CN104940252A - Method for extracting total flavonoids of gingko leaves - Google Patents
Method for extracting total flavonoids of gingko leaves Download PDFInfo
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- CN104940252A CN104940252A CN201510357616.9A CN201510357616A CN104940252A CN 104940252 A CN104940252 A CN 104940252A CN 201510357616 A CN201510357616 A CN 201510357616A CN 104940252 A CN104940252 A CN 104940252A
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Abstract
The invention discloses a method for extracting total flavonoids of gingko leaves. The method comprises the following steps: adding the gingko leaves in a mixed liquid of isopropanol and water, adding ammonium sulfate solids, placing the mixed liquid in a homogenate extraction device to perform homogenate processing, and after the homogenate is finished, performing standing layering, evaporation and drying. The method for extracting the total flavonoids of the gingko leaves shortens extracting time, improves extracting yield and purity and is simple to operate.
Description
Technical field
The present invention relates to extraction process technology field, particularly relate to a kind of method extracting Folium Ginkgo total flavones.
Background technology
Semen Ginkgo, has another name called maidenhair tree, Gong Sunshu, is China's endemic tree.The leaf of Semen Ginkgo, really, bark all can be used as medicine, and the medical value of You Yiye is the highest.The chemical composition of Folium Ginkgo is comparatively complicated, main containing flavone compound and diterpene-kind compound in its extract, there are expansion cardiovascular and cerebrovascular vessel, improve microcirculation, suppress the effects such as platelet aggregation, antioxidation, removing and suppression oxygen-derived free radicals, antiviral, anti-inflammation, endocrine regulation.The content of flavone compound in ginkgo biloba succi accounts for 5.91%, and its kind is flavone, flavanone, flavonol and catechin and two pyrite.The extracting method of existing Folium Ginkgo flavone compounds has organic solvent extraction, super critical point purification method, water extraction method, but all there is the high defect of cost.In view of unique physiological action, clinical treatment and health value that ginkgetin has, become one of focus of international and domestic research and development in recent years, therefore, the content constantly exploring new extraction process raising flavone compound has become the hot issue of people's concern.
Summary of the invention
The object of the invention is to solve the shortcoming existed in prior art, and a kind of method extracting Folium Ginkgo total flavones proposed, which shorten extraction time, improve extraction efficiency and purity, and simple to operate.
To achieve these goals, present invention employs following technical scheme:
Extract a method for Folium Ginkgo total flavones, comprise the following steps: added by Folium Ginkgo in the mixed liquor of the third alcohol and water, add ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, homogenate terminates rear stratification, evaporation, drying.
Preferably, in the mixed liquor of the third alcohol and water, propanol is 5-7:8-12 with the ratio of the volume of water.
Preferably, the mass ratio of described ammonium sulfate solids and Folium Ginkgo is 15-20:18-22.
Preferably, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 0.8-5min, and the interval of adjacent twice homogenate is 5-15s.
Preferably, the method of described extraction Folium Ginkgo total flavones, comprise the following steps: 18-22g Folium Ginkgo is added in beaker, add the mixed liquor of 55-65ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 5-7:8-12, add 15-20g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 0.8-5min, the interval of adjacent twice homogenate is 5-15s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 4-6h in exsiccator again.
Preferably, the method of described extraction Folium Ginkgo total flavones, comprise the following steps: 20g Folium Ginkgo is added in beaker, add the mixed liquor of 60ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 3:5, add 18g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 1min, the interval of adjacent twice homogenate is 10s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 5h in exsiccator again.
Homogenized refers to that biological tissue passes through to add Extraction solvent and carries out tissue homogenate or defibrination, to extract a kind of extracting method of effective ingredient in biological tissue.Application homogenate method extracts bioactive ingredients, can directly be placed in refiner by fresh material material, add solvent extracting directly.At present, application the method has report to the research that aminoacid, protein and terpene substances are extracted, but research the method being applied to flavones ingredient extraction aspect there is not yet bibliographical information.
Normal propyl alcohol-ammonium sulfate double-aqueous phase system refers to and add ammonium sulfate in water solublity propanol, utilizes the salting out of ammonium sulfate to form double-aqueous phase system, can be controlled the formation of double-aqueous phase system by the consumption changing propanol-water and salt.
In the present invention, according to the character of Flavonoid substances, phase on propanol is allocated in normal propyl alcohol-ammonium sulfate double-aqueous phase system, other water soluble ingredients as saccharide etc. be then allocated in salt under water mutually in, thus being separated of flavone and some invalid components is achieved while extracting, effectively improve the purity of product.Simultaneously, Flavonoid substances is transferred to phase on propanol, the chemical equilibrium in leaching process can be changed, be conducive to the stripping of effective ingredient, coordinate homogenized, be coupled with achieving homogenate and normal propyl alcohol-ammonium sulfate double-aqueous phase system, shorten extraction time greatly, improve productive rate and purity, and simple to operate.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
A kind of method extracting Folium Ginkgo total flavones, comprise the following steps: 22g Folium Ginkgo is added in beaker, add the mixed liquor of 55ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 7:12, add 20g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 5min, the interval of adjacent twice homogenate is 5s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 6h in exsiccator again.
