Method for extracting walnut ketones from epicarps of carya cathayensis Sarg and preparing walnut ketone standard product

A technology of walnut ketone and pecan, applied in the field of preparing walnut ketone standard products, can solve the problems of walnut skin and hickory exocarp raw materials, composition differences, long crystallization and recrystallization operation time, and lack of purity, so as to promote industrial development , reliable method and good stability

Inactive Publication Date: 2011-10-19
ANHUI AGRICULTURAL UNIVERSITY
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Problems solved by technology

It can be seen that the yield of this method is equivalent to 40 μg crude product / g dry powder, the purity is lacking, the yield is low, the operation time of crystallization and recrystallization is long, and it is greatly affected by temperature and humidity, and walnut ketone has certain hygroscopicity, so the actual This method is not advisable when applying
Furthermore, there are differences in raw materials and composition between walnut skin and pecan exocarp

Method used

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Embodiment Construction

[0025] Now take the laboratory implementation as an example, and the non-limiting examples are described as follows:

[0026] The pecan exocarp dried in the shade was vacuum-dried at 50° C., pulverized, and passed through a 60-mesh sieve (aperture 0.25 mm). Take 600g of raw material powder and add ammonia water with a concentration of 10-20%, mix well until moist, then add 6kg of 95% ethanol, heat reflux extraction at 50°C-80°C for 4 times, each time for 1.5h, and centrifuge the extract (3500r / min, 15min), the supernatants were combined, and concentrated under reduced pressure to an extract. Dissolve the extract with 300mL 1-3% hydrochloric acid to obtain an acidic aqueous solution (adjust pH=2-4); extract the acidic aqueous solution with 300mL chloroform, remove the lower chloroform layer, extract with 300mL 2-4% NaOH and let stand, and take the upper layer Alkaline water solution, adjust pH=7-9 with 10-20% hydrochloric acid, let stand, the lower chloroform layer is the sam...

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Abstract

The invention provides method for extracting walnut ketones from epicarps of carya cathayensis Sarg and preparing walnut ketone standard product. The method comprises the steps of: firstly, crushing the epicarps of the carya cathayensis Sargs, moistening with aqueous ammonia, adding 95 percent of ethanol solution, carrying out hot reflux extraction, extracting extract with chloroform to obtain carya cathayensis Sarg ketone sample liquid, concentrating the sample liquid, purifying by thin layer chromatography to obtain rough walnut ketone, further purifying the rough walnut ketone by using C18 reverse-phase column chromatography, collecting the rough walnut ketone eluent by segments, combining the eluent with purity larger than 95 percent detected by HPLC (High Performance Liquid Chromatography), and carrying out nitrogen blowing to remove a solvent, thus obtaining the walnut ketone standard product. For the method, the extraction process is simple, the walnut ketone has high yield and high purity, theoretical and practical application basis can be provided for comprehensively utilizing carya cathayensis Sarg resources by taking the epicarps of the carya cathayensis Sargs as raw materials, thus having an effect on changing wastes into treasures.

Description

technical background [0001] The invention belongs to the field of separation and purification of natural products, in particular to a method for extracting walnut ketone from pecan exocarp and preparing a standard product of walnut ketone. Background technique [0002] Carya cathayensis Sarg. is a plant of the genus Carya, with 17 species and 2 varieties. Hickory nuts in my country are mainly produced in the Tianmu Mountains at the junction of Zhejiang and Anhui. They are distributed in Changhua and Yuqian in Lin'an, Zhejiang Province, Linqi and Tangcun in Chun'an, Xiaofeng in Anji, Fenshui in Tonglu; Ningguo in Anhui Province, She County, Jingde, Jixi and other counties. In addition, in the 1990s, thousands of acres of wild pecans were discovered in Jinzhai County, Dabie Mountains, Anhui Province. For a long time, the comprehensive development of hickory nuts in our country is not strong enough, the technology is backward, and the utilization rate of resources is low, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/747C07C45/78
Inventor 丁之恩王晓燕屈晓清王敏丽
Owner ANHUI AGRICULTURAL UNIVERSITY
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