Pimaric acid type resin acid product and method for extracting pimaric acid type resin acid product from torreya grandis aril

The technology of Torreya aril and resin acid is applied in the field of pimaric acid-type resin acid mixture products, which can solve the problems of interference, difficulty and obstruction in separation and purification, and achieve the effects of easy separation and purification, simple operation and quality improvement.

Active Publication Date: 2014-10-15
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for Torreya aril, its chemical composition is completely different from that of rosin or rosin. Although Torreya aril contains more pimaric acid-type resin acids, it also contains lignin, tannin, Water-insoluble or water-soluble substances such as polysaccharides and pectin also contain more oil-soluble substances such as chlorophyll, resin esters, waxes, and other neutral substances. Contains some impurities such as pectin and polysaccharides. Therefore, when preparing pimaric acid-type resin acids from Torreya aril and its essential oil extraction residue as raw materials, these impurities with different properties will seriously interfere and hinder the separation and purification. function, that is to say, to exclude the interference of these complex components, it is very difficult to effectively extract the pimaric acid type resin acid from Torreya torreya aril

Method used

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  • Pimaric acid type resin acid product and method for extracting pimaric acid type resin acid product from torreya grandis aril
  • Pimaric acid type resin acid product and method for extracting pimaric acid type resin acid product from torreya grandis aril
  • Pimaric acid type resin acid product and method for extracting pimaric acid type resin acid product from torreya grandis aril

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Weigh about 200g of fresh Torreya aril, cut it into pieces and put it in a 1000mL flask, add about 300mL~400mL of distilled water and a few grains of zeolite, connect the volatile oil detector and distilled water generator, and heat the flask until there is basically no oil on the wall of the condenser tube. Turn off the heat source, cool to room temperature, and obtain 2.0mL of essential oil; for the residue in the flask, use the method of centrifugation (4000r / min, 5min) and then suction filtration to separate the aqueous solution from the solid, and the obtained solid is the essential oil Extract the residue, repeat the above process until a sufficient amount of essential oil extraction residue is obtained.

[0046] Weigh 350g of the above-mentioned essential oil extraction residue, crush it and put it into a 2000mL flask, add about 1000mL of absolute ethanol, connect the reflux condenser, reflux for 3 hours, separate the solid and liquid by suction filtration, and re...

Embodiment 2

[0051]Weigh 350g of the dried residue after industrial extraction of essential oils (provided by Fengri Perfume Technology Co., Ltd., Zhuji City, Zhejiang Province), add 1000mL of absolute ethanol, perform three extractions, and share 3000mL of ethanol to obtain 96.1g of brown extract, which is analyzed by GC The results show that there are as many as 200 components contained in the extract, and the total content of resin acid is about 50%. After removing the chlorophyll and polysaccharides that do not appear in the GC analysis process, it is estimated that the actual resin acid content is about 50%. It is about 30%. Weigh 45.2g of the obtained extract, put it in a beaker, add 60mL of water, put it in a hot water bath, stir and heat to 60°C-70°C, add 100mL of KOH aqueous solution with a mass fraction of 10% for saponification for 2h, add 150mL of diethyl ether Extracted 3 times, added dropwise HCl aqueous solution with a mass fraction of 10% for acidification, and collected 23...

Embodiment 3

[0054] Weigh 38.0 g of the extract obtained in Example 2 and place it in a beaker, add 60 mL of water, place it in a hot water bath, stir and heat to 60°C-70°C, add 40mL of KOH aqueous solution with a mass fraction of 15% for saponification, add 150mL Diethyl ether was extracted three times, and 20% HCl aqueous solution was added dropwise for acidification, and the precipitated solid matter was collected to obtain 17.2 g of a yellow-green solid product. Weighed 3.53 g of this solid product, and carried out silica gel column chromatography separation using benzene:ethyl acetate=10:1 eluent to obtain 0.85 g of pimaric acid-type resin acid mixture product, with a total extraction rate of 3.2%. All the other operations that are not described are the same as in Example 1. The GC analysis result of the pimaric acid type resin acid mixture product shows that: the content of pimaric acid type resin acid is 89.45%, and the total resin acid content is 98.15%.

[0055] The main composit...

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Abstract

The invention discloses a pimaric acid type resin acid product and a method for extracting the pimaric acid type resin acid product from torreya grandis aril. The method includes the following steps: residues obtained by extracting torreya grandis aril essential oil is used as raw material, and ethyl alcohol, methylbenzene or hexane is used as a solvent; reflux extraction is performed, and separation is performed for removing the solvent, so that a paste extract is obtained; the paste extract is dissolved in water, a sodium hydroxide aqueous solution or a potassium hydroxide aqueous solution is added for saponification, so that acids such resin acid and other esters are converted into water-soluble resin acid salts; the water-soluble resin acid salts are extracted by an organic solvent to enable the water-soluble resin acid salts to be separated from non-acid substances, resinate in the obtained aqueous solution is converted into free resin acid by hydrochloric acid or sulfuric acid, and the free resin acid is separated out from the solution, and the obtained free resin acid is subjected to column chromatography isolation and purification, so that a pimaric acid type resin acid mixture product is obtained. The main component of the product is pimaric acid type resin acid, and meanwhile, the product contains less secondary component abietic acid type resin acid.

Description

technical field [0001] The invention relates to the field of plant extracts, in particular to a pimaric acid-type resin acid mixture product extracted from Torreya aril and a technical method for extracting the pimaric acid-type resin acid mixture product from Torreya aril. Background technique [0002] Torreya torreya is a plant of the genus Taxaceae, which is mainly produced in China. Its cultivation history in my country has reached 1300 years. Zhuji and Dongyang in Zhejiang Province are its main planting areas. At present, the output of Torreya torreya in Zhejiang Province is about 1,000 tons to 1,500 tons. Torreya torreya is rich in nutrition, rich in fat, protein and multivitamins, and has high medicinal value. Its seeds have a history of eating for thousands of years as valuable nuts and dried fruits. The outer layer of Torreya torreya fruit is wrapped with a layer of fleshy aril, which accounts for about 50% to 60% of the fresh weight of its seeds. Different from T...

Claims

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Application Information

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IPC IPC(8): C09F1/04C09F1/02
Inventor 赵振东王婧李冬梅古研卢言菊毕良武陈玉湘徐士超
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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