CN111214503A - Method for extracting ginkgetin from ginkgo leaves - Google Patents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A—HUMAN NECESSITIES
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses a method for extracting ginkgetin from ginkgo leaves, which comprises the following steps: (1) performing early-stage treatment on the ginkgo leaves; (2) carrying out ultrasonic device extraction; (3) concentrating under reduced pressure; (4) treating with macroporous resin; (5) collecting the eluent; (6) concentrating under reduced pressure; (7) detecting the extract; (8) drying and storing the extract obtained by the above steps. The extract obtained by the invention has high content of ginkgetin and bilobalide, avoids the loss of active ingredients, simplifies the production process, shortens the production period, and greatly reduces the content of the treated ginkgolic acid.
Description
Technical Field
The invention relates to a process for extracting ginkgo flavone from ginkgo leaves, in particular to a method for extracting ginkgo flavone from ginkgo leaves.
Background
Ginkgo of Ginkgoaceae (Ginkgo biloba L.) (Ginkgobiloba) Is a special tree species in China, and the ginkgo leaves contain effective components such as flavonoid (about 20 or more species), terpenoids, phenols, beneficial trace elements, 17 amino acids and the like. At present, ginkgo biloba extracts are developed into medicines, health care products and cosmetics in the countries of America, Japan, Germany, Italian, Korea and the like, and China also raises the hot trend of development and research of ginkgo biloba. Several hundreds of manufacturers have produced dry ginkgo extract in China, and ginkgo leaf products are put on the market successively.
The folium Ginkgo extract rarely contains a large amount of ginkgetin and bilobalide, and has effects of increasing cerebral blood vessel flow, improving cerebral blood vessel circulation function, protecting brain cells, dilating coronary artery, preventing angina pectoris and myocardial infarction, preventing thrombosis, and improving immunity. Is beneficial to patients with coronary heart disease, angina pectoris, cerebral arteriosclerosis, senile dementia and hypertension.
In the traditional extraction process, a solvent easily or more quickly enters cells under the heating condition, but soluble substances have higher solubility under the heating condition and are dissolved successively to generate high osmotic pressure, so that the extraction rate is low, the active ingredients are low, the process is complicated, and the production period is long.
Disclosure of Invention
In order to overcome the defects, the invention provides an effective and high-speed process for extracting ginkgo flavone and bilobalide and other extracts from ginkgo leaves.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for extracting ginkgetin from folium Ginkgo comprises the following steps:
(1) carrying out pretreatment on the ginkgo leaves: air drying dry folium Ginkgo, and pulverizing into powder;
(2) extracting with ultrasonic wave, mixing the raw material with extraction solvent in a ratio of 1: after fully mixing 10 (g/mL) of material-liquid ratio, extracting the material liquid for 25 minutes at the frequency of 70KHz and the temperature of 25 ℃ by using an extraction solvent which is water or low-carbon alcohol for 1-2 times, wherein the extraction time is 25 minutes each time, filtering after extraction, and combining the filtrates;
(3) and (3) concentrating under reduced pressure: putting the extracting solution obtained in the step (2) into a rotary evaporator, and concentrating under reduced pressure, wherein the temperature is controlled to be 45-55 ℃, the vacuum degree is controlled to be 0.1MPa, and the volume is concentrated to 1/10 of the original volume;
(4) and (3) treatment by macroporous resin: filtering the extract concentrated in the step (3), and directly introducing into macroporous resin for treatment;
(5) collecting the eluent: collecting effluent liquid from the macroporous resin column and eluent eluted by alcohol water solution with low concentration to high concentration;
(6) and (3) concentrating under reduced pressure: concentrating the eluent in the step (5) under reduced pressure to 1/10 of the original volume;
(7) and (3) detecting the extract: detecting the content of ginkgetin, bilobalide and phenolic acid in the extract by High Performance Liquid Chromatography (HPLC), wherein the method for detecting the content of ginkgetin, bilobalide and ginkgolic acid comprises the following steps: the detection method of the ginkgo flavone comprises the following steps: mobile phase: methanol: phosphoric acid: water =57:0.2:42.8, flow rate 1.0ml/min, detection wavelength 370nm, column temperature: 25 ℃, sample introduction: 20 mu L of ginkgolide, the detection method comprises the following steps: the mobile phase is methanol: water =25:75, flow rate 1.0mL/min, detector ELSD; the ginkgolic acid detection method comprises the following steps: methanol: water =90:10, flow rate 1.0mL/min, detection wavelength 310 nm;
(8) and drying and storing the extract extracted by the steps until the whole process step is finished.
As a further improvement of the invention, the lower alcohol is methanol, and the volume concentration of the lower alcohol is 75%.
The invention has the beneficial effects that: the invention carries out solvent extraction by an ultrasonic method, not only plays roles of stirring and auxiliary heating, but also more importantly, the 'cavitation effect' and the mechanical action generated by the ultrasonic in the solvent extraction can effectively break the cell walls of the medicinal materials on one hand, lead the effective components to be in a free state and be dissolved in the solvent extraction, and accelerate the molecular motion of the solvent extraction on the other hand, the extraction solvent and the effective components in the medicinal materials are quickly contacted, mutually fused and mixed, so that the action of each point in a sample medium is consistent, the whole sample is more uniformly extracted, the leaching extraction of the effective components of plants is accelerated, the extraction rate is improved, the content of the ginkgetin and the bilobalide in the extract is high, the loss of active ingredients is avoided, the production process is simplified, the production period is shortened, and the content of the treated ginkgolic acid is greatly reduced.
Detailed Description
The present invention will be described in more detail with reference to examples.
Example 1
(1) Carrying out pretreatment on the ginkgo leaves: air drying dry folium Ginkgo, and pulverizing into powder;
(2) putting the raw materials and water into an extraction tank according to a ratio of 1:10, extracting by using ultrasonic waves, wherein the ultrasonic working frequency of ultrasonic extraction is 70KHz, the extraction time is 25 minutes, filtering, adding water to the original volume, continuing to perform ultrasonic extraction for 25 minutes, filtering, and combining filtrates;
(3) and (3) concentrating under reduced pressure: concentrating the extractive solution in a rotary evaporator under reduced pressure at 55 deg.C under 0.1MPa to 1/10;
(4) and (3) treatment by macroporous resin: filtering the extract concentrated in the step (3), and directly introducing into macroporous resin for treatment;
(5) collecting the eluent: collecting effluent liquid from the macroporous resin column and eluent eluted by alcohol water solution with low concentration to high concentration;
(6) and (3) concentrating under reduced pressure: concentrating the eluent in the step (5) under reduced pressure to 1/10 of the original volume;
(7) the method for detecting the content of ginkgetin, bilobalide and ginkgolic acid in the extract by using High Performance Liquid Chromatography (HPLC) respectively comprises the following steps: the detection method of the ginkgo flavone comprises the following steps: mobile phase: methanol: phosphoric acid: water =57:0.2:42.8, flow rate 1.0ml/min, detection wavelength 370nm, column temperature: 25 ℃, sample introduction: 20 mu L of ginkgolide, the detection method comprises the following steps: the mobile phase is methanol: water =25:75, flow rate 1.0mL/min, detector ELSD; the ginkgolic acid detection method comprises the following steps: water =90:10, flow rate 1.0mL/min, detection wavelength 310 nm;
(8) and drying and storing the extract extracted by the steps until the whole process step is finished.
Example 2
(1) Carrying out pretreatment on the ginkgo leaves: air drying dry folium Ginkgo, and pulverizing into powder;
(2) ultrasonic extraction, namely putting the raw materials and 75% methanol by volume into an extraction tank according to the proportion of 1:10, extracting by using ultrasonic waves, wherein the ultrasonic working frequency of the ultrasonic extraction is 70KHz, the extraction time is 25 minutes at 25 ℃, filtering, supplementing the methanol to the original volume, continuing to perform ultrasonic extraction for 25 minutes, filtering, and combining the filtrates;
(3) and (3) concentrating under reduced pressure: concentrating the extractive solution in a rotary evaporator under reduced pressure at 45 deg.C under 0.1MPa to 1/8;
(4) and (3) treatment by macroporous resin: filtering the extract concentrated in the step (3), and directly introducing into macroporous resin for treatment;
(5) collecting the eluent: collecting effluent liquid from the macroporous resin column and eluent eluted by alcohol water solution with low concentration to high concentration;
(6) and (3) concentrating under reduced pressure: concentrating the eluent in the step (5) under reduced pressure to 1/10 of the original volume;
(7) the method for detecting the content of ginkgetin, bilobalide and ginkgolic acid in the extract by using High Performance Liquid Chromatography (HPLC) respectively comprises the following steps: the detection method of the ginkgo flavone comprises the following steps: mobile phase: methanol: phosphoric acid: water =57:0.2:42.8, flow rate 1.0ml/min, detection wavelength 370nm, column temperature: 25 ℃, sample introduction: 20 mu L of ginkgolide, the detection method comprises the following steps: the mobile phase is methanol: water =25:75, flow rate 1.0mL/min, detector ELSD; the ginkgolic acid detection method comprises the following steps: water =90:10, flow rate 1.0mL/min, detection wavelength 310 nm;
(8) and drying and storing the extract extracted by the steps until the whole process step is finished.
