CN103073474B - The production technique of a kind of Motherwort Herb stachydrine - Google Patents
The production technique of a kind of Motherwort Herb stachydrine Download PDFInfo
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- CN103073474B CN103073474B CN201210595342.3A CN201210595342A CN103073474B CN 103073474 B CN103073474 B CN 103073474B CN 201210595342 A CN201210595342 A CN 201210595342A CN 103073474 B CN103073474 B CN 103073474B
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- motherwort herb
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Abstract
The present invention discloses the production technique of a kind of Motherwort Herb stachydrine, the method is: drop into after raw material pulverizing from cast hopper, extractor group main frame rotates, material is slowly advanced backward from unit front end, Extraction solvent enters in extractor from the liquid-inlet pipe of unit end simultaneously, flow by the material forward end of tank rear end through movement, Gu liquid two-phase material fully contacts in this kind of inverse motion, thus by extracts active ingredients in medicinal material out. The dregs of a decoction are forced to be pushed to slag notch and discharge through discharging forwarder, and the dregs of a decoction are extruded by special Juice squeezer, and dregs of a decoction Shen residual liquor is extruded medicinal material tissue, reduce dregs of a decoction 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. Can obtain the highest receipts rate is 0.4%, and content is the Motherwort Herb stachydrine finished product of more than 95.5%.
Description
Technical field:
The invention belongs to field of natural organic chemistry, it relates to the production technique of a kind of stachydrine, particularly relate to a kind of production technique utilizing countercurrent extraction, macroporous adsorbent resin coupling silica gel column chromatography separation and purification Motherwort Herb stachydrine.
Background technology:
The Motherwort Herb another name female wormwood artemisia of Motherwort Herb benefit, the female Chinese mugwort of benefit, safflower Chinese mugwort, female grass, motherwort, triangle linseed, four stupefied son wild flax, sweet fiber crops, nine tower flowers, mountain fiber crops and veronica. These product are the fresh or dry aerial parts of labiate Motherwort Herb LeonurusjaponicusHoutt.. Summer, autumn extract full grass on the ground when blooming, remove impurity, and cut-out is dried. Full grass, containing syringic acid.delta.-guanidinobutyl ester (leonurine) 0.05%, is bloomed this composition of initial stage only containing trace, and is increased gradually in flowering period. Another containing stachydrine (stachydrine), syringic acid.delta.-guanidinobutyl ester first and second, syringic acid.delta.-guanidinobutyl ester first is the nitrite (leonurinenitrite) of syringic acid.delta.-guanidinobutyl ester. in addition, containing phytomelin and fumaric acid. and laudanum alkane (labdan) type diterpene compound Motherwort Herb element (leosibirin), different Motherwort Herb element (isoleosibirin) and Motherwort Herb qin element (leosibiricin). flower is containing Motherwort Herb booth alkali (leonuridine).
Stachydrine Stachydrine belongs to alkaloids, and this product has promoting blood flow to regulate menstruation, inducing diuresis to remove edema, shrinks the effect in uterus. Myocardial ischemia caused by suprarenin is improved coronary artery and cardiac muscle nutritional blood flow, minimizing myocardium cell necrosis amount, reduces blood viscosity, reduce vascular resistance, improve microcirculation, the effect such as reducing heart rate, minimizing cardiac output and anti-platelet aggregation. Existing Motherwort Herb technique many employings traditional extraction, Zeo-karb processes, ammoniacal liquor wash-out, or agent treated again. Publication number be CN101863814A with profit application, it discloses the method for refining stachydrine in a kind of Motherwort Herb, product content is up to 95%, but this extraction and separation process, extraction efficiency is lower, complex steps in later stage exquisiteness, practical application effect is nothing like the effect utilizing the coupling silica gel column chromatography separation of countercurrent extraction, macroporous adsorbent resin.
