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Method for extracting and purifying nepodin

A purification method and technology of romaine, applied in the separation/purification of carbonyl compounds, organic chemistry, production of bulk chemicals, etc., can solve the problems of unsuitability for large-scale production, small separation amount, long extraction time, etc.

Inactive Publication Date: 2011-02-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] At present, there is no patent on the extraction and purification process of sorrel in China. In the "Research on the Chemical Components of Chinese Medicine Row's Foot (I)" published by Zheng Shuiqing, 80% ethanol was used to extract several times by cold soaking at room temperature, concentrated under reduced pressure, and then dichloromethane, etc. A variety of solvents are extracted, and the extract of dichloromethane is separated by silica gel column chromatography to obtain sorrel. This method has low extraction rate, long extraction time, and small separation amount, which is not suitable for large-scale production.

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  • Method for extracting and purifying nepodin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Weigh 1 kg of gold root and grind it into coarse powder, fill it into the percolation column, add 700ml of methanol solution to the percolation column, soak it at 40-5°C for 30 minutes to fully infiltrate it, and turn on the percolation column under heat preservation Outlet valve, at the same time continuously add methanol solution from the top of the percolation column, control the flow rate at 15ml / min, until 3000ml percolation extract is collected;

[0032] b. Concentrate the extract into extract, use DM301 macroporous adsorption resin chromatography column to absorb, the adsorption speed is 3ml / min, wash the chromatography column with 3BV deionized water, discard the eluent of this step, and then use 5BV acetic acid Elution with ethyl ester-methanol (1:2), follow-up monitoring by HPLC, collect target fractions with a content higher than 65%, concentrate and dry the eluate into a yellow powder;

[0033] c. Add the above yellow powder to ethyl acetate for saturated...

Embodiment 2

[0037] a. Weigh 2kg of Radix Hibiscus (about 0.66% of sorrel) and pulverize it into a coarse powder, add 80% ethanol aqueous solution according to the mass ratio of 1:4, heat and reflux for extraction 3 times, each time for 2.5 hours, Filter and combine the filtrates;

[0038] b. Concentrate the filtrate into extract, use LSA-21 macroporous adsorption resin chromatography column to absorb, the adsorption speed is 5ml / min, wash the chromatography column with 3BV deionized water, discard the eluent of this step, and then use chloroform - Methanol 100: 1, 50: 1, 10: 1, 5: 1 gradient for elution, the amount of each elution is 3-5 column volumes, HPLC tracking monitoring, collecting target fractions with a content higher than 65%, Concentrate and dry the eluate into a yellow powder;

[0039] c. Add the above yellow powder to ethyl acetate for saturated dissolution, filter the crystals with suction, and recrystallize 3 times to obtain sorrel with a purity of 96%;

[0040] d. Satur...

Embodiment 3

[0043] a. Weigh 2 kg of Rumex dentatus and crush it into coarse powder, put it into an ultrasonic extraction tank, add methanol solution according to the ratio of mass ratio 1:8, and extract 3 times by ultrasonic extraction at a power of 50W for 1 hour, filter, and combine the filtrates;

[0044] b. Concentrate the filtrate into extract, use LSA-5B macroporous adsorption resin chromatography column to absorb, the adsorption speed is 4ml / min, wash the chromatography column with 4BV deionized water, discard the eluent of this step, and then use chloroform - Gradient elution with ethyl acetate 20:1, 10:1, 5:1, the amount of each elution is 3-5 column volumes, HPLC tracking monitoring, collect the target fraction with content higher than 65%, concentrate and dry The eluent becomes a yellow powder;

[0045] c. Add the above yellow powder to ethyl acetate for saturated dissolution, filter the crystals with suction, and recrystallize twice to obtain sorrel with a purity of 96%;

[0...

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Abstract

The invention provides a method for extracting and purifying nepodin, which consists of three parts: leaching raw materials with a solvent to obtain extract, enrichment and separation by macroporous resin and crystallization. The method comprises the following steps: crushing the raw materials, adding the solvent into the crushed raw materials for leaching for 3 times; combining the extract obtained at the three times; loading the extract for absorption by the macroporous resin; eluting by using solution of one or more than two of chloroform, ethyl acetate, acetone and methanol as eluting agent or eluting according to different proportions and with different gradients; collecting eluent, concentrating and drying to obtain yellow crude extract; performing recrystallization by using ethyl acetate as a recrystallization solvent; and performing supercritical CO2 fluid solvent resistant crystallization under a pressure of less than or equal to 15MPa and at the temperature of less than or equal to 78 DEG C. The maximum product content is up to over 98.5 percent. The extraction and purification process has the advantages of high product purity, high speed and short period.

Description

Technical field: [0001] The invention relates to a method for extracting and purifying sorrel, in particular to a method for extracting and purifying sorrel by resin adsorption and supercritical CO 2 Anti-solvent crystallization combined separation and purification method. Background technique: [0002] Musizin, also known as Musizin. [0003] Chemical name: 1-(1,8-dihydroxy-3-methylnaphthalen-2-yl)ethanone; [0004] Molecular formula: C 13 h 12 o 3 ;Molecular weight: 216.23; [0005] The molecular structure is: [0006] [0007] Physical and chemical properties: It is yellow needle crystal, mp.164℃-165℃. [0008] Pharmacological studies have shown that sorrel has antibacterial and antifungal effects. The minimum inhibitory concentrations against Trichophyton crimson, Bacillus subtilis, Candida albicans and Sarcina are respectively: 50, 25, 100, 100 μg / ml; it can be used as an antioxidant in food and cosmetics. It has an inhibitory effect on testosterone reductas...

Claims

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Application Information

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IPC IPC(8): C07C45/78C07C49/83
CPCY02P20/54
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH