CN1374300A

CN1374300A - Resin process of eliminating ginkgolic acid from gingko leaf extractive

Info

Publication number: CN1374300A
Application number: CN 02113529
Authority: CN
Inventors: 张迪清; 何珺; 何照范; 邓秀兴; 张天常; 黄英
Original assignee: GUIZHOU BIO-CHEMICAL ENGINEERING CENTER
Current assignee: GUIZHOU BIO-CHEMICAL ENGINEERING CENTER
Priority date: 2002-03-26
Filing date: 2002-03-26
Publication date: 2002-10-16

Abstract

The resin process of eliminating ginkgolic acid from gingko leaf extractive consists of the steps of resin processing, depuration and eliminating ginkgolic acid, and resin regeneration. The step of depuration and eliminating ginkgolic acid includes mixing gingko leaf extractive with alcohol while stirring, filtering, adding distilled water to the filtrate, letting stand to separate partial deposit, filtering and treating with macroporous resin column. Compared with available technology, the present invention has very simple technological process to separate gingkolic acid from gingko leaf extractive and to raise the quality of gingko leaf extractive. The process of the present invention has been applied in industrial trial production.

Description

From Folium Ginkgo extract, take off the technology of ginkgoic acid with resin method

The present invention is a kind of technology of taking off ginkgoic acid with resin method from Folium Ginkgo extract, belongs to the field of biochemical engineering technology

From Ginkgo Leaf, extract active substance----ginkgo GBE and be used for health care, treatment of human body etc., can guarantee that in the domestic extraction process technology of China the content that extracts can meet or exceed international most advanced level at present; But this wherein has a fatal especially problem, the too high levels of ginkgoic acid in extract, because the toxic side effect of ginkgoic acid is big, can influence health care, the result of treatment of Semen Ginkgo extrac, influence the outlet and the product price of product, do not finish fully as yet for the research of from Folium Ginkgo extract, taking off ginkgoic acid in the prior art, so effectively bibliographical information is also fewer.

The objective of the invention is to: a kind of technology of taking off ginkgoic acid with resin method from Folium Ginkgo extract is provided, this technology can be on relatively simple basis, most economical separates ginkgoic acid from Folium Ginkgo extract, thereby guarantees the quality of Folium Ginkgo extract.

The present invention constitutes like this: it is made of plastic resin treatment, impurity elimination depickling, these several procedures of resin regeneration, wherein the impurity elimination deacidification process is performed such: get Folium Ginkgo extract, add dissolution with solvents, filter then, add the distilled water of certain volume in the filtrate, place, separate out partly precipitated thing after-filtration after the stirring, cross macroporous resin column, cross post with distilled water again, collect effluent liquid, must take off the product of ginkgoic acid after effluent liquid is evaporated, concentrates; Specifically: it is by plastic resin treatment, the impurity elimination depickling, these several procedures of resin regeneration constitute, wherein the impurity elimination deacidification process is performed such: get Folium Ginkgo extract 2-20 kilogram, adding solvent 100L stirs, filter then, lixiviate is once again for filter residue, the distilled water that adds 2-10 times of volume in the filtrate, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, cross macroporous resin column, cross post in every 1-3 kilogram Folium Ginkgo extract with the ratio of 1L resin with 50-150L distilled water again, collect effluent liquid, it is evaporated, must take off the product of ginkgoic acid after concentrating; More particularly: it is by plastic resin treatment, the impurity elimination depickling, these several procedures of resin regeneration constitute, the plastic resin treatment operation adopts prior art that commercially available resin is handled, it is standby in the glass chromatography column to pack into then, concrete impurity elimination deacidification process is performed such: get 10 kilograms of Folium Ginkgo extracts, add entry, organic solvent or its mixture 100L stirred 15 minutes, filter then, the distilled water that adds 300L in the filter residue lixiviate first-time filtrate again stirs the back and placed 12 hours, separates out partly precipitated thing after-filtration, cross post, the volume of its center pillar is 50L, crosses post with 100L distilled water again, collects effluent liquid, with film under vacuum evaporator evaporation alcohol and water, it is dry that concentrated solution is put into Minton dryer, and wherein vacuum tightness is-0.07--0.08MPa, and temperature is 60 degree Celsius, pulverize, must take off the product of ginkgoic acid excessively behind 80 mesh sieves.

Compared with prior art: technology of the present invention is simple especially, the equipment, the starting material that need are easily got and are easy to get, and are with low cost, can be on relatively simple basis, most economical separates ginkgoic acid from Folium Ginkgo extract, thereby guarantee the quality of Folium Ginkgo extract, the present invention utilizes the saturation characteristic of polymeric adsorbent to take off ginkgoic acid, and promptly extract solution is crossed a spot of resin column, because of resin reaches supersaturation, effective ingredient flows out, and ginkgoic acid is retained in the post, and reaches the purpose of depickling.

