize earth, scrape off cork, dry cut into serving pieces.Its chemical composition has kikyosaponin (platycodin) A; C; D[1]; D2; D3; remove celery glycosyl kikyosaponin (deapioplatycodin) D; D3; 2-O-=acetyl group kikyosaponin (2-O-acetylplatycodin) D2; 3-O-acetyl group kikyosaponin (3-O-acetylplaty-codin) D2; polygalin (polyglalacin) D; D2; 2-O-acetyl group polygalin (2-O-acetylpolygalacin) D; D2; 3-O-acetyl group polygalin (3-O-acetylpolygalacin) D; D2; Radix Platycodonis glycoside acid-A methyl ester (methyl platyconate-A); 2-O-methyl Radix Platycodonis glycoside acid-A methyl ester (methyl-2-O-methyplatyconate-A); Radix Platycodonis glycoside acid-A lactone (platyconic acid-Alactone) [2]; wherein main constituent is platycodin D; Platycodin A C D is called again 2-O-acetyl group platycodin D, and platycodoside C is called again 3-O-acetyl group platycodin D.Etc. various Saponins.
Kikyosaponin has the effect of eliminating the phlegm with antitussive effect, inhibition gastric secretion and antiulcer action, antiinflammatory action and promotion blood circulation.This year is more and more to the research of Radix Platycodonis, and publication number is the patent application of CN101084971, and it discloses a kind of preparation method of Radix Platycodi total saponins, comprise the steps: that in order (1) get the Radix Platycodonis medical material, add solvent, extract again after solution is transferred to alkalescence, get extracting solution; (2) macroporous type alkali anion exchange column on the extracting solution is used first aqueous alkali and pure water rinsing, and flushing liquor discards, and uses the aquiferous ethanol eluting again, and eluent is concentrated, namely gets Radix Platycodi total saponins.This technique final products purity is not high, and yield is general, and practical application effect is nothing like the effect of countercurrent extraction, the separation of macroporous adsorbent resin coupling silica gel column chromatography.
Summary of the invention
The object of the invention is to provide a kind of production method of Radix Platycodonis general glycoside; The object of the invention also be to provide a kind of convenient and swift, raw material sources abundant, extraction efficiency is high, separation and purification successful, the production technology of utilizing Continuous Countercurrent Extraction and enriching and purifying macroporous resin Radix Platycodonis general glycoside that dna purity is high.
The present invention seeks to be achieved through the following technical solutions.
A kind of production method of Radix Platycodonis general glycoside, its step is as follows:
(1) Radix Platycodonis is pulverized the rear continuous countercurrent extracting tank ethanol water reflux, extract, that adds;
(2) extracting liquid filtering that will process through (1) gets Radix Platycodonis general glycoside crude extract;
(3) gained Radix Platycodonis general glycoside crude extract is concentrated, get the thick concentrated solution of Radix Platycodonis general glycoside;
(4) with the thick concentrated solution thin up of gained Radix Platycodonis general glycoside, and filter, get filtrate;
(5) with the upper broad spectrum type macroporous resin adsorption post of gained filtrate, adsorb the complete impurity that washes with water, use again the ethanol aqueous wash impurity of low powered posterior chamber, then use the ethanol water eluting of the high number of degrees, get Radix Platycodonis general glycoside eluent;
(6) the gained eluent is condensed into cream, gets Radix Platycodonis general glycoside condensed cream;
(7) Radix Platycodonis general glycoside condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate and petroleum ether mixed liquor eluting, gets eluent as for the silicagel column top;
(8) eluent is reclaimed solvent after concentrate drying get Radix Platycodonis general glycoside semi-finished product;
(9) Radix Platycodonis general glycoside semi-finished product are dissolved with ethanol water, filter, Recycled ethanol, concentrated, place crystallize out, sucking filtration gets Radix Platycodonis general glycoside finished product.
In the described step (1), cross 30～80 mesh sieves after Radix Platycodonis is pulverized and carry out the ethanol water reflux, extract, again, the extraction solvent is 50%～85% ethanol water.
In the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises elevator, charging transmission, countercurrent extraction tank group main frame 1, draws glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draws glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary tank, heat exchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by elevator charge door place behind the crushing screening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
In the described step (1), adverse current production line parameter is elevator frequency 15～30Hz, main frame 1 frequency 18～20Hz, Juice squeezer 1 frequency 45～50Hz, main frame 2 frequencies 20～22Hz, Juice squeezer 2 frequencies 40～45Hz, Pump for giving-out flow 0.5～2T/h, charging 100～400kg/h.
In the described step (4), the dilution water yield is 5 times of concentrated solution volume, filters to such an extent that impurity discards.
In the described step (5), the macroporous resin adsorption step adopts wet method dress post, keeps liquid level, and filtrate is passed through adsorption column, flow velocity per minute 0.05ml/g resin, and the resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
In the described step (5), the macroporous adsorptive resins ratio of height to diameter is 10～5: 1, 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, the ethanol water amount of washing the impurity low powered posterior chamber is 1～2BV, and the ethanol water amount of the high number of degrees of eluting is 4BV.
