CN108864219B - Method for extracting gastrodin by high-pressure supercritical carbon dioxide - Google Patents
Method for extracting gastrodin by high-pressure supercritical carbon dioxide Download PDFInfo
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- CN108864219B CN108864219B CN201810553394.1A CN201810553394A CN108864219B CN 108864219 B CN108864219 B CN 108864219B CN 201810553394 A CN201810553394 A CN 201810553394A CN 108864219 B CN108864219 B CN 108864219B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a method for extracting gastrodin by high-pressure supercritical carbon dioxide, which comprises the step of filling a pre-crushed gastrodia elata medicinal material into high-pressure supercritical CO2In an extraction kettle of extraction equipment, the extraction kettle and a separation kettle are respectively heated to extraction temperature, and CO is added2Pumping the mixture into an extraction kettle and a separation kettle by using a high-pressure pump, adjusting a valve to enable the extraction kettle and the separation kettle to respectively reach set pressure, starting to perform circular extraction, pumping an entrainer into the extraction kettle and starting timing after set parameters are stable, wherein the using amount of the entrainer in each gram of gastrodia elata medicinal material is 0-3 ml, and discharging and collecting gastrodin extracts from the separation kettle after extraction is finished. The method improves the extraction rate of the gastrodin by high-pressure supercritical carbon dioxide extraction, shortens the production period of the gastrodin, has simple and convenient operation, small solvent consumption, easy separation and small environmental pollution of the production process, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of extraction of chemical components of traditional Chinese medicinal materials, in particular to a method for extracting gastrodin by high-pressure supercritical carbon dioxide.
Background
The gastrodia elata is a rare traditional Chinese medicinal material, has a medicinal history of more than two thousand years in China, and researches at home and abroad at present find that gastrodine as a main component of the gastrodia elata can treat diseases such as pain and dizziness, numbness of limbs, convulsion and the like, and the gastrodine is mainly used for clinically treating arterial insufficiency, vestibular neuronitis, vertigo, coronary heart disease and the like.
The traditional process for extracting gastrodin at present mainly comprises the following steps: alcohol extraction, microwave extraction, ultrasonic extraction, enzyme extraction, and the like. The problems generally existing in the prior art are that the extraction rate of gastrodin is low, the product output content is low, and meanwhile, the process and equipment conditions are complex, so that the operation of amplification production and the control of cost are not facilitated.
Supercritical carbon dioxide extraction is a non-research in recent yearsThe frequently active technology is widely used in the fields of medicine, food, spice, petrochemical industry, environmental protection and the like, and becomes an effective way for obtaining high-quality, green and environmental-friendly products. At present, few reports about supercritical extraction of gastrodin exist, and the traditional supercritical CO2The maximum extraction pressure of the extraction is 40MPa, the method is suitable for extracting conventional fat-soluble components, is not suitable for extracting gastrodin, and has low extraction rate of the gastrodin.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a method for extracting gastrodin by high-pressure supercritical carbon dioxide. The method has the advantages of simple operation, easily controlled parameters, suitability for scale-up production, high gastrodin extraction transfer rate, and less impurity components.
The purpose of the invention is realized by the following technical method: a method for extracting gastrodin by high pressure supercritical carbon dioxide comprises loading pre-pulverized rhizoma Gastrodiae into high pressure supercritical CO2In an extraction kettle of extraction equipment, the extraction kettle and a separation kettle are respectively heated to extraction temperature, and CO is added2Pumping the mixture into an extraction kettle and a separation kettle by using a high-pressure pump, adjusting a valve to enable the extraction kettle and the separation kettle to respectively reach set pressure, starting circular extraction, pumping an entrainer after set parameters are stable, starting timing, controlling the use amount of the entrainer in each gram of gastrodia elata medicinal material to be 0-3 ml, finishing extraction after the extraction time is reached, discharging the material from the separation kettle, and collecting gastrodin extract.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the gastrodia elata medicinal material is crushed into gastrodia elata medicinal material powder with the granularity of 80-200 meshes and then filled into high-pressure supercritical CO2In an extraction kettle of the extraction equipment.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the temperature of the extraction kettle is 35-65 ℃, and the pressure of the extraction kettle is 35-65 MPa.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the temperature of the extraction kettle is 50 ℃, and the pressure of the extraction kettle is 65 MPa.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the temperature of the separation kettle is 35-60 ℃, and the pressure of the separation kettle is 6-14 MPa.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the temperature of the separation kettle is 50 ℃, and the pressure of the separation kettle is 11 MPa.
Preferably, the method for extracting gastrodin by using high-pressure supercritical carbon dioxide is used, and the extraction time is 30-120 min.
Preferably, the method for extracting gastrodin by using high-pressure supercritical carbon dioxide is used, and the extraction time is 60 min.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the dosage of the entrainer in each gram of the gastrodia elata medicinal material is 1.5 ml.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the entrainer is ethanol, and the volume fraction of the ethanol is 50-95%.
Preferably, in the method for extracting gastrodin by using high-pressure supercritical carbon dioxide, the entrainer is ethanol with a volume fraction of 95%.
Compared with the prior art, the invention has the following beneficial effects: the invention improves the extraction rate of gastrodin by high-pressure supercritical carbon dioxide extraction, shortens the production period of gastrodin, has simple and convenient operation, small solvent dosage, easy separation and small environmental pollution of production process, is suitable for industrial production, can effectively extract gastrodin, and has high purity of the obtained product. With conventional supercritical CO2Compared with the extraction technology, the method adopts high-pressure supercritical CO2The extraction technology improves the polar range of extraction of the extract, shortens the extraction time and improves the extraction efficiency.
Detailed Description
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
Example 1
A method for extracting gastrodin by high pressure supercritical carbon dioxide comprises pulverizing rhizoma Gastrodiae to 200 mesh, and loading into high pressure supercritical CO2In the extraction kettle of the extraction equipment, the extraction kettle and the separation kettle are respectively heated, and when the temperatures of the extraction kettle and the separation kettle reach 50 ℃ and 50 ℃, CO is added2Pumping the mixture into an extraction kettle and a separation kettle by using a high-pressure pump, adjusting valves to enable the pressures of the extraction kettle and the separation kettle to respectively reach 65MPa and 11MPa, starting to perform circular extraction, pumping 95% volume fraction ethanol into the extraction kettle and starting timing after the pressure and the temperature are stable, wherein the dosage of entrainer in each gram of gastrodia elata medicinal material is 1.5ml, the extraction time is 60min, discharging the material from the separation kettle and collecting gastrodin extract after the extraction is finished. Through analysis and detection, the extraction rate of the gastrodia elata in the invention is calculated to be 94.5% according to the content of gastrodin in the gastrodia elata and the content of gastrodin in an extracting solution.
Example 2
A method for extracting gastrodin by high pressure supercritical carbon dioxide comprises pulverizing rhizoma Gastrodiae to 80 mesh, and loading into high pressure supercritical CO2In the extraction kettle of the extraction equipment, the extraction kettle and the separation kettle are respectively heated, and when the temperatures of the extraction kettle and the separation kettle reach 65 ℃ and 35 ℃, CO is added2Pumping the mixture into an extraction kettle and a separation kettle by using a high-pressure pump, adjusting valves to enable the pressures of the extraction kettle and the separation kettle to respectively reach 35MPa and 14MPa, starting to perform circular extraction, pumping 50% volume fraction ethanol into the extraction kettle and starting timing after the pressure and the temperature are stable, wherein the dosage of entrainer in each gram of gastrodia elata medicinal material is 3ml, the extraction time is 120min, discharging the material from the separation kettle and collecting gastrodin extract after the extraction is finished. Through analysis and detection, the extraction rate of the gastrodia elata in the invention is calculated to be 69.3% according to the content of gastrodin in the gastrodia elata and the content of gastrodin in an extracting solution.
Example 3
A method for extracting gastrodin by high pressure supercritical carbon dioxide comprises pulverizing rhizoma Gastrodiae to 120 mesh, and loading into high pressure supercritical CO2In the extraction kettle of the extraction equipment, the extraction kettle and the separation kettle are dividedHeating respectively, and adding CO when the temperature of the extraction kettle and the separation kettle reaches 35 ℃ and 60 ℃ respectively2Pumping into an extraction kettle and a separation kettle by a high-pressure pump, adjusting a valve to enable the pressure of the extraction kettle and the pressure of the separation kettle to reach 50MPa and 6MPa respectively, starting to perform circular extraction, timing, discharging for 60min, and collecting gastrodin extract. Through analysis and detection, the extraction rate of the gastrodia elata in the invention is calculated to be 80.5% according to the content of gastrodin in the gastrodia elata and the content of gastrodin in an extracting solution.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. A method for extracting gastrodin by high-pressure supercritical carbon dioxide is characterized by comprising the following steps: loading pre-pulverized rhizoma Gastrodiae into high pressure supercritical CO2In the extraction kettle of the extraction equipment, the extraction kettle and the separation kettle are respectively heated to 50 ℃ and 50 ℃, and CO is added2Pumping the mixture into an extraction kettle and a separation kettle by using a high-pressure pump, adjusting a valve to enable the extraction kettle and the separation kettle to respectively reach set pressures of 65MPa and 11MPa, starting to perform circular extraction, pumping an entrainer with volume fraction of 95% after set parameters are stable, starting to time, wherein the entrainer is ethanol with volume fraction of 1.5ml in each gram of rhizoma gastrodiae medicinal material, extracting for 60min, discharging the material from the separation kettle, and collecting gastrodin extract after extraction time is reached.
2. The method for extracting gastrodin by high-pressure supercritical carbon dioxide according to claim 1, characterized in that: the gastrodia elata medicinal material is crushed to the granularity of 80-200 meshes and then filled into high-pressure supercritical CO2In an extraction kettle of the extraction equipment.
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| CN114621304A (en) * | 2022-02-24 | 2022-06-14 | 西藏天虹科技股份有限责任公司 | Process for extracting gastrodin |
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Non-Patent Citations (2)
| Title |
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| 夹带剂在超临界CO2萃取中药有效成分中的应用;孙亚伟;《药学研究》;20140131;第33卷(第1期);第39-41页，参见摘要、第39页左栏 * |
| 超临界CO2提取天麻素的工艺研究;毛双群等;《豆丁网》;20110227;第1-9页 * |
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