Summary of the invention
The object of the invention is to provide the production technique of a kind of Motherwort Herb stachydrine; The object of the invention also be to provide a kind of convenient and swift, abundant raw material source, extraction efficiency height, separation and purification successful, DNA purity high utilize Continuous Countercurrent Extraction and the production technique of enriching and purifying macroporous resin Motherwort Herb stachydrine.
The present invention seeks to be achieved through the following technical solutions.
A production technique for Motherwort Herb stachydrine, its step is as follows:
(1) continuous countercurrent extracting tank aqueous ethanolic solution refluxing extraction is added after being pulverized by Motherwort Herb;
(2) extracting liquid filtering that will process through (1), obtains Motherwort Herb stachydrine crude extract:
(3) gained Motherwort Herb stachydrine crude extract is concentrated, obtain the thick concentrated solution of Motherwort Herb stachydrine;
(4) by thick for gained Motherwort Herb stachydrine concentrated solution thin up, and filter, obtain filtrate;
(5) by upper for gained filtrate broad spectrum type macroporous resin adsorption post, adsorb and complete wash impurity with water, then with the ethanol aqueous wash impurity of the low number of degrees, then with the aqueous ethanolic solution wash-out of the high number of degrees, obtain Motherwort Herb stachydrine elutriant;
(6) gained elutriant is condensed into cream, obtains Motherwort Herb stachydrine condensed cream;
(7) Motherwort Herb stachydrine condensed cream is mixed silica gel, and by the mixture mixed as, above silicagel column, through ethyl acetate and sherwood oil mixed solution wash-out, obtaining elutriant;
(8) concentrate drying after elutriant recycling design is obtained Motherwort Herb stachydrine work in-process;
(9) Motherwort Herb stachydrine work in-process aqueous ethanolic solution is dissolved, filter, reclaim ethanol, concentrated, place crystallize out, take out and filter to obtain Motherwort Herb stachydrine finished product.
In described step (1), Motherwort Herb crosses 30��80 order sieves and carries out aqueous ethanolic solution refluxing extraction again after pulverizing, Extraction solvent is the aqueous ethanolic solution of 50%��85%.
In described step (1), the equipment extracted is countercurrent extraction production line, comprise lift, charging transmission, countercurrent extraction tank group main frame 1, draw glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draw glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary storage tank, interchanger, liquid flowing valve etc. The rear raw material that pulverizes and sieves at the uniform velocity is added by lift charging opening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
In described step (1), adverse current production line parameter is, lift frequency 15��30Hz, 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 concentrated solution volume, filter impurity is abandoned.
In described step (5), macroporous resin adsorption step adopts wet method dress post, retains liquid level, and by filtrate by adsorption column, flow velocity every minute 0.05ml/g resin, resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
In described step (5), macroporous adsorptive resins aspect ratio is 10��5: 1, the aqueous ethanolic solution of the low number of degrees is 5%��20% aqueous ethanolic solution, the aqueous ethanolic solution of the high number of degrees is 50%��80% aqueous ethanolic solution, washing the impurity water yield is 3��5BV, the aqueous ethanolic solution amount washing the low number of degrees of impurity is 1��2BV, and the aqueous ethanolic solution amount of the wash-out height number of degrees is 4BV.
In described step (7), silica gel column chromatography step adopts wet method dress post, retain liquid level, condensed cream is mixed activation rear silica gel by weight at 1: 1, and the mixture mixed is placed in above silicagel column, elutriant is ethyl acetate: sherwood oil volume ratio is ethyl acetate and the petroleum ether mixtures of 50��85: 15, and elution flow rate every minute 0.1ml/g silica gel, elution volume is 5BV. Silica gel activating condition is, 110 DEG C of 30min.
In described step (9), Motherwort Herb stachydrine work in-process are molten by 12��16 times amount 50% aqueous ethanolic solution 60 DEG C of heat. Concentration densities is d=1.03��1.05.
The present invention discloses the production technique of a kind of Motherwort Herb stachydrine, the method is: drop into after raw material pulverizing from cast hopper, extractor group main frame rotates, material is slowly advanced backward from unit front end, Extraction solvent enters in extractor from the liquid-inlet pipe of unit end simultaneously, flow by the material forward end of tank rear end through movement, Gu liquid two-phase material fully contacts in this kind of inverse motion, thus by extracts active ingredients in medicinal material out. The dregs of a decoction are forced to be pushed to slag notch and discharge through discharging forwarder, and the dregs of a decoction are extruded by special Juice squeezer, and dregs of a decoction Shen residual liquor is extruded medicinal material tissue, reduce dregs of a decoction 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.
Embodiment:
Embodiment 1:
Take Motherwort Herb 2T, 40 order sieves are crossed after pulverizing, at the uniform velocity add with the speed of 400kg/h by lift charging opening, 75% aqueous ethanolic solution in-line pump is added by liquid-inlet pipe with the flow of 2T/h, and lift frequency setting is 30Hz, and main frame 1 frequency setting is 20Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency setting is 22Hz, and Juice squeezer 2 frequency setting is 45Hz, obtains Motherwort Herb stachydrine crude extract 10T; From flowing to, temporary storage tank concentrates to concentration tank Motherwort Herb stachydrine crude extract via Pump for giving-out continuous pump, obtains the thick concentrated solution 600L of Motherwort Herb stachydrine; Gained concentrated solution is added the dilution of 3T water, is filtered to remove impurity; Filtrate crosses HPD400 macroporous adsorbent resin, and resin column aspect ratio is 5: 1, adsorbs saturated rear 6T and washes impurity, 2T5% ethanol aqueous wash impurity, and 8T80% aqueous ethanolic solution wash-out, obtains Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to obtain Motherwort Herb stachydrine condensed cream 40kg; Motherwort Herb stachydrine condensed cream mixes 40kg activated silica gel, is placed in above silicagel column, and elutriant is ethyl acetate: sherwood oil volume ratio is ethyl acetate and the petroleum ether mixtures of 85: 15, and elution flow rate every minute 0.1ml/g silica gel, obtains elutriant 200kg; After elutriant recycling design, concentrate drying obtains Motherwort Herb stachydrine work in-process 24kg; Motherwort Herb stachydrine work in-process 360L50% aqueous ethanolic solution 60 DEG C of heat are molten, filter, and reclaim ethanol, concentrate to d=1.05, place crystallize out, take out and filter to obtain Motherwort Herb stachydrine finished product 8kg, content 97.2%.
Embodiment 2:
Take Motherwort Herb 800kg, 60 order sieves are crossed after pulverizing, at the uniform velocity add with the speed of 200kg/h by lift charging opening, 65% aqueous ethanolic solution in-line pump is added by liquid-inlet pipe with the flow of 1T/h, and lift frequency setting is 25Hz, and main frame 1 frequency setting is 18Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency setting is 22Hz, and Juice squeezer 2 frequency setting is 45Hz, obtains Motherwort Herb stachydrine crude extract 4T; From flowing to, temporary storage tank concentrates to concentration tank Motherwort Herb stachydrine crude extract via Pump for giving-out continuous pump, obtains the thick concentrated solution 250L of Motherwort Herb stachydrine; Gained concentrated solution is added the dilution of 1.25T water, is filtered to remove impurity; Filtrate crosses AB-8 macroporous adsorbent resin, and resin column aspect ratio is 5: 1, adsorbs saturated rear 6T and washes impurity, 2T20% ethanol aqueous wash impurity, and 8T600% aqueous ethanolic solution wash-out, obtains Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to obtain Motherwort Herb stachydrine condensed cream 15kg; Motherwort Herb stachydrine condensed cream mixes 15kg activated silica gel, is placed in above silicagel column, and elutriant is ethyl acetate: sherwood oil volume ratio is ethyl acetate and the petroleum ether mixtures of 65: 15, and elution flow rate every minute 0.1ml/g silica gel, obtains elutriant 75kg; After elutriant recycling design, concentrate drying obtains Motherwort Herb stachydrine work in-process 5kg; Motherwort Herb stachydrine work in-process 80L50% aqueous ethanolic solution 60 DEG C of heat are molten, filter, and reclaim ethanol, concentrate to d=1.04, place crystallize out, take out and filter to obtain Motherwort Herb stachydrine finished product 3kg, content 95.8%.
Embodiment 3:
Take Motherwort Herb 1.6T, 30 order sieves are crossed after pulverizing, at the uniform velocity add with the speed of 100kg/h by lift charging opening, 75% aqueous ethanolic solution in-line pump is added by liquid-inlet pipe with the flow of 500kg/h, and lift frequency setting is 25Hz, and main frame 1 frequency setting is 18Hz, Juice squeezer 1 frequency setting is 50Hz, main frame 2 frequency setting is 22Hz, and Juice squeezer 2 frequency setting is 45Hz, obtains Motherwort Herb stachydrine crude extract 8T; From flowing to, temporary storage tank concentrates to concentration tank Motherwort Herb stachydrine crude extract via Pump for giving-out continuous pump, obtains the thick concentrated solution 500L of Motherwort Herb stachydrine; Gained concentrated solution is added the dilution of 2.5T water, is filtered to remove impurity; Filtrate crosses DM-130 macroporous adsorbent resin, and resin column aspect ratio is 5: 1, adsorbs saturated rear 6T and washes impurity, 2T15% ethanol aqueous wash impurity, and 8T70% aqueous ethanolic solution wash-out, obtains Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to obtain Motherwort Herb stachydrine condensed cream 31kg; Motherwort Herb stachydrine condensed cream mixes 31kg activated silica gel, is placed in above silicagel column, and elutriant is ethyl acetate: sherwood oil volume ratio is ethyl acetate and the petroleum ether mixtures of 75: 15, and elution flow rate every minute 0.1ml/g silica gel, obtains elutriant 150L; After elutriant recycling design, concentrate drying obtains Motherwort Herb stachydrine work in-process 11kg; Motherwort Herb stachydrine work in-process 160L50% aqueous ethanolic solution 60 DEG C of heat are molten, filter, and reclaim ethanol, concentrate to d=1.03, place crystallize out, take out and filter to obtain Motherwort Herb stachydrine finished product 6kg, content 96%.
Claims (9)
1. the production technique of a Motherwort Herb stachydrine, it is characterised in that the method comprises the steps:
(1) continuous countercurrent extracting tank aqueous ethanolic solution Continuous Countercurrent Extraction is added after being pulverized by Motherwort Herb;
(2) extracting liquid filtering that will process through (1), obtains Motherwort Herb stachydrine crude extract:
(3) gained Motherwort Herb stachydrine crude extract is concentrated, obtain the thick concentrated solution of Motherwort Herb stachydrine;
(4) by thick for gained Motherwort Herb stachydrine concentrated solution thin up, and filter, obtain filtrate;
(5) by upper for step (4) gained filtrate broad spectrum type macroporous resin adsorption post, adsorb and complete wash impurity with water, it is 5%��20% ethanol aqueous wash impurity by concentration again, then it is the aqueous ethanolic solution wash-out of 50%��80% by concentration, obtains Motherwort Herb stachydrine elutriant;
(6) gained Motherwort Herb stachydrine elutriant is condensed into cream, obtains Motherwort Herb stachydrine condensed cream;
(7) Motherwort Herb stachydrine condensed cream is mixed silica gel, and the mixture mixed is placed in above silicagel column, through ethyl acetate and sherwood oil mixed solution wash-out, obtain elutriant;
(8) concentrate drying after step (7) gained elutriant recycling design is obtained Motherwort Herb stachydrine work in-process;
(9) Motherwort Herb stachydrine work in-process aqueous ethanolic solution is dissolved, filter, reclaim ethanol, concentrated, place crystallize out, take out and filter to obtain Motherwort Herb stachydrine finished product.
2. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterized in that in described step (1), Motherwort Herb crosses 30��80 order sieves and carries out aqueous ethanolic solution Continuous Countercurrent Extraction again after pulverizing, Extraction solvent is the aqueous ethanolic solution of 50%��85%.
3. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterized in that in described step (1), the equipment extracted is Continuous Countercurrent Extraction production line, comprise lift, charging transmission, countercurrent extraction tank group main frame 1, draw glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draw glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporarily storage tank, interchanger and liquid flowing valve; The rear raw material that pulverizes and sieves at the uniform velocity is added by lift charging opening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
4. the production technique of Motherwort Herb stachydrine according to claim 3, it is characterized in that in described step (1), Continuous Countercurrent Extraction production line parameter is, lift frequency 15��30Hz, countercurrent extraction tank group main frame 1 frequency 18��20Hz, Juice squeezer 1 frequency 45��50Hz, countercurrent extraction tank group 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.
5. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterised in that in described step (4), the dilution water yield is 5 times of concentrated solution volume, filter impurity is abandoned.
6. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterized in that in described step (5), macroporous resin adsorption step adopts wet method dress post, retain liquid level, filtrate is passed through adsorption column, flow velocity every minute 0.05ml/g resin, resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
7. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterized in that in described step (5), broad spectrum type macroporous resin adsorption post aspect ratio is 10��5:1, washing the impurity water yield is 3��5BV, wash impurity concentration be 5%��20% aqueous ethanolic solution amount be 1��2BV, wash-out concentration is the aqueous ethanolic solution amount of 50%��80% is 4BV.
8. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterized in that in described step (7), silica gel column chromatography step adopts wet method dress post, retain liquid level, by condensed cream by weight 1:1 mix silica gel after activation, and the mixture mixed is placed in above silicagel column, elutriant is ethyl acetate: sherwood oil volume ratio is the mixture of 50��85:15, elution flow rate every minute 0.1ml/g silica gel, elution volume is 5BV; Silica gel activating condition is, 110 DEG C of 30min.
9. the production technique of Motherwort Herb stachydrine according to claim 1, it is characterised in that in described step (9), Motherwort Herb stachydrine work in-process are molten by 12��16 times amount 50% aqueous ethanolic solution 60 DEG C of heat; Concentration densities is d=1.03��1.05.
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| CN106928115A (en) * | 2017-03-29 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract stachydrine hydrochloride in motherwort |
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| WO2007110637A1 (en) * | 2006-03-28 | 2007-10-04 | Bioniqs Limited | Method for extracting target alkaloid using an ionic liquid as extracting solvent |
| CN101244060A (en) * | 2007-02-15 | 2008-08-20 | 北京天新园医药科技开发有限公司 | Leonurus heterophyllus alkaloid composition and method of preparing the same |
| CN101863814A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Method for refining stachydrine from motherwort |
| CN102702061A (en) * | 2012-06-07 | 2012-10-03 | 浙江维康药业有限公司 | Stachydrine hydrochloride compound and medicinal composition containing stachydrine hydrochloride compound |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007110637A1 (en) * | 2006-03-28 | 2007-10-04 | Bioniqs Limited | Method for extracting target alkaloid using an ionic liquid as extracting solvent |
| CN101244060A (en) * | 2007-02-15 | 2008-08-20 | 北京天新园医药科技开发有限公司 | Leonurus heterophyllus alkaloid composition and method of preparing the same |
| CN101863814A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Method for refining stachydrine from motherwort |
| CN102702061A (en) * | 2012-06-07 | 2012-10-03 | 浙江维康药业有限公司 | Stachydrine hydrochloride compound and medicinal composition containing stachydrine hydrochloride compound |
Non-Patent Citations (2)
| Title |
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