Through the implementation of the embodiment, the content of the effective components of the ginkgo biloba extract obtained by the method provided by the invention is high, the content of the ginkgetin in the extract is 25-30% according to the High Performance Liquid Chromatography (HPLC), the content is improved by 5-10% compared with the traditional hot extraction, and meanwhile, the content of the ginkgolide in the extract is also improved by 8-12%. The content of the ginkgolic acid in the treated extract is reduced by 0.0020-0.0030 percent compared with that in the traditional extraction method, and the content of the ginkgolic acid reaches 0.0010-0.0015 percent. The ginkgo biloba extract obtained by the invention has high content of ginkgo flavone and ginkgolide, avoids the loss of active ingredients, simplifies the production process and shortens the production period.
Claims (2)
1. A method for extracting ginkgetin from ginkgo leaves is characterized by comprising the following steps: the method takes dry ginkgo leaves as raw materials, and comprises the following process steps:
(1) carrying out pretreatment on the ginkgo leaves: pulverizing dry folium Ginkgo into powder;
(2) extracting with ultrasonic wave, mixing the raw material with extraction solvent in a ratio of 1: after fully mixing 10 (g/mL) of material-liquid ratio, extracting the material-liquid for 1-2 times at a frequency of 70KHz and a temperature of 25 ℃ for 25 minutes, filtering after extraction, and combining the filtrates, wherein the extraction solvent is water or low-carbon alcohol;
(3) and (3) concentrating under reduced pressure: putting the extracting solution obtained in the step (2) into a rotary evaporator, and concentrating under reduced pressure, wherein the temperature is controlled to be 45-55 ℃, the vacuum degree is controlled to be 0.1MPa, and the volume is concentrated to 1/10 of the original volume;
(4) and (3) treatment by macroporous resin: filtering the extract concentrated in the step (3), and directly introducing into macroporous resin for treatment;
(5) collecting the eluent: collecting effluent liquid from the macroporous resin column and eluent eluted by alcohol water solution with low concentration to high concentration;
(6) and (3) concentrating under reduced pressure: concentrating the eluent in the step (5) under reduced pressure to 1/10 of the original volume;
(7) and (3) detecting the extract: detecting the content of ginkgetin, bilobalide and phenolic acid in the extract by High Performance Liquid Chromatography (HPLC), wherein the method for detecting the content of ginkgetin, bilobalide and ginkgolic acid comprises the following steps: the detection method of the ginkgo flavone comprises the following steps: mobile phase: methanol: phosphoric acid: water =57:0.2:42.8, flow rate 1.0ml/min, detection wavelength 370nm, column temperature: 25 ℃, sample introduction: 20 mu L of ginkgolide, the detection method comprises the following steps: the mobile phase is methanol: water =25:75, flow rate 1.0mL/min, detector ELSD; the ginkgolic acid detection method comprises the following steps: methanol: water =90:10, flow rate 1.0mL/min, detection wavelength 310 nm;
(8) and drying and storing the extract extracted by the steps until the whole process step is finished.
2. The method for extracting ginkgetin from ginkgo leaves according to claim 1, wherein: the low carbon alcohol is methanol, and the volume concentration of the low carbon alcohol is 75%.
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| CN201811421117.1A CN111214503A (en) | 2018-11-27 | 2018-11-27 | Method for extracting ginkgetin from ginkgo leaves |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114705776A (en) * | 2022-03-31 | 2022-07-05 | 苏州汇通色谱分离纯化有限公司 | Multidimensional liquid chromatography device and method for purifying ginkgetin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114705776A (en) * | 2022-03-31 | 2022-07-05 | 苏州汇通色谱分离纯化有限公司 | Multidimensional liquid chromatography device and method for purifying ginkgetin |
| CN114705776B (en) * | 2022-03-31 | 2023-09-08 | 苏州汇通色谱分离纯化有限公司 | Method for purifying ginkgo flavone |
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