CN102078342A - Preparation method of water-soluble ginkgo biloba extract (GBE) - Google Patents
Preparation method of water-soluble ginkgo biloba extract (GBE) Download PDFInfo
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Abstract
The invention relates to a preparation method of a water-soluble ginkgo biloba extract (GBE), which comprises the following steps: taking ginkgo biloba leaves as raw materials; adding ethanol and heating and refluxing; concentrating the extracting liquid, and recovering ethanol; treating through a macroporous resin column; desorbing with the ethanol; recovering the ethanol again; adding water for diluting, and then, adding gel-type hydrogen-bonded adsorption resin to collect effluent liquid and stripping liquid; and concentrating and drying to obtain a water-soluble GBE product meeting the standards. The product which is prepared by the method provided by the invention has the advantages of stable and controllable quality, simple production process and low cost, and toxic organic solvents are not used so that the process is environment-friendly. The obtained water-soluble GBE has stable and controllable quality and can be used in an injection preparation or an infusion preparation of ginkgo biloba products.
Description
Technical field
The present invention relates to a kind of preparation method of water-soluble gingko extract,, belong to the technical field of fine chemistry industry in particular to the production technology of from Folium Ginkgo, extracting the water-soluble gingko extract that meets national standard.
Background technology
Semen Ginkgo (Ginkgo biloba L.) is a kind of important medicinal plants, and Folium Ginkgo is the leaf of Ginkgoaceae plant Ginkgo biloba, and its bitter and puckery flavor, property are put down, and Ginkgo total flavones that it is contained and terpene lactones have important medical value.But also there are some harmful materials in the Folium Ginkgo, as ginkgoic acid.Therefore, how enriching ginkgetin and terpene lactones from Folium Ginkgo are removed ginkgoic acid simultaneously to greatest extent, are once becoming the focus of research.The seventies in last century, Germany takes the lead in having formulated quality standard, i.e. standard silver Fructus Pruni extract (Ginkgo total flavones 〉=24%, terpene lactones 〉=6% for Semen Ginkgo extrac (being called for short GBE), ginkgoic acid≤10ppm), this standard and then also become the international international standard of Semen Ginkgo extrac.The appearance of this standard was once limiting China GBE production greatly.Also promote China to produce the innovation of GBE technology.There have been tens of to produce GBE technology patent at present.But most productions that are limited to common Semen Ginkgo extrac.Production technology about water-soluble gingko extract mainly contains following: CN 02113533.9 adopts double suction attached column method to produce water solublity GBE, do not mention concrete water solublity index in the patent, the application of ion exchange resin simultaneously, also caused infringement to environment, the increase of processing step, both increase cost, also reduced yield.It is raw material that CN1772009A adopts the GBE crude product, adopts multistep precipitation, filtration steps such as gelatin, ethanol.Make so-called water solublity GBE.Mentioned the employing anhydrous alcohol solution, steps such as vacuum hot-air dry in this patent process.In this patent working process, be subjected to the restriction of raw material sources quality, underproof product (having added rutin or Quercetin in the raw material) is difficult to produce qualified water solublity GBE.
In a word, the water-soluble gingko extract extensive market is especially aspect gingko injection or infusion solutions Products Development.The crucial production technology of water solublity GBE product still remains further ripe, invent a kind of simply, production technology efficiently, will have vast market value and great social significance.
Summary of the invention
Purpose of the present invention just is to provide a kind of preparation method of water-soluble gingko extract.It is a kind of simple, reliable, is the water solublity GBE production technology that meets state-promulgated pharmacopoeia (2010 editions) standard of raw material with the Folium Ginkgo.
Purpose of the present invention can realize by following technical scheme: this method is raw material with the Folium Ginkgo, extract with the lixiviate of alcoholic solution reflux, extracting solution concentrates and reclaims ethanol, crosses macroporous resin column and separates alcohol desorption, reclaim ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up by adding gel-type hydrogen bonding adsorption resin, is collected effluent and stripping liquid again, concentrated, dry, promptly obtain water solublity GBE product.
In the said extracted process, the alcoholic acid mass fraction of lixiviate is 30-90%, preferred 50-80%.Extraction temperature is 20-90 ℃, and the lixiviate number of times is 2 times, each 0.5-3 hour.
In the above-mentioned absorption-desorption process, the post of adsorption column is directly than being 3-10: 1, the weight ratio of resin and Folium Ginkgo is 0.5-3: 1, the absorption and the flow velocity of desorbing be 0.5-3BV/H (BV: bed volume, H: hour).Stripping liquid is the ethanol water of 10-90%, preferred 50-70%.
Used macroporous resin is for being macroporous resin FL-2, AB-8 or the D101 of main skeleton with styrene in the described separation process.
Described gel-type adsorbent resin is MG-1, MG-2.
The resulting high-purity ginkgetin of the present invention, be the sundown powder, mildly bitter flavor, ginkgetin 〉=50%, Quercetin and kaempferol peak are than between the 0.8--1.2, and isorhamnetin and Quercetin peak compare 〉=0.15, ginkgoic acid＜1ppm, residue on ignition＜0.8%, water content＜5.0%, dissolubility: 5 grams/100 ml waters.The injection or the transfusion dosage form that can be used as the Semen Ginkgo extrac medicine are used.
The present invention does from the source, thereby has guaranteed the stable and controllable of products obtained therefrom quality.The production technology of this water solublity GBE is simple, and cost is low, does not use toxic organic solvent in the process, is a kind of environmentally friendly technology.Resulting water solublity GBE is stable and controllable for quality, and quality index such as water solublity meet Chinese Pharmacopoeia (2010 editions) requirement fully.The injection or the transfusion dosage form that can be used as the Semen Ginkgo product are used.
The specific embodiment
Can further specify the present invention below in conjunction with embodiment:
Embodiment 1
1, the extraction of Folium Ginkgo: get the 400g Folium Ginkgo, add for the first time the ethanol water (2000ml) of 5 times of amounts 80%, 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600ml) of 4 times of amounts 80% for the second time, 70 ℃ of reflux, extract, 3 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 4 hours, filtered, and must clarify extracting solution.
2, separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (600g) (Tianjin Ourui Biology Technology Co., Ltd., public offering), resin column is directly than 7: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400ml) desorbing of 4BV70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, gets paste GBE product.
3, the preparation of water solublity GBE: above-mentioned paste GBE thin up to 400ml, is fed MG-2 (200g) resin column (Tianjin Ourui Biology Technology Co., Ltd. provides, public offering), and resin column is directly than 10: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400ml) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, collects effluent, uses 70% ethanol water desorbing then, merges stripping liquid and effluent, concentrates, and vacuum drying promptly gets standard water dissolubility GBE product.
4, standard water dissolubility GBE product (is measured) the water-soluble gingko extract standard that meets the state-promulgated pharmacopoeia regulation after testing according to official method.
Embodiment 2
1, the extraction of Folium Ginkgo: get the 400kg Folium Ginkgo, add for the first time the ethanol water (2000L) of 5 times of amounts 80%, 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600L) of 4 times of amounts 80% for the second time, 70 ℃ of reflux, extract, 3 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 4 hours, filtered, and must clarify extracting solution.
2, separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (600kg) (Tianjin Ourui Biology Technology Co., Ltd.), resin column is directly than 7: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400L) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, gets paste GBE product.
3, the preparation of water solublity GBE: above-mentioned paste GBE thin up to 400L, is fed MG-2 (200kg) resin column (Tianjin Ourui Biology Technology Co., Ltd. provides), and resin column is directly than 10: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (2400L) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, connects effluent, uses 70% ethanol water desorbing then, merges stripping liquid and effluent, concentrates, and vacuum drying promptly gets standard water dissolubility GBE product.
4, standard water dissolubility GBE product meets the water-soluble gingko extract standard of state-promulgated pharmacopoeia regulation after testing.
Embodiment 3
1, the extraction of Folium Ginkgo: get the 400kg Folium Ginkgo, add for the first time the ethanol water (2000L) of 5 times of amounts 50%, 70 ℃ of reflux, extract, 3 hours add the ethanol water (1600L) of 4 times of amounts 50% for the second time, 70 ℃ of reflux, extract, 2 hours.Merge extracted twice liquid, reclaim ethanol, thin up left standstill 6 hours, filtered, and must clarify extracting solution.
2, separation and purification: will go up step gained extracting solution and feed adsorption resin column FL-2 (400kg) (Tianjin Ourui Biology Technology Co., Ltd.), resin column is directly than 12: 1, and the absorption flow velocity is 1BV/H.After absorption finishes, with ethanol water (1600L) desorbing of 4BV 70%, flow velocity 1BV/H.Stripping liquid reclaims ethanol, obtains standard GBE (poorly water-soluble) powder after vacuum or the spray drying.
3, the preparation of water solublity GBE: above-mentioned paste GBE thin up to 200L, is fed MG-1 (200kg) resin column (Tianjin Ourui Biology Technology Co., Ltd. provides), and resin column is directly than 10: 1, and the absorption flow velocity is 2BV/H.Connect effluent, after absorption finishes, with ethanol water (1500L) desorbing of 4BV 50%, flow velocity 2BV/H.Merge stripping liquid and effluent, concentrate, vacuum drying promptly gets standard water dissolubility GBE product.
4, standard water dissolubility GBE product meets the water-soluble gingko extract standard of state-promulgated pharmacopoeia regulation after testing.
Claims (7)
1. the preparation method of a water-soluble gingko extract, it is characterized in that it is is raw material with the Folium Ginkgo, with the lixiviate of alcoholic solution reflux, extracting solution concentrates and reclaims ethanol, crossing macroporous resin column separates, alcohol desorption reclaims ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up, again by adding gel-type hydrogen bonding adsorption resin, collect effluent and stripping liquid, concentrated, dry, promptly obtain water solublity GBE product.
2. in accordance with the method for claim 1, the mass fraction that it is characterized in that the alcoholic solution that described lixiviate is used is 30-90%.
3. in accordance with the method for claim 2, the mass fraction that it is characterized in that the alcoholic solution that described lixiviate is used is 50-80%
4. in accordance with the method for claim 1, it is characterized in that macroporous resin used in the described separation process is for being macroporous resin FL-2, AB-8 or the D101 of main skeleton with styrene.
5. in accordance with the method for claim 1, it is characterized in that described gel-type adsorbent resin is MG-1, MG-2.
6. in accordance with the method for claim 1, it is characterized in that being used for the consumption of isolating resin and the mass ratio of raw material is 0.5-3: 1; Extraction temperature is 20-90 ℃, and the lixiviate number of times is 2 times, each 0.5-3 hour.
7. in accordance with the method for claim 1, it is characterized in that the described alcoholic solution mass fraction that is used for desorbing is the alcoholic solution of 50-70%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293790A (en) * | 2011-07-26 | 2011-12-28 | 天津泰阳制药有限公司 | High purity ginkgolide composition |
| CN102772452A (en) * | 2012-08-17 | 2012-11-14 | 天津泰阳制药有限公司 | Method for producing ultra-low-acid ginkgo leaf extract |
| CN106235260A (en) * | 2016-08-19 | 2016-12-21 | 中盐新干盐化有限公司 | A kind of preparation method of food curing salt |
| CN106262668A (en) * | 2016-08-10 | 2017-01-04 | 中盐新干盐化有限公司 | A kind of preparation method of bacon salt |
| CN116899271A (en) * | 2023-09-14 | 2023-10-20 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293790A (en) * | 2011-07-26 | 2011-12-28 | 天津泰阳制药有限公司 | High purity ginkgolide composition |
| CN102772452A (en) * | 2012-08-17 | 2012-11-14 | 天津泰阳制药有限公司 | Method for producing ultra-low-acid ginkgo leaf extract |
| CN106262668A (en) * | 2016-08-10 | 2017-01-04 | 中盐新干盐化有限公司 | A kind of preparation method of bacon salt |
| CN106235260A (en) * | 2016-08-19 | 2016-12-21 | 中盐新干盐化有限公司 | A kind of preparation method of food curing salt |
| CN116899271A (en) * | 2023-09-14 | 2023-10-20 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
| CN116899271B (en) * | 2023-09-14 | 2023-12-12 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
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Application publication date: 20110601 |