CN103073474A - Manufacturing technology for leonurus stachydrine - Google Patents
Manufacturing technology for leonurus stachydrine Download PDFInfo
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- CN103073474A CN103073474A CN2012105953423A CN201210595342A CN103073474A CN 103073474 A CN103073474 A CN 103073474A CN 2012105953423 A CN2012105953423 A CN 2012105953423A CN 201210595342 A CN201210595342 A CN 201210595342A CN 103073474 A CN103073474 A CN 103073474A
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- stachydrine
- motherwort herb
- aqueous ethanolic
- ethanolic solution
- herb
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Abstract
The invention discloses a manufacturing technology for leonurus stachydrine, which comprises the following steps: crushed raw materials are fed from a feeding hopper; an extraction tank group host machine rotates; the materials are pushed backwards slowly from the front end of a machine set; meanwhile, resolvent is extracted, and enters into an extraction tank through a liquid feeding pipe at the tail end of the machine set; materials passing through the rear end of the tank flow to the front end; solid and liquid materials are in sound contact during the inverse motion, so as to extract effective components from herbs; herb residue is forcibly pushed through a discharging transmitter to a residue discharge opening and then discharged, and is extruded through a dedicated extruder, so as to extrude residual liquid in the herb residue from herb tissues, and reduce the content of residual liquid in the herb residue. The method has the advantages that the extraction efficiency is higher; and the extraction is more complete. Moreover, macroporous resin is adopted and the silica gel column chromatography is combined for purification, so that the separation effect is better. The leonurus stachydrine finished product with 0.4 percent of maximum yield and higher than 95.5 percent content can be obtained.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of production technique of stachydrine, particularly relate to a kind of production technique of utilizing countercurrent extraction, macroporous adsorbent resin coupling silica gel column chromatography separation and purification Motherwort Herb stachydrine.
Background technology:
Motherwort Herb is called the female wormwood artemisia of Motherwort Herb benefit, benefit female Chinese mugwort, safflower Chinese mugwort, female grass, motherwort, triangle linseed, four a stupefied son wild flax, Tian Ma Kuo, nine towers are colored, the mountain is numb and veronica.These product are the fresh or dry aerial parts of labiate Motherwort Herb Leonurus japonicus Houtt..Summer, extract herb on the ground when the autumn blooms, remove impurity, cut-out is dried.Herb contains syringic acid.delta.-guanidinobutyl ester (leonurine) 0.05%, and this composition that comes into bloom only contains trace, and increases gradually in flowering period.Other contains stachydrine (stachydrine), syringic acid.delta.-guanidinobutyl ester first and second, the syringic acid.delta.-guanidinobutyl ester first is the nitrite (leonurinenitrite) of syringic acid.delta.-guanidinobutyl ester. in addition, contain 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 contains 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, the effect in contraction uterus.To myocardial ischemia that suprarenin causes be improved coronary artery and Nutritional myocardium blood flow amount, reduce the myocardium cell necrosis amount, reduce blood viscosity, reduce vascular resistance, improve microcirculation, the effects such as reducing heart rate, minimizing cardiac output and anti-platelet aggregation.Existing Motherwort Herb technique adopts conventional the extraction more, and Zeo-karb is processed, ammoniacal liquor wash-out, or agent treated again.Publication number be CN101863814A with the 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 the later stage exquisiteness, practical application effect are nothing like the effect of utilizing countercurrent extraction, macroporous adsorbent resin coupling silica gel column chromatography to separate.
Summary of the invention
The object of the invention is to provide a kind of production technique of Motherwort Herb stachydrine; 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 technique of utilizing Continuous Countercurrent Extraction and enriching and purifying macroporous resin Motherwort Herb stachydrine that dna purity is high.
The present invention seeks to be achieved through the following technical solutions.
A kind of production technique of Motherwort Herb stachydrine, its step is as follows:
(1) Motherwort Herb is pulverized the rear continuous countercurrent extracting tank aqueous ethanolic solution refluxing extraction that adds;
(2) extracting liquid filtering that will process through (1) gets Motherwort Herb stachydrine crude extract:
(3) gained Motherwort Herb stachydrine crude extract is concentrated, get the thick concentrated solution of Motherwort Herb stachydrine;
(4) with the thick concentrated solution thin up of gained Motherwort Herb stachydrine, 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 aqueous ethanolic solution wash-out of the high number of degrees, get Motherwort Herb stachydrine elutriant;
(6) the gained elutriant is condensed into cream, gets Motherwort Herb stachydrine condensed cream;
(7) Motherwort Herb stachydrine condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate and sherwood oil mixed solution wash-out, gets elutriant as for the silicagel column top;
(8) elutriant is reclaimed solvent after concentrate drying get Motherwort Herb stachydrine work in-process;
(9) Motherwort Herb stachydrine work in-process are dissolved with aqueous ethanolic solution, filter, Recycled ethanol, concentrated, place crystallize out, suction filtration gets Motherwort Herb stachydrine finished product.