Embodiments of the invention 1: it is by plastic resin treatment, the impurity elimination depickling, these several procedures of resin regeneration constitute, the plastic resin treatment operation adopts prior art that commercially available macroporous resin is handled, it is standby in the chromatography column to pack into then, specifically be such: get macroporous resin, soaked 48 hours, it is standby to select 20-60 purpose resin with sub-sieve at the washing screen of the tap water of crossing the 0.45um microporous membrane, get 200 kilograms of 20-60 purpose resins, clean repeatedly to nearly neutrality with distilled water, the hydrochloric acid 30L that adds 4mol/l, soaked 4 hours, be washed till nearly neutrality with distilled water, add 80% ethanol 40L, soak and clean repeatedly to alcohol-free smell with distilled water after 10 hours, stand-by with distilled water immersion, as to pack into and handled well macroporous resin; Concrete impurity elimination deacidification process is performed such: get 10 kilograms of Folium Ginkgo extracts, the alcohol 100L of adding 95% stirred 15 minutes, filter then, filter residue is again with 95% alcohol 50L dissolving, refilter, the distilled water that adds 300L in the filtrate, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, cross macroporous resin column, cross post with 100L distilled water again, cross post in every 1-3 kilogram Folium Ginkgo extract with the ratio of 1L resin, at this time, acid is stayed in the post, and effective ingredient flows out, collect effluent liquid, with film under vacuum evaporator evaporation alcohol and water, it is dry that concentrated solution is put into Minton dryer, and wherein vacuum tightness is-0.07--0.08MPa, and temperature is 60 degree Celsius, pulverize, must take off the product of ginkgoic acid excessively behind 80 mesh sieves.

Embodiments of the invention 2: it is made of plastic resin treatment, impurity elimination depickling, these several procedures of resin regeneration, wherein the impurity elimination deacidification process is performed such: get 2 kilograms of Folium Ginkgo extracts, adding entry 100L stirs, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, commercially available excessively macroporous resin column is crossed post with 50L distilled water again, collect effluent liquid, must take off the product of ginkgoic acid after it is evaporated, concentrates.

Embodiments of the invention 3: it is made of plastic resin treatment, impurity elimination depickling, these several procedures of resin regeneration, wherein the impurity elimination deacidification process is performed such: get 20 kilograms of Folium Ginkgo extracts, adding organic solvent 100L stirs, filter then, filter residue again with identical dissolving, refilter, the distilled water that adds 10 times of volumes in the filtrate, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, cross macroporous resin column, cross post with 100L distilled water again, collect effluent liquid, must take off the product of ginkgoic acid after it is evaporated, concentrates.

Claims

1, a kind of technology of from Folium Ginkgo extract, taking off ginkgoic acid with resin method, it is characterized in that: it is made of plastic resin treatment, impurity elimination depickling, these several procedures of resin regeneration, wherein the impurity elimination deacidification process is performed such: get Folium Ginkgo extract, add dissolution with solvents, filter then, the distilled water that adds certain volume in the filtrate, place, separate out partly precipitated thing after-filtration after the stirring, cross macroporous resin column, cross post with distilled water again, collect effluent liquid, must take off the product of ginkgoic acid after effluent liquid is evaporated, concentrates.

2, according to the described this technology of from Folium Ginkgo extract, taking off ginkgoic acid with resin method of claim 1, it is characterized in that: it is by plastic resin treatment, the impurity elimination depickling, these several procedures of resin regeneration constitute, wherein the impurity elimination deacidification process is performed such: get Folium Ginkgo extract 2-20 kilogram, adding solvent 100L stirs, filter then, lixiviate is once again for filter residue, the distilled water that adds 2-10 times of volume in the filtrate, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, cross macroporous resin column, cross post in every 1-3 kilogram Folium Ginkgo extract with the ratio of 1L resin with 50-150L distilled water again, collect effluent liquid, it is evaporated, must take off the product of ginkgoic acid after concentrating.

3, according to claim 1,2 described this technologies of from Folium Ginkgo extract, taking off ginkgoic acid with resin method, it is characterized in that: it is by plastic resin treatment, the impurity elimination depickling, these several procedures of resin regeneration constitute, the plastic resin treatment operation adopts prior art that commercially available resin is handled, it is standby in the glass chromatography column to pack into then, concrete impurity elimination deacidification process is performed such: get 10 kilograms of Folium Ginkgo extracts, add entry, organic solvent or its mixture 100L stirred 15 minutes, filter then, the distilled water that adds 300L in the filter residue lixiviate first-time filtrate again, stirring the back placed 12 hours, separate out partly precipitated thing after-filtration, cross post, the volume of its center pillar is 50L, cross post with 100L distilled water again, collect effluent liquid, with film under vacuum evaporator evaporation alcohol and water, it is dry that concentrated solution is put into Minton dryer, wherein vacuum tightness is-0.07--0.08MPa, temperature is 60 degree Celsius, pulverizes, and must take off the product of ginkgoic acid excessively behind 80 mesh sieves.