Embodiment 2
A kind of method extracting Folium Ginkgo total flavones, comprise the following steps: 18g Folium Ginkgo is added in beaker, add the mixed liquor of 65ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 5:8, add 15g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 0.8min, the interval of adjacent twice homogenate is 15s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 4h in exsiccator again.
Embodiment 3
A kind of method extracting Folium Ginkgo total flavones, comprise the following steps: 20g Folium Ginkgo is added in beaker, add the mixed liquor of 60ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 3:5, add 18g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 1min, the interval of adjacent twice homogenate is 10s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 5h in exsiccator again.
The method and common ultrasonic method, microwave method and circumfluence method of extracting Folium Ginkgo total flavones described in embodiment 3 are compared, its result is as shown in the table:
| Extraction conditions | Extraction ratio (%) | |
| Embodiment 3 method | 5.28 | |
| Alcohol-water circumfluence method | 70% ethanol (solid-liquid ratio 1:10) reflux, extract, twice, first time 2h, second time 1h, merging filtrate, 60 DEG C of distilling under reduced pressure | 4.79 |
| Ultrasonic method | 70% ethanol (solid-liquid ratio 1:10) ultrasonic 30min, filters, distilling under reduced pressure | 4.52 |
| Microwave method | 70% ethanol (solid-liquid ratio 1:10) microwave 10min, filters, distilling under reduced pressure | 3.02 |
| Water extraction method | 2h is extracted in water (solid-liquid ratio 1:10) water-bath | 1.28 |
As seen from the above table, in the Folium Ginkgo of the method extraction of extraction Folium Ginkgo total flavones of the present invention, the yield of total flavones is the highest, and eliminate the step of material being dried, pulverizing, utilize comparatively simple equipment, and within the extremely short time, just can obtain higher yields and purity in a mild condition.
Claims (6)
1. one kind is extracted the method for Folium Ginkgo total flavones, it is characterized in that, comprise the following steps: Folium Ginkgo is added in the mixed liquor of the third alcohol and water, add ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, homogenate terminates rear stratification, evaporation, drying.
2. extract the method for Folium Ginkgo total flavones according to claim 1, it is characterized in that, in the mixed liquor of the third alcohol and water, propanol is 5-7:8-12 with the ratio of the volume of water.
3. extract the method for Folium Ginkgo total flavones according to claim 1, it is characterized in that, the mass ratio of described ammonium sulfate solids and Folium Ginkgo is 15-20:18-22.
4. extract the method for Folium Ginkgo total flavones according to claim 1, it is characterized in that, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 0.8-5min, and the interval of adjacent twice homogenate is 5-15s.
5. according to any one of claim 1-4, extract the method for Folium Ginkgo total flavones, it is characterized in that, comprise the following steps: 18-22g Folium Ginkgo is added in beaker, add the mixed liquor of 55-65ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 5-7:8-12, add 15-20g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 0.8-5min, the interval of adjacent twice homogenate is 5-15s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 4-6h in exsiccator again.
6. extract the method for Folium Ginkgo total flavones according to claim 5, it is characterized in that, comprise the following steps: 20g Folium Ginkgo is added in beaker, add the mixed liquor of 60ml third alcohol and water, wherein, in the mixed liquor of the third alcohol and water, the volume ratio of propanol and water is 3:5, add 18g ammonium sulfate solids, then put into homogenate extraction equipment and carry out homogenized, wherein, described homogenized comprises a homogenate, secondary homogenate and three homogenate, and the time of each homogenate is 1min, the interval of adjacent twice homogenate is 10s, homogenate terminates to be placed on stratification in separatory funnel, divide and remove normal propyl alcohol, then Rotary Evaporators is utilized to boil off normal propyl alcohol, vacuum drying 5h in exsiccator again.
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| CN104523771A (en) * | 2015-01-13 | 2015-04-22 | 中国药科大学 | Ginkgo leaf total flavones and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104523771A (en) * | 2015-01-13 | 2015-04-22 | 中国药科大学 | Ginkgo leaf total flavones and preparing method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 刘晓芳 等: "双水相-匀浆萃取法提取芒果核多酚工艺研究", 《云南民族大学学报：自然科学版》 * |
| 辜鹏: "无机盐/低分子有机物双水相体系的研究及其应用", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》 * |
| 那吉 等: "超声波协同丙醇-硫酸铵双水相体系提取灯盏花总黄酮的研究", 《化学与生物工程》 * |
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Application publication date: 20150930 |