Extracting method of 2'-hydroxy-4'-methoxyacetopheone

A kind of extraction method, technology of paeonol

Inactive Publication Date: 2016-07-27
CHONGQING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among the above-mentioned several extraction methods of paeonol at present, the use of chloroform and carbon tetrachloride in the solvent method has high toxicity and heavy pollution, and is not suitable for industrialized production. Although ethanol is weak in toxicity, the efficiency of ethanol extraction is slightly low, even if more The method of extracting several times can also cause the problem of a corresponding increase in the amount of impurities extracted, and still use organic solvents, which is poor in environmental protection
The extraction rate is 88.1% after two extractions using only steam distillation, and the 30min efficiency of the second stage of steam distillation is extremely low, and the energy cost is correspondingly increased, which also has certain problems
while CO 2 Although the extraction of supercritical extraction technology can better bring out the organic matter in the medicinal materials, the content of other organic impurities is also high, and the selectivity is poor.

Method used

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  • Extracting method of 2'-hydroxy-4'-methoxyacetopheone
  • Extracting method of 2'-hydroxy-4'-methoxyacetopheone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 A method for extracting paeonol, comprising the steps of:

[0020] 1) Break the dry peony cortex into powder, the powder is off-white, after 10 # Sieve (particle size less than 2mm) as raw material; accurately weigh 25.0g of Moutan Cortex powder, place it in a 250mL round bottom flask, add 150mL of distilled water for warm soaking, and warm soaking time is 19h, in order to make more substances in Moutan Cortex Dissolve it in distilled water, soak it and place it in an ultrasonic cleaner (100KHz, 50W) for 20min.

[0021] 2) Step 1) After the immersion is completed, transfer the extract and raw materials into the flask together, set up the steam distillation device, start the steam distillation, collect the distillate, and wait until the turbidity of the distillate in the condensation tube is obvious Descend, stop distillation when the mass volume ratio of described raw material and distillate is 1:2.5, the quality of taking distillate is between 63.5 ~ 64.5g...

Embodiment 2

[0028] Example 2 A method for extracting paeonol, comprising the steps of:

[0029] 1) Break the whole Xu Changqing dry product into powder, after 10 # Sieve (particle size less than 2mm) as raw material; accurately weigh 25.0g of the whole plant Xu Changqing powder, place it in a 250mL round bottom flask, add 250mL distilled water for warm soaking, and warm soaking time is 15h, in order to make the whole plant Xu Changqing It is more soluble in solvent water, and after soaking, place it in an ultrasonic cleaner (100KHz, 50W) for 10min.

[0030] 2) Step 1) After the immersion is completed, transfer the extract and raw materials into the flask together, set up the steam distillation device, and start the steam distillation. After the turbidity of the distillate in the condensation tube decreases significantly, the distillate Stop the distillation when the mass is 2.5 times the mass of the Xu Changqing powder raw material of the whole plant, cool the distillate in the refrige...

Embodiment 3

[0034] Example 3 A method for extracting paeonol, comprising the steps of:

[0035] 1) Break the dried root of Xu Changqing into powder, after 10 # Sieve (particle size less than 2mm) as raw material; Accurately weigh 25.0g of Xu Changqing root powder, put it in a 250mL round bottom flask, add 200mL distilled water for warm soaking, warm soaking time is 10h, in order to make more substances in Xu Changqing root Dissolve it in solvent water, put it in an ultrasonic cleaner (100KHz, 50W) for 30min after soaking.

[0036] 2) Step 1) After the immersion is completed, transfer the extract and raw materials into the flask together, set up the steam distillation device, and start the steam distillation. After the turbidity of the distillate in the condensation tube decreases significantly, the distillate Stop distillation when the mass is 3 times the mass of Xu Changqing root powder raw material, cool the distillate in a refrigerator (4-6°C) for 24 hours and then filter, the obtai...

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Abstract

The invention provides an extracting method of 2'-hydroxy-4'-methoxyacetopheone.The method comprises the steps that a water steam distillation and alkali-dissolution and acid-precipitation combined method is adopted to extract 2'-hydroxy-4'-methoxyacetopheone, moutan bark and whole plants of paniculate swallowwort or paniculate swallowwort roots serve as the raw materials, the raw materials are smashed and subjected to water extraction for 10 h-23 h, water steam distillation is conducted, and distillation is stopped when the mass of distillate is 2.5-3 times that of the raw materials; the distillate is cooled and filtered, a product A is obtained, the pH of the raw material and residual liquid in a flask after water steam distillation is conducted is adjusted to be 12-14, and alkali dissolution is conducted; the pH of the solution is adjusted to be 5-7 after alkali dissolution is conducted, acid precipitation is conducted, cooling and filtering are conducted, and a product B is obtained.The method can efficiently extract 2'-hydroxy-4'-methoxyacetopheone, the extraction rate reaches up to 95.3%, and the purity of obtained 2'-hydroxy-4'-methoxyacetopheone reaches up to 98.8%; according to the method, no organic solvent is adopted, environmental pollution is avoided, and environmental friendliness is better achieved.

Description

Technical field [0001] The present invention is an active ingredient and application field in Chinese herbal medicines, and it involves a method of extract for a dehuminol. Background technique [0002] Danol is the root skin that is mainly separated from the root skin of the peony or the Moroic plant of the peony of the peony.It has been found to have a variety of medicinal effects. The main pharmacological effects are sedative, hypnosis, antioxidant, lowering blood pressure, antibacterial, anti -inflammatory and other effects. Danol can reduce the fading of pigments deposited in the skin to increase the skin whitening the skin.It is widely used in cosmetics, toothpaste, ruling liquid, and tooth powder. [0003] The main extraction methods of peony skin or Xu Changqing are the following: 1. Organic solvent immersion method.Kang Yebin, Shang Hongsheng, etc. In the "Optimization of the Craft Optimization of the Solid Method Extraction", the amount of chlorine, tetrachloride, ace...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C45/84C07C45/85C07C49/84
CPCC07C45/78C07C45/84C07C45/85C07C49/84
Inventor 穆小静李泉丹陈刚吴丁丁祖丽皮艳.阿布力米特
Owner CHONGQING UNIV
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