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.