In the described step (7), the silica gel column chromatography step adopts wet method dress post, keep liquid level, condensed cream is mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix places the silicagel column top, eluent is ethyl acetate: the petroleum ether volume ratio is 50～85: 15 ethyl acetate and petroleum ether mixture, elution flow rate per minute 0.1ml/g silica gel, and elution volume is 5BV.The silica gel activating condition is 110 ℃ of 30min.
In the described step (9), Radix Platycodonis general glycoside semi-finished product are measured 60 ℃ of thermosols of 50% ethanol water with 12～16 times.Concentrated density is d=1.03～1.05.
The present invention discloses a kind of production method of Radix Platycodonis general glycoside, the method is: will drop into from cast hopper after the raw material pulverizing, the rotation of extraction pot group main frame, material is slowly advanced backward from the unit front end, the feed tube that extracts simultaneously solvent slave group end enters in the extraction pot, pass mobile material forward end by the tank rear end and flow, the biphase material of solid-liquid is fully contact in this reverse movement, thereby with extracts active ingredients in the medical material out.Medicinal residues are forced to be pushed to slag notch and are discharged through the discharging conveyer, and special Juice squeezer pushes medicinal residues, and medicinal residues Shen residual liquor is extruded the medical material tissue, reduces medicinal residues Shen residual liquor content.Extraction efficiency is higher, extraction is more complete.
The present invention selects macroporous adsorbent resin and binding silica gel column chromatography purification simultaneously, and separating effect is better.
The specific embodiment:
Embodiment 1:
Take by weighing Radix Platycodonis 2T, cross 40 mesh sieves after pulverizing, at the uniform velocity added by the speed of elevator charge door with 400kg/h, 75% ethanol water is added by feed tube with the flow of tubing pump with 2T/h, and the elevator frequency setting is 30Hz, and main frame 1 frequency setting is 20Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz, get Radix Platycodonis general glycoside crude extract 10T; Radix Platycodonis general glycoside crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 600L of Radix Platycodonis general glycoside; The gained concentrated solution is added the dilution of 3T water, remove by filter impurity; Filtrate is crossed the HPD400 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T5% ethanol aqueous wash impurity, and 8T80% ethanol water eluting gets Radix Platycodonis general glycoside eluent 7.8T; Eluent concentrates to get Radix Platycodonis general glycoside condensed cream 400kg; Radix Platycodonis general glycoside condensed cream is mixed the 400kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 85: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 2000kg; Concentrate drying got Radix Platycodonis general glycoside semi-finished product 120kg after eluent reclaimed solvent; Radix Platycodonis general glycoside semi-finished product filter with 60 ℃ of thermosols of 1500L50% ethanol water, and Recycled ethanol is concentrated into d=1.05, place crystallize out, and sucking filtration gets Radix Platycodonis general glycoside finished product 40kg, content 92%.
Embodiment 2:
Take by weighing Radix Platycodonis 800kg, cross 60 mesh sieves after pulverizing, at the uniform velocity added by the speed of elevator charge door with 200kg/h, 65% ethanol water is added by feed tube with the flow of tubing pump with 1T/h, and the elevator frequency setting is 25Hz, and main frame 1 frequency setting is 18Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz, get Radix Platycodonis general glycoside crude extract 4T; Radix Platycodonis general glycoside crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 250L of Radix Platycodonis general glycoside; The gained concentrated solution is added the dilution of 1.25T water, remove by filter impurity; Filtrate is crossed the AB-8 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T20% ethanol aqueous wash impurity, and 8T600% ethanol water eluting gets Radix Platycodonis general glycoside eluent 7.8T; Eluent concentrates to get Radix Platycodonis general glycoside condensed cream 150kg; Radix Platycodonis general glycoside condensed cream is mixed the 150kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 65: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 750kg; Concentrate drying got Radix Platycodonis general glycoside semi-finished product 50kg after eluent reclaimed solvent; Radix Platycodonis general glycoside semi-finished product filter with 60 ℃ of thermosols of 600L50% ethanol water, and Recycled ethanol is concentrated into d=1.04, place crystallize out, and sucking filtration gets Radix Platycodonis general glycoside finished product 24kg, content 93%.
