Separation of sihydroartemisinic acid from artemisinin production waste by means of alkali dissolution and acid deposition

A technology of dihydroartemisinic acid and production waste, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of waste of resources, high cost of industrialized development, etc., achieve high recovery rate, improve extraction efficiency and The effect of high recovery rate and production volume

Inactive Publication Date: 2015-01-07
HUNAN AGRICULTURAL UNIV
View PDF4 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the above-mentioned method of heterologous synthesis of artemisinic acid has made progress in stages, it has not yet been developed industrially due to the high cost.
In the production process of artemisinin, dihydroartemisinic acid is also extracted from the plant at the same time, but in the further separation and purification of artemisinin, dihydroartemisinic acid is left in the production waste liquid, and Not being used again, resulting in a lot of waste of resources
Therefore, research on the separation of dihydroartemisinic acid from artemisinin production waste liquid is of great significance to fully utilize Artemisia annua resources, increase product added value and reduce production cost of artemisinin. There is no relevant literature report so far.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Separation of sihydroartemisinic acid from artemisinin production waste by means of alkali dissolution and acid deposition
  • Separation of sihydroartemisinic acid from artemisinin production waste by means of alkali dissolution and acid deposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 20L of artemisinin production waste liquid, concentrate in vacuum at 33°C until the organic solvent evaporates to dryness, add 450mL of methanol, concentrate in vacuum at 40°C until the solution is completely evaporated, weigh the residue, weigh 2.3Kg; add 11.5L to achieve a mass volume concentration of 0.2% 80 watts of sodium hydroxide solution, 80 watts of ultrasonic extraction twice, ultrasonic temperature is 50 ℃, 60min each time, the two extracts are combined, and centrifuged at 3000rpm at room temperature for 10min, to remove the precipitate, collect the supernatant, and obtain a clarified extract solution. Add 1mol / L hydrochloric acid solution to the extraction solution, and keep stirring until the pH value of the solution is 4.5, place it at room temperature until the precipitate is completely precipitated, pour off the supernatant, collect the precipitate, wash the precipitate twice with 150 mL distilled water, and wash the precipitate Pre-freeze at -21°C f...

Embodiment 2

[0020] Take 5kg of artemisinin production waste paste, add 410mL of absolute ethanol, concentrate in vacuo at 40°C until the solvent is completely evaporated, weigh the residue, weighing 3.7Kg; add 11.1L of sodium bicarbonate solution with a mass volume concentration of 0.6%, 90W Ultrasonic extraction 2 times, 50min each time, the ultrasonic temperature is 45 ℃, combined the 2 extracts, centrifuged at 3000rpm at room temperature for 12min, to remove the precipitate, collect the supernatant to obtain a clarified extract solution; add 0.5mol / L to the clarified extract solution sulfuric acid solution, and kept stirring until the pH value of the solution was 3.2, placed at room temperature until the precipitate was completely precipitated, poured off the supernatant, collected the precipitate, rinsed the precipitate twice with 190mL distilled water, and pre-frozen the washed precipitate at -21°C for 15h. Vacuum freeze-drying until the moisture content of the product is lower than 1...

Embodiment 3

[0022]Take 4 kg of artemisinin production waste paste, add 350 mL of methanol, concentrate in vacuo at 33°C until the solvent evaporates completely, weigh the residue, weighing 2.9Kg; Ultrasonic extraction 2 times, 45min each time, the ultrasonic temperature is 40 ℃, combine the 2 extracts, centrifuge at 3000rpm at room temperature for 15min, remove the precipitate, collect the supernatant to obtain a clarified extract, add 2mol / L of Phosphoric acid solution, and keep stirring until the pH value of the solution is 1.0, place it at room temperature until the precipitate is completely precipitated, pour off the supernatant, collect the precipitate, rinse the precipitate twice with 150mL distilled water, pre-freeze the washed precipitate at -21°C for 24h, vacuum Freeze-dry until the moisture content of the product is lower than 1%, and the product of dihydroartemisinin is obtained. The product weighs 72.5g, and the detection by gas chromatography (the method is the same as in Exam...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses separation of sihydroartemisinic acid from artemisinin production waste by means of alkali dissolution and acid deposition. The method comprises the following steps of: concentrating in vacuum to volatilize residual solvents in production waste liquid or waste paste by using the artemisinin production waste liquid or the waste paste as raw materials; ultrasonically extracting by using alkali solution; mixing extracting solution with one another and removing sediments to obtain supernate; adding acid solution into the supernate; collecting sediments; washing the sediments by using clean distilled water; freeze-drying to obtain a dry sihydroartemisinic product. A method for separating sihydroartemisinic from the artemisinin production waste is established at first, and then an ultrasonic-assisted extracting method is adopted, so that the extraction efficiency and the recovery rate are effectively improved; by utilizing a freeze-drying method, the problem of degradation of the sihydroartemisinic acid product caused in the traditional drying method is effectively solved; the purity of the product is more than 72 percent, and the recovery rate is more than 90 percent; moreover, the production capacity is high, and the industrialized production is easily realized.

Description

technical field [0001] The invention relates to a preparation method of dihydroartemisinic acid, in particular to a method for separating dihydroartemisinic acid from artemisinin production waste by using an alkali extraction and acid precipitation method. Background technique [0002] Artemisinin is the first natural medicine discovered in my country that is internationally recognized and has independent intellectual property rights. It is also the only Chinese medicine that has been approved by the WHO and developed according to Western medicine research standards. Artemisinin currently on the market is produced in my country, which plays an important role in promoting the development of my country's traditional Chinese medicine industry. Since the World Health Organization identified artemisinin as the safest and most effective antimalarial drug at present, and as the first drug to treat malaria, the market demand for artemisinin has grown rapidly. Malaria is the most wi...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/26C07C51/42C07C51/48
CPCC07C51/42C07C51/47C07C51/50C07C2602/28C07C57/26
Inventor 刘硕谦曹娟廖欢周兰杨威田冬铭吴敦超
Owner HUNAN AGRICULTURAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap