Production technique of Ivalin

A technology of evalrin and its production process, which is applied in the field of production process of evalrin, can solve the problems such as the undiscovered process method of evalrin, etc., and achieve the effects of easy industrial production, high efficiency and high product purity

Inactive Publication Date: 2013-01-09
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] After searching, there is no report on the process of preparing evalrin in large quantities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Get 1 kg of the flowers and leaves of the small head Yiwa chrysanthemum and crush them through a 40-mesh sieve, add them to a supercritical extraction kettle, and use supercritical CO 2 For extraction, 180ml of ethanol aqueous solution with a mass percentage concentration of 70% was introduced as an entrainer to participate in the extraction. The extraction parameters were set as follows: extraction temperature 48°C, extraction pressure 19.2MPa, CO 2 The flow rate is 15L / h, the extraction time is 3h, the analysis temperature is 35°C, and the analysis pressure is 4MPa. Collect the extract, add 6 times the volume of acetone to heat and reflux for extraction for 1.0h, extract twice, combine and concentrate the extracts into The extract is extracted 5 times with n-butanol of equal volume, the extract is concentrated and dissolved in methanol and put on the column by wet method to a silica gel high-pressure column with a filler of 200-300 mesh, the column pressure is 2.4MPa, ...

Embodiment 2

[0017] Get 1 kg of the flowers and leaves of the small head Yiwa chrysanthemum and crush them through a 60-mesh sieve, add them to a supercritical extraction kettle, and use supercritical CO 2 For extraction, 150ml of ethanol aqueous solution with a mass percentage concentration of 70% was introduced as an entrainer to participate in the extraction. The extraction parameters were set as follows: extraction temperature 46°C, extraction pressure 20.6MPa, CO 2 The flow rate is 16L / h, the extraction time is 3.5h, the analysis temperature is 40°C, and the analysis pressure is 6MPa. Collect the extract, add 5 times the volume of acetone to heat and reflux for extraction for 1.5h, concentrate the extract into an extract, and use 2 Double the volume of n-butanol and extract 3 times, concentrate the extract and dissolve it in methanol and put it on the column by wet method to a high-pressure silica gel column with a filler of 200-300 mesh, the column pressure is 2.8MPa, and the column d...

Embodiment 3

[0019] Take 1 kg of Inula inula herb and crush it through a 40-mesh sieve, add it to a supercritical extraction kettle, and use supercritical CO 2 For extraction, 300ml of ethanol aqueous solution with a mass percentage concentration of 70% was introduced as an entrainer to participate in the extraction. The extraction parameters were set as follows: extraction temperature 52°C, extraction pressure 21.7MPa, CO 2 The flow rate is 18L / h, the extraction time is 2h, the analysis temperature is 45°C, and the analysis pressure is 8MPa. Collect the extract, add 3 times the volume of acetone to heat and reflux for extraction for 0.5h, extract twice, combine and concentrate the extracts into The extract is extracted 4 times with 2 times the volume of n-butanol, and the extract is concentrated and dissolved in methanol and put on the column by wet method to a high-pressure silica gel column with a packing of 200-300 mesh, the column pressure is 3.2MPa, and the column diameter-to-height r...

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Abstract

The invention belongs to the field of traditional Chinese medicine chemistry, and relates to a production technique of Ivalin, which comprises the following steps: pulverizing the raw material chrysanthemum flower or Inula britannica chinensis to 40-60 meshes, adding into a supercritical extraction kettle, carrying out supercritical CO2 extraction by using 70 wt% ethanol as an entrainer, collecting the extract in a separation kettle, extracting under reflux with acetone, concentrating the extracting solution, extracting with n-butanol, adding the extract into a silica gel high-pressure column, carrying out gradient elution with petroleum ether-acetone, recovering the reagent from the eluate to proper volume, crystallizing, and recrystallizing with an n-heptane-ethanol mixed solution. The technique provided by the invention has the advantages of environmental protection, high extraction efficiency and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine chemistry and relates to a production process of evalrin. Background technique [0002] Ivalin, molecular weight 346.38, molecular formula C 19 h 22 o 6 , CAS registration number is 5938-03-4, is a sesquiterpene lactone compound, mp.130-132 ℃, mainly found in Asteraceae inula, glabrous chrysanthemum, small-headed Evalia, rough soil shrubs , Trilobed azulene and other plants. Pharmacological studies have shown that Evalerin has an effect on the ED of murine lymphoid leukemia P388, human nasopharyngeal carcinoma KB-3 and vinblastine-resistant KB-VI cells. 50 (μg / mL) were 0.14, 1.8, 1.3 respectively; the MIC for Bacillus subtilis was 375μg / mL. In addition, Evalthrin also has molluscicide activity and inhibits glycolytic enzymes. [0003] After searching, there is no report on the process of preparing evalrin in large quantities. Contents of the invention [0004] The obj...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/92
CPCY02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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