In the described step (1), cross 30～80 mesh sieves after Motherwort Herb is pulverized and carry out the aqueous ethanolic solution refluxing extraction again, the extraction solvent is 50%～85% aqueous ethanolic solution.
In the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises lift, 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, interchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by lift charging opening 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 lift 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 aspect ratio is 10～5: 1, the aqueous ethanolic solution of low powered posterior chamber 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 of washing the impurity low powered posterior chamber is 1～2BV, and the aqueous ethanolic solution amount of the high number of degrees of wash-out 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, elutriant is ethyl acetate: the sherwood oil volume ratio is 50～85: 15 ethyl acetate and sherwood oil 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), Motherwort Herb stachydrine work in-process are measured 60 ℃ of thermosols of 50% aqueous ethanolic solution with 12～16 times.Concentrated density is d=1.03～1.05.
The present invention discloses a kind of production technique of Motherwort Herb stachydrine, the method is: will drop into from cast hopper after the raw material pulverizing, the rotation of extractor group main frame, material is slowly advanced backward from the unit front end, the liquid-inlet pipe that extracts simultaneously solvent slave group end enters in the extractor, pass mobile material forward end by the tank rear end and flow, solid-liquid two-phase material is fully contact in this inverse motion, thereby with extracts active ingredients in the medicinal material out.The dregs of a decoction are forced to be pushed to slag notch and are discharged through the discharging forwarder, and special Juice squeezer pushes the dregs of a decoction, and dregs of a decoction Shen residual liquor is extruded the 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 adsorbent resin and binding silica gel column chromatography purification simultaneously, and separating effect is better.
Embodiment:
Embodiment 1:
Take by weighing Motherwort Herb 2T, cross 40 mesh sieves after pulverizing, at the uniform velocity added by the speed of lift charging opening with 400kg/h, 75% aqueous ethanolic solution is added by liquid-inlet pipe with the flow of in-line pump with 2T/h, and the lift 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 Motherwort Herb stachydrine crude extract 10T; Motherwort Herb stachydrine 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 Motherwort Herb stachydrine; 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 aspect ratio is 5: 1, adsorbs saturated rear 6T washing impurity, 2T5% ethanol aqueous wash impurity, and 8T80% aqueous ethanolic solution wash-out gets Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to get Motherwort Herb stachydrine condensed cream 40kg; Motherwort Herb stachydrine condensed cream is mixed the 40kg activated silica gel, places the silicagel column top, and elutriant is ethyl acetate: the sherwood oil volume ratio is 85: 15 ethyl acetate and sherwood oil mixture, and elution flow rate per minute 0.1ml/g silica gel gets elutriant 200kg; Concentrate drying got Motherwort Herb stachydrine work in-process 24kg after elutriant reclaimed solvent; Motherwort Herb stachydrine work in-process filter with 60 ℃ of thermosols of 360L50% aqueous ethanolic solution, and Recycled ethanol is concentrated into d=1.05, place crystallize out, and suction filtration gets Motherwort Herb stachydrine finished product 8kg, content 97.2%.
Embodiment 2:
Take by weighing Motherwort Herb 800kg, cross 60 mesh sieves after pulverizing, at the uniform velocity added by the speed of lift charging opening with 200kg/h, 65% aqueous ethanolic solution is added by liquid-inlet pipe with the flow of in-line pump with 1T/h, and the lift 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 Motherwort Herb stachydrine crude extract 4T; Motherwort Herb stachydrine 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 Motherwort Herb stachydrine; 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 aspect ratio is 5: 1, adsorbs saturated rear 6T washing impurity, 2T20% ethanol aqueous wash impurity, and 8T600% aqueous ethanolic solution wash-out gets Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to get Motherwort Herb stachydrine condensed cream 15kg; Motherwort Herb stachydrine condensed cream is mixed the 15kg activated silica gel, places the silicagel column top, and elutriant is ethyl acetate: the sherwood oil volume ratio is 65: 15 ethyl acetate and sherwood oil mixture, and elution flow rate per minute 0.1ml/g silica gel gets elutriant 75kg; Concentrate drying got Motherwort Herb stachydrine work in-process 5kg after elutriant reclaimed solvent; Motherwort Herb stachydrine work in-process filter with 60 ℃ of thermosols of 80L50% aqueous ethanolic solution, and Recycled ethanol is concentrated into d=1.04, place crystallize out, and suction filtration gets Motherwort Herb stachydrine finished product 3kg, content 95.8%.
