CN110551572A - Extraction method of cassia twig volatile oil - Google Patents
Extraction method of cassia twig volatile oil Download PDFInfo
- Publication number
- CN110551572A CN110551572A CN201810536425.2A CN201810536425A CN110551572A CN 110551572 A CN110551572 A CN 110551572A CN 201810536425 A CN201810536425 A CN 201810536425A CN 110551572 A CN110551572 A CN 110551572A
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- CN
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- kettle
- extraction
- separation
- separation kettle
- cassia twig
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Abstract
The invention discloses an extraction method of cassia twig volatile oil, which comprises the following steps: drying and crushing cassia twig medicinal materials, and sieving the crushed cassia twig medicinal materials with a 18-mesh sieve. Drying at 60 deg.C for 4 hr, precisely weighing 100g (to 0.0001g), and placing into extraction kettle. Heating the extraction kettle, the separation kettle I and the separation kettle II, and pressurizing the system by a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 35-40 ℃. When the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 15-35MPa, the flow of CO2 is adjusted, and the constant temperature and the constant pressure are kept. And after the selected extraction time is reached, discharging from discharge ports of the separation kettle I and the separation kettle II, and respectively collecting and storing the extracts. Separating the extract with chromatography column. The extraction method of the invention is simple and easy to implement, has high yield, does not need a large amount of organic solvents, is safe and nontoxic, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, and in particular relates to a method for extracting cassia twig volatile oil. Background
Ramulus Cinnamomi, also known as ramulus Cinnamomi, is the dry twig of Cinnamomum cassia of Lauraceae, produced mainly in Guangdong, Guangxi and Yunnan provinces. Collected in spring and summer, leaves are removed, and the product is dried in the sun or sliced and dried in the sun, unprocessed. The medicine property is pungent, sweet and warm; meridian tropism includes heart, lung and bladder; has effects in inducing sweat, expelling pathogenic factors from muscles, warming and activating channels, and supporting yang to regulate qi, and can be used for treating dyspepsia, gastritis, blood circulation disorder, and inflammatory diseases. Cassia twig has also been found to have antioxidant activity, inhibiting the synthesis of cyclooxygenase and nitric oxide.
One of the main effective substances of cassia twig is volatile oil, which mainly contains cinnamaldehyde, and in addition, contains all the components of phenols, organic acids, polysaccharides, glycosides, coumarins, tannins and the like. In recent years, a plurality of researchers deeply research the raw pharmaceutical and chemical components of the cassia twig, but the corresponding production process reports that the prior reported extraction methods of the cassia twig volatile oil comprise a supercritical CO2 extraction method and a conventional volatile oil extraction method (a steam distillation method), and the invention adopts the supercritical CO2 extraction method to extract the cassia twig volatile oil and aims at selecting a new method for industrially extracting the cassia twig volatile oil.
Disclosure of Invention
The invention aims to provide the extraction method of the cassia twig volatile oil, which has the advantages of safety, no toxicity, short time consumption, high extraction rate, simple process and continuous operation.
The invention comprises the following steps:
a. Drying and crushing cassia twig medicinal materials, and sieving the crushed cassia twig medicinal materials with a 18-mesh sieve.
b.60 ℃ drying for 4h, accurately weighing 100g (to the accuracy of 0.0001g), and placing into an extraction kettle.
c. and (3) extraction: heating the extraction kettle, the separation kettle I and the separation kettle II, and pressurizing the system by a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 35-40 ℃. When the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 15-35MPa, the flow of CO2 is adjusted, and the constant temperature and the constant pressure are kept. And after the selected extraction time is reached, discharging from the discharge holes of the separation kettle I and the separation kettle II, and respectively collecting and storing.
d. Extraction and separation: separating the extract with chromatography column.
The extraction method of the invention is simple and easy, does not need a large amount of organic solvent, is safe and nontoxic, and is suitable for industrial production.
The specific implementation mode is as follows:
The invention is illustrated below by way of example, without the protection of the invention being restricted thereto.
Example 1:
drying and crushing cassia twig medicinal materials, sieving the crushed cassia twig medicinal materials with a 18-mesh sieve, drying the cassia twig medicinal materials for 4 hours at 60 ℃, precisely weighing 100g (precisely 0.0001g) of the cassia twig medicinal materials, putting the cassia twig medicinal materials into an extraction kettle, heating the extraction kettle, a separation kettle I and a separation kettle II, pressurizing a system by a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 35 ℃, regulating the flow of CO 2 when the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 15MPa respectively, keeping constant temperature and constant pressure, discharging the materials from discharge holes of the separation kettle I and the separation kettle II after the selected extraction time is reached, respectively collecting and storing the materials, and passing the obtained extract through a chromatographic column to
Example 2:
Drying and crushing cassia twig medicinal materials, sieving the crushed cassia twig medicinal materials with a 18-mesh sieve, drying the cassia twig medicinal materials for 4 hours at 60 ℃, precisely weighing 100g (precisely 0.0001g) of the cassia twig medicinal materials, putting the cassia twig medicinal materials into an extraction kettle, heating the extraction kettle, a separation kettle I and a separation kettle II, pressurizing a system through a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 35 ℃, adjusting the flow of CO 2 when the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 25MPa respectively, keeping constant temperature and constant pressure, discharging the materials from discharge holes of the separation kettle I and the separation kettle II after the selected extraction time is reached, respectively collecting and storing the materials, and passing the obtained extract through a chromatographic column to.
Example 3:
Drying and crushing cassia twig medicinal materials, sieving the crushed cassia twig medicinal materials with a 18-mesh sieve, drying the cassia twig medicinal materials for 4 hours at 60 ℃, precisely weighing 100g (precisely 0.0001g) of the cassia twig medicinal materials, putting the cassia twig medicinal materials into an extraction kettle, heating the extraction kettle, a separation kettle I and a separation kettle II, pressurizing a system through a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 45 ℃, adjusting the flow of CO 2 when the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 25MPa respectively, keeping constant temperature and constant pressure, discharging the materials from discharge holes of the separation kettle I and the separation kettle II after the selected extraction time is reached, respectively collecting and storing the materials, and passing the obtained extract through a chromatographic column to.
Example 4:
drying and crushing cassia twig medicinal materials, sieving the crushed cassia twig medicinal materials with a 18-mesh sieve, drying the cassia twig medicinal materials for 4 hours at 60 ℃, precisely weighing 100g (precisely 0.0001g) of the cassia twig medicinal materials, putting the cassia twig medicinal materials into an extraction kettle, heating the extraction kettle, a separation kettle I and a separation kettle II, pressurizing a system through a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 45 ℃, adjusting the flow of CO 2 when the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 35MPa respectively, keeping constant temperature and constant pressure, discharging the materials from discharge holes of the separation kettle I and the separation kettle II after the selected extraction time is reached, respectively collecting and storing the materials, and passing the obtained extract through a chromatographic column to.
Claims (2)
1. the extraction method of the cassia twig volatile oil is characterized by comprising the following steps:
a. Drying and crushing cassia twig medicinal materials, and sieving the crushed cassia twig medicinal materials with a 18-mesh sieve.
b.60 ℃ drying for 4h, accurately weighing 100g (to the accuracy of 0.0001g), and placing into an extraction kettle.
c. and (3) extraction: heating the extraction kettle, the separation kettle I and the separation kettle II, and pressurizing the system by a high-pressure pump when the temperature of the extraction kettle, the separation kettle I and the separation kettle II reaches 35-40 ℃. When the pressure of the extraction kettle, the separation kettle I and the separation kettle II reaches 15-35MPa, the flow of CO2 is adjusted, and the constant temperature and the constant pressure are kept. And after the selected extraction time is reached, discharging from the discharge holes of the separation kettle I and the separation kettle II, and respectively collecting and storing.
d. Extraction and separation: separating the extract with chromatography column.
2. The method for extracting cassia twig volatile oil as claimed in claim 1, wherein the extraction and separation device in step d is a 20mm x 600mm chromatographic column with 100 ~ 200 mesh sand, and the developing solvent is methylcyclohexane and ethyl acetate (5: 1).
Priority Applications (1)
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CN201810536425.2A CN110551572A (en) | 2018-05-30 | 2018-05-30 | Extraction method of cassia twig volatile oil |
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CN201810536425.2A CN110551572A (en) | 2018-05-30 | 2018-05-30 | Extraction method of cassia twig volatile oil |
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CN110551572A true CN110551572A (en) | 2019-12-10 |
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CN201810536425.2A Pending CN110551572A (en) | 2018-05-30 | 2018-05-30 | Extraction method of cassia twig volatile oil |
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CN (1) | CN110551572A (en) |
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2018
- 2018-05-30 CN CN201810536425.2A patent/CN110551572A/en active Pending
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WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20191210 |
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WD01 | Invention patent application deemed withdrawn after publication |