CN102727538B - Process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves - Google Patents
Process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves Download PDFInfo
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- CN102727538B CN102727538B CN201210152676.3A CN201210152676A CN102727538B CN 102727538 B CN102727538 B CN 102727538B CN 201210152676 A CN201210152676 A CN 201210152676A CN 102727538 B CN102727538 B CN 102727538B
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Abstract
The present invention discloses a process for extracting ginkgo biloba flavone, ginkgo biloba lactone and ginkgo biloba phenolic acid from ginkgo biloba leaves. The process comprises the following steps: (1) carrying out a pretreatment on ginkgo biloba leaves; (2) carrying out extraction by an ultrasonic device; (3) carrying out reduced pressure concentration; (4) loading the resulting solution on a macroporous resin to carry out a treatment; (5) collecting the resulting eluate; (6) carrying out reduced pressure concentration; (7) detecting the resulting extract; and (8) carrying out drying and storing on the extract. With the process of the present invention, the ginkgo biloba flavone content and the ginkgo biloba lactone content in the extract prepared by the process of the present invention are high, the loss of active ingredients are avoided, the production process is simplified, the production cycle is shortened, and the ginkgo biloba phenolic acid content after treatment is substantially reduced.
Description
Technical field
The present invention relates to a kind of technique of extract from Folium Ginkgo, particularly relate to a kind of technique extracting ginkgetin, bilobalide and gingkolic acid from Folium Ginkgo.
Background technology
Ginkgoaceae plant Ginkgo biloba (
ginkgo biloba) be the endemic tree of China, containing effective ingredient such as flavonoid (about more than 20 plant), terpenoid, phenols, healthy trace elements with household and 17 seed amino acids in Folium Ginkgo.Current Folium Ginkgo extract has been developed to medicine, health product and cosmetics in countries such as U.S., day, moral, meaning, Korea Spro, and China has also started the upsurge to Ginkgo developing and research.Domestic existing hundreds of manufacturer production Semen Ginkgo dry extract, and in succession have Folium Ginkgo goods to put goods on the market.
The materials such as the rare a large amount of ginkgetin of Folium Ginkgo extract and bilobalide, it can increase cerebrovascular flow, improves Cerebrovascular disorders function; protection brain cell, coronary artery dilator, prevents angina pectoris and myocardial infarction; prevent thrombosis, improve body immunity.Very useful per capita to coronary heart diseases and angina pectoris, cerebral arteriosclerosis, alzheimer disease, hypertension.
In traditional leaching process, solvent easily or faster enters cell under the condition of heating, but solable matter is higher at the condition dissolubility of heat, successively occurred very high osmotic pressure by dissolving, cause extraction ratio low, active component is low, and technique is loaded down with trivial details, the production cycle is long.
Summary of the invention
In order to overcome above-mentioned defect, the invention provides a kind of technique extracting the extract such as ginkgetin and bilobalide from Folium Ginkgo effectively, at a high speed.
The present invention in order to the technical scheme solving its technical problem and adopt is: a kind of technique extracting ginkgetin, bilobalide and gingkolic acid from Folium Ginkgo, and take Folium Ginkgo as raw material, its processing step comprises:
(1) process in early stage is carried out to Folium Ginkgo: be crushed to Powdered after dry Folium Ginkgo is air-dry;
(2) ultrasonic extraction is passed through, by raw material with extract solvent with 1:10(g/mL) solid-liquid ratio fully mix after, described extraction solvent is water or low-carbon alcohols, in 70KHz frequency, at the temperature of 25 DEG C, extraction is carried out 25 minutes to feed liquid, extract 1 ~ 2 time, each time of extracting is 25 minutes, filtration, merging filtrate after extracting;
(3) concentrating under reduced pressure: the extracting solution in step (2) is put into Rotary Evaporators concentrating under reduced pressure, temperature controls 45 ~ 55 DEG C, and vacuum degree control is at 0.1MPa, and concentrated volume is to 1/10 of original volume;
(4) macroporous resin treatment is entered: after the extracting liquid filtering after concentrated in step (3), directly enter macroporous resin and process;
(5) eluent is collected: collect from the effluent macroporous resin column and the eluent through concentration alcohol-water solution eluting from low to high;
(6) concentrating under reduced pressure: the eluent in step (5) is carried out concentrating under reduced pressure, is concentrated into 1/10 of original volume;
(7) Detection and Extraction thing: with the content of ginkgetin, bilobalide and the phenolic acid in high performance liquid chromatography (HPLC) Detection and Extraction thing; the method wherein detecting ginkgetin, bilobalide and gingkolic acid content is respectively: the detection method of ginkgetin is: mobile phase: methanol: phosphoric acid: water=57:0.2:42.8; flow velocity is 1.0ml/min; determined wavelength is 370nm; chromatographic column temperature: 25 DEG C, sample size: 20 μ L; The detection method of bilobalide is: mobile phase is methanol: water=25:75, flow velocity 1.0mL/min, and detector is ELSD; Gingkolic acid detection method is: methanol: water=90:10, and flow velocity is 1.0mL/min, and determined wavelength is 310nm;
(8) extract extracted through above-mentioned steps is carried out stored dry, so far whole processing step completes.
As a further improvement on the present invention, described low-carbon alcohols is methanol, and the volumetric concentration of described low-carbon alcohols is 75%.
The invention has the beneficial effects as follows: the present invention carries out solvent extraction by hyperacoustic method, not only serve the effect of stirring and auxiliary heating, the more important thing is ultrasound wave extract in solvent " cavitation effect " that produce and mechanism one side can the cell wall of broken medical material effectively, make effective ingredient be free state and dissolve in extract in solvent, the molecular motion of extracting solvent can be accelerated on the other hand, make to extract the effective ingredient Rapid contact in solvent and medical material, mutually fused, mixing, the effect that each point in sample media is subject to is consistent, make whole sample extraction evenly, the leaching accelerating active ingredients of plants is extracted, improve extraction ratio, make ginkgetin and bilobalide content in extract high, avoid the loss of active component, simplify production technology, shorten the production cycle, simultaneously the content of gingkolic acid after treatment greatly reduces.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
(1) process in early stage is carried out to Folium Ginkgo: after dry Folium Ginkgo is air-dry, be crushed to powder;
(2) raw material and water are put into extraction pot in 1:10 ratio, utilize ultrasound wave to extract, the ultrasound works frequency of ultrasonic extraction is 70KHz, 25 minutes extraction times, filters, and mends and adds water to original volume, continues supersound extraction 25 minutes, filters, merging filtrate;
(3) concentrating under reduced pressure: extracting solution is put into Rotary Evaporators concentrating under reduced pressure, temperature controls 55 DEG C, and vacuum degree control is at 0.1MPa, and concentrated volume is to 1/10 of original volume;
(4) macroporous resin treatment is entered: after the extracting liquid filtering after concentrated in step (3), directly enter macroporous resin and process;
(5) eluent is collected: collect from the effluent macroporous resin column and the eluent through concentration alcohol-water solution eluting from low to high;
(6) concentrating under reduced pressure: the eluent in step (5) is carried out concentrating under reduced pressure, is concentrated into 1/10 of original volume;
(7) be respectively by the method for ginkgetin, bilobalide and gingkolic acid content in high performance liquid chromatography (HPLC) Detection and Extraction thing: the detection method of ginkgetin is: mobile phase: methanol: phosphoric acid: water=57:0.2:42.8; flow velocity is 1.0ml/min; determined wavelength is 370nm; chromatographic column temperature: 25 DEG C, sample size: 20 μ L; The detection method of bilobalide is: mobile phase is methanol: water=25:75, flow velocity 1.0mL/min, and detector is ELSD; Gingkolic acid detection method is methanol: water=90:10, and flow velocity is 1.0mL/min, and determined wavelength is 310nm;
(8) extract extracted through above-mentioned steps is carried out stored dry, so far whole processing step completes.
Embodiment 2
(1) process in early stage is carried out to Folium Ginkgo: be crushed to Powdered after dry Folium Ginkgo is air-dry;
(2) supersound extraction, the methanol being 75% by raw material and volumetric concentration puts into extraction pot in 1:10 ratio, ultrasound wave is utilized to extract, the ultrasound works frequency of ultrasonic extraction is 70KHz, 25 minutes extraction times at 25 DEG C, filters, add methanol to original volume, continue supersound extraction 25 minutes, filter, merging filtrate;
(3) concentrating under reduced pressure: extracting solution is put into Rotary Evaporators concentrating under reduced pressure, temperature controls 45 DEG C, and vacuum degree control is at 0.1MPa, and concentrated volume is to 1/8 of original volume;
(4) macroporous resin treatment is entered: after the extracting liquid filtering after concentrated in step (3), directly enter macroporous resin and process;
(5) eluent is collected: collect from the effluent macroporous resin column and the eluent through concentration alcohol-water solution eluting from low to high;
(6) concentrating under reduced pressure: the eluent in step (5) is carried out concentrating under reduced pressure, is concentrated into 1/10 of original volume;
(7) be respectively by the method for ginkgetin, bilobalide and gingkolic acid content in high performance liquid chromatography (HPLC) Detection and Extraction thing: the detection method of ginkgetin is: mobile phase: methanol: phosphoric acid: water=57:0.2:42.8; flow velocity is 1.0ml/min; determined wavelength is 370nm; chromatographic column temperature: 25 DEG C, sample size: 20 μ L; The detection method of bilobalide is: mobile phase is methanol: water=25:75, flow velocity 1.0mL/min, and detector is ELSD; Gingkolic acid detection method is methanol: water=90:10, and flow velocity is 1.0mL/min, and determined wavelength is 310nm;
(8) extract extracted through above-mentioned steps is carried out stored dry, so far whole processing step completes.