Embodiment 3:
Take by weighing Motherwort Herb 1.6T, cross 30 mesh sieves after pulverizing, at the uniform velocity added by the speed of lift charging opening with 100kg/h, 75% aqueous ethanolic solution is added by liquid-inlet pipe with the flow of in-line pump with 500kg/h, and the lift 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 Motherwort Herb stachydrine crude extract 8T; Motherwort Herb stachydrine 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 Motherwort Herb stachydrine; 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 aspect ratio is 5: 1, adsorbs saturated rear 6T washing impurity, 2T15% ethanol aqueous wash impurity, and 8T70% aqueous ethanolic solution wash-out gets Motherwort Herb stachydrine elutriant 7.8T; Elutriant concentrates to get Motherwort Herb stachydrine condensed cream 31kg; Motherwort Herb stachydrine condensed cream is mixed the 31kg activated silica gel, places the silicagel column top, and elutriant is ethyl acetate: the sherwood oil volume ratio is 75: 15 ethyl acetate and sherwood oil mixture, and elution flow rate per minute 0.1ml/g silica gel gets elutriant 150L; Concentrate drying got Motherwort Herb stachydrine work in-process 11kg after elutriant reclaimed solvent; Motherwort Herb stachydrine work in-process filter with 60 ℃ of thermosols of 160L50% aqueous ethanolic solution, and Recycled ethanol is concentrated into d=1.03, place crystallize out, and suction filtration gets Motherwort Herb stachydrine finished product 6kg, content 96%.
Claims (9)
1. the production technique of a Motherwort Herb stachydrine is characterized in that the method comprises the steps:
(1) Motherwort Herb is pulverized the rear continuous countercurrent extracting tank aqueous ethanolic solution refluxing extraction that adds;
(2) will be through 1) extracting liquid filtering processed, get Motherwort Herb stachydrine crude extract:
(3) gained Motherwort Herb stachydrine crude extract is concentrated, get the thick concentrated solution of Motherwort Herb stachydrine;
(4) with the thick concentrated solution thin up of gained Motherwort Herb stachydrine, 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 aqueous ethanolic solution wash-out of the high number of degrees, get Motherwort Herb stachydrine elutriant;
(6) the gained elutriant is condensed into cream, gets Motherwort Herb stachydrine condensed cream;
(7) Motherwort Herb stachydrine condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate and sherwood oil mixed solution wash-out, gets elutriant as for the silicagel column top;
(8) elutriant is reclaimed solvent after concentrate drying get Motherwort Herb stachydrine work in-process;
(9) Motherwort Herb stachydrine work in-process are dissolved with aqueous ethanolic solution, filter, Recycled ethanol, concentrated, place crystallize out, suction filtration gets Motherwort Herb stachydrine finished product.
2. the production technique of Motherwort Herb stachydrine according to claim 1 is characterized in that in the described step (1), crosses 30～80 mesh sieves after Motherwort Herb is pulverized and carries out the aqueous ethanolic solution refluxing extraction again, and the extraction solvent is 50%～85% aqueous ethanolic solution.
3. the production technique of Motherwort Herb stachydrine according to claim 1 is characterized in that in the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises lift, 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, interchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by lift charging opening place behind the crushing screening, 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 1 is characterized in that in the 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 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 technique of Motherwort Herb stachydrine 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 technique of Motherwort Herb stachydrine 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 technique of Motherwort Herb stachydrine according to claim 1 is characterized in that in the described step (5), the macroporous adsorptive resins aspect ratio is 10～5: 1, the aqueous ethanolic solution of low powered posterior chamber 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 of washing the impurity low powered posterior chamber is 1～2BV, and the aqueous ethanolic solution amount of the high number of degrees of wash-out is 4BV.
8. the production technique of Motherwort Herb stachydrine 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 the silicagel column top, elutriant is ethyl acetate: the sherwood oil volume ratio is 50～85: 15 ethyl acetate and sherwood oil 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.
9. the production technique of Motherwort Herb stachydrine according to claim 1 is characterized in that in the described step (9), and Motherwort Herb stachydrine work in-process are measured 60 ℃ of thermosols of 50% aqueous ethanolic solution with 12～16 times.Concentrated density is d=1.03～1.05.
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| CN201210595342.3A CN103073474B (en) | 2012-12-13 | 2012-12-13 | The production technique of a kind of Motherwort Herb stachydrine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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 |
-
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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 |
|---|
| 刘莉，等: "益母草提取工艺优选", 《中国实验方剂学杂志》, vol. 9, no. 2, 30 April 2003 (2003-04-30), pages 3 - 5 * |
| 王坤: "益母草罐组式动态逆流提取工艺研究", 《安徽中医学院学报》, vol. 19, no. 5, 31 October 2000 (2000-10-31), pages 46 - 47 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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