Embodiment 3:
Take by weighing Radix Platycodonis 1.6T, cross 80 mesh sieves after pulverizing, at the uniform velocity added by the speed of elevator charge door with 100kg/h, 75% ethanol water is added by feed tube with the flow of tubing pump with 500kg/h, and the elevator frequency setting is 25Hz, and main frame 1 frequency setting is 18Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency settings are 22Hz, and Juice squeezer 2 frequency settings are 45Hz, get Radix Platycodonis general glycoside crude extract 8T; Radix Platycodonis general glycoside crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 500L of Radix Platycodonis general glycoside; The gained concentrated solution is added the dilution of 2.5T water, remove by filter impurity; Filtrate is crossed the DM-130 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T15% ethanol aqueous wash impurity, and 8T70% ethanol water eluting gets Radix Platycodonis general glycoside eluent 7.8T; Eluent concentrates to get Radix Platycodonis general glycoside condensed cream 310kg; Radix Platycodonis general glycoside condensed cream is mixed the 310kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 75: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 1.5T; Concentrate drying got Radix Platycodonis general glycoside semi-finished product 110kg after eluent reclaimed solvent; Radix Platycodonis general glycoside semi-finished product filter with 60 ℃ of thermosols of 1.6T50% ethanol water, and Recycled ethanol is concentrated into d=1.03, place crystallize out, and sucking filtration gets Radix Platycodonis general glycoside finished product 38kg, content 94%.
Claims (9)
1. the production method of a Radix Platycodonis general glycoside is characterized in that the method comprises the steps:
(1) Radix Platycodonis is pulverized the rear continuous countercurrent extracting tank ethanol water reflux, extract, that adds;
(2) extracting liquid filtering that will process through (1) gets Radix Platycodonis general glycoside crude extract;
(3) gained Radix Platycodonis general glycoside crude extract is concentrated, get the thick concentrated solution of Radix Platycodonis general glycoside;
(4) with the thick concentrated solution thin up of gained Radix Platycodonis general glycoside, and filter, get filtrate;
(5) with the upper broad spectrum type macroporous resin adsorption post of gained filtrate, adsorb the complete impurity that washes with water, use again the ethanol aqueous wash impurity of low powered posterior chamber, then use the ethanol water eluting of the high number of degrees, get Radix Platycodonis general glycoside eluent;
(6) the gained eluent is condensed into cream, gets Radix Platycodonis general glycoside condensed cream;
(7) Radix Platycodonis general glycoside condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate and petroleum ether mixed liquor eluting, gets eluent as for the silicagel column top;
(8) eluent is reclaimed solvent after concentrate drying get Radix Platycodonis general glycoside semi-finished product;
(9) Radix Platycodonis general glycoside semi-finished product are dissolved with ethanol water, filter, Recycled ethanol, concentrated, place crystallize out, sucking filtration gets Radix Platycodonis general glycoside finished product.
2. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (1), crosses 30～80 mesh sieves after Radix Platycodonis is pulverized and carries out the ethanol water reflux, extract, again, and the extraction solvent is 50%～85% ethanol water.
3. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises elevator, charging transmission, countercurrent extraction tank group main frame 1, draws glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draws glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary tank, heat exchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by elevator charge door place behind the crushing screening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
4. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (1), adverse current production line parameter is, elevator frequency 15～30Hz, main frame 1 frequency 18～20Hz, Juice squeezer 1 frequency 45～50Hz, main frame 2 frequencies 20～22Hz, Juice squeezer 2 frequencies 40～45Hz, Pump for giving-out flow 0.5～2T/h, charging 100～400kg/h.
5. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (4), and the dilution water yield is 5 times of concentrated solution volume, filters to such an extent that impurity discards.
6. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (5), the macroporous resin adsorption step adopts wet method dress post, keep liquid level, filtrate is passed through adsorption column, flow velocity per minute 0.05ml/g resin, resin model are HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
7. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (5), the macroporous adsorptive resins ratio of height to diameter is 10～5: 1, 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, the ethanol water amount of washing the impurity low powered posterior chamber is 1～2BV, and the ethanol water amount of the high number of degrees of eluting is 4BV.
8. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (7), the silica gel column chromatography step adopts wet method dress post, keep liquid level, condensed cream is mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix places silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 50～85: 15 ethyl acetate and petroleum ether mixture, elution flow rate per minute 0.1ml/g silica gel, elution volume is 5BV, and the silica gel activating condition is 110 ℃ of 30min.
9. the production method of Radix Platycodonis general glycoside according to claim 1 is characterized in that in the described step (9), and Radix Platycodonis general glycoside semi-finished product are measured 60 ℃ of thermosols of 50% ethanol water with 12～16 times.Concentrated density is d=1.03～1.05.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210595584.2A CN103040901B (en) | 2012-12-13 | 2012-12-13 | A kind of production method of balloonflower root general glycoside |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210595584.2A CN103040901B (en) | 2012-12-13 | 2012-12-13 | A kind of production method of balloonflower root general glycoside |
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| CN103040901A true CN103040901A (en) | 2013-04-17 |
| CN103040901B CN103040901B (en) | 2016-05-25 |
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| CN201210595584.2A Expired - Fee Related CN103040901B (en) | 2012-12-13 | 2012-12-13 | A kind of production method of balloonflower root general glycoside |
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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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2012
- 2012-12-13 CN CN201210595584.2A patent/CN103040901B/en not_active Expired - Fee Related
Patent 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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| CN103040901B (en) | 2016-05-25 |
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