?through the realization of the above embodiments, the Semen Ginkgo extrac active constituent content obtained by method provided by the invention is high, the content measuring ginkgetin in extract by high performance liquid chromatography (HPLC) is 25 ~ 30%, extract raising 5 ~ 10% than traditional heat, the bilobalide simultaneously in extract has also brought up to 8 ~ 12%., time extract ginkgoic acid after treatment content have dropped 0.0020 ~ 0.0030% than traditional extraction process, content reaches 0.0010 ~ 0.0015%.The loss that the present invention sends out the Folium Ginkgo extract ginkgetin that obtains and bilobalide content is high, avoid active component, simplifies production technology, shortens the production cycle.
Claims (2)
1. from Folium Ginkgo, extract a technique for ginkgetin, bilobalide and gingkolic acid, it is characterized in that: take dry Folium Ginkgo as raw material, its processing step comprises:
(1) process in early stage is carried out to Folium Ginkgo: be crushed to by dry Folium Ginkgo Powdered;
(2) ultrasonic extraction is passed through, by raw material with extract solvent with 1:10(g/mL) solid-liquid ratio fully mix after, described extraction solvent is water or low-carbon alcohols, in 70KHz frequency, at the temperature of 25 DEG C, feed liquid is carried out, extract 1 ~ 2 time, each time of extracting is 25 minutes, filtration, merging filtrate after extracting;
(3) concentrating under reduced pressure: the extracting solution in step (2) is put into Rotary Evaporators concentrating under reduced pressure, temperature controls 45 ~ 55 DEG C, and vacuum degree control is at 0.1MPa, and concentrated volume is to 1/10 of original volume;
(4) macroporous resin treatment is entered: after the extracting liquid filtering after concentrated in step (3), directly enter macroporous resin and process;
(5) eluent is collected: collect from the effluent macroporous resin column and the eluent through concentration alcohol-water solution eluting from low to high;
(6) concentrating under reduced pressure: the eluent in step (5) is carried out concentrating under reduced pressure, is concentrated into 1/10 of original volume;
(7) Detection and Extraction thing: with the content of ginkgetin, bilobalide and the phenolic acid in high performance liquid chromatography (HPLC) Detection and Extraction thing; the method wherein detecting ginkgetin, bilobalide and gingkolic acid content is respectively: the detection method of ginkgetin is: mobile phase: methanol: phosphoric acid: water=57:0.2:42.8; flow velocity is 1.0ml/min; determined wavelength is 370nm; chromatographic column temperature: 25 DEG C, sample size: 20 μ L; The detection method of bilobalide is: mobile phase is methanol: water=25:75, flow velocity 1.0mL/min, and detector is ELSD; Gingkolic acid detection method is: methanol: water=90:10, and flow velocity is 1.0mL/min, and determined wavelength is 310nm;
(8) extract extracted through above-mentioned steps is carried out stored dry, so far whole processing step completes.
2. the technique extracting ginkgetin, bilobalide and gingkolic acid from Folium Ginkgo according to claim 1, is characterized in that: described low-carbon alcohols is methanol, and the volumetric concentration of low-carbon alcohols is 75%.
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| CN103463145B (en) * | 2013-08-05 | 2015-09-02 | 南京中医药大学 | The Folium Ginkgo being raw material with Semen Ginkgo fallen leaves refines extract and preparation method thereof and application |
| CN104593182A (en) * | 2014-12-30 | 2015-05-06 | 东莞市高明企业服务有限公司 | Natural plant extract scrubbing solution and preparation method thereof |
| CN106568872A (en) * | 2016-10-30 | 2017-04-19 | 徐志扬 | Preparation method of ginkgo leaf extract and determination method of effective components |
| CN109939131B (en) | 2017-12-20 | 2021-07-20 | 上海上药杏灵科技药业股份有限公司 | Preparation method and application of high-purity ginkgo total flavonol glycosides |
| CN108721346A (en) * | 2018-06-19 | 2018-11-02 | 安徽省百禾农业科技发展有限公司 | A kind of ginkgo flavone extraction method |
| CN108703981B (en) * | 2018-07-09 | 2021-04-13 | 湖北工程学院 | Method for extracting ginkgetin from ginkgo leaves |
| CN110585251A (en) * | 2019-10-21 | 2019-12-20 | 西安工程大学 | Method for extracting ginkgetin by using n-butanol |
| CN112494524A (en) * | 2020-12-24 | 2021-03-16 | 海南海力制药有限公司 | Method for preparing ginkgo leaf dispersible tablets |
| CN115112783A (en) * | 2022-03-01 | 2022-09-27 | 江苏康缘药业股份有限公司 | Ginkgo leaf detection method and construction and application of fingerprint spectrum with simultaneous reflection of multiple components |
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