Method for preparing high-purity phloretin by utilizing shaddock peels

A technology of pomelo peel and phloretin, which is applied in the field of separation and purification of natural medicines, can solve the problems of expensive equipment, complex process, and cumbersome preparation methods, and achieve the effect of meeting industrial production requirements, simplifying complex processes, and simple process steps

Active Publication Date: 2016-06-22
LIANYUAN KANGLU BIOLOGICAL TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The content of phloretin in natural plants is scarce and the extraction rate is low, which limits the development and application of phloretin
Chinese patent (publication number CN103922914A) discloses a preparation method of high-purity phloretin, which specifically discloses that litchi peel is used as raw material, and litchi peel extract is prepared by heating with a high-purity, weakly polar solvent, and the obtained extract is subjected to liquid-liquid extraction. (including two-phase extraction), membrane technology separation and other separation and purification process steps to obtain high-purity phloretin. The process is complicated, the equipment required is expensive, and the yield of phloretin is low.
Chinese patent (publication number CN104292094A) discloses a preparation method of high-purity phloretin, which specifically discloses the steps of using apple root bark as a raw material, crushing, extraction, concentration, centrifugation, purification of macroporous adsorption resin, crystallization, acid hydrolysis, etc. , the phloretin produced industrially, the process is complicated, and the yield is low
Chinese patent (publication number CN103230408B) specifically discloses the use of naringin in the presence of lye and rare metal catalysts to carry out catalytic hydrogenation with hydrogen at medium pressure and normal temperature or under heating, and then collect naringin dihydrochalcone from the reaction system , then use naringin dihydrochalcone to heat and hydrolyze under the action of dilute acid, and purify to obtain phloretin. The initial raw material adopted in this method is naringin, and naringin itself is a kind of difficult compound to obtain, and its preparation method is loaded down with trivial details, The price is relatively expensive, which is not conducive to industrial application production
The steps for obtaining naringin or hesperidin in these methods are cumbersome and inefficient, resulting in limitations in the subsequent industrial production of phloretin

Method used

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  • Method for preparing high-purity phloretin by utilizing shaddock peels
  • Method for preparing high-purity phloretin by utilizing shaddock peels

Examples

Experimental program
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Embodiment 1

[0032] Crush 1 kg of pomelo peel into 10 meshes, extract with boiling water 3 times, each time for 2 hours, use water with 6 times the mass of grapefruit peel powder each time, combine the filtered filtrate after each extraction, add concentrated hydrochloric acid to configure the concentration of hydrochloric acid in mass percent 2% solution, reflux acid hydrolysis for 4 hours, filter while hot, collect the precipitate as the intermediate, add the intermediate to the reaction kettle, add 5g of palladium carbon, and 10 times the mass of the intermediate product (mass percentage concentration is 5%) Hydroxide Sodium solution, hydrogen pressure 0.8Mpa, react at 40°C for 12h, filter and recover palladium carbon, adjust the filtrate to pH=4, let it stand for 12h, filter to obtain phloretin coarse crystals, use 10 times the mass of coarse crystals (mass Percentage concentration is 50%) ethanol, coarse crystal quality 1% gac is refluxed and dissolved, filtered while hot, the filtrate...

Embodiment 2

[0034] Grind 1 kg of pomelo peel into 20 meshes, extract with boiling water twice, each time for 2 hours, use water with 8 times the mass of grapefruit peel powder each time, combine the filtrate obtained by filtering after each extraction, add concentrated sulfuric acid to configure the mass percent concentration of sulfuric acid as 3% solution, reflux acid hydrolysis for 6 hours, filter while hot, collect the precipitate as the intermediate, add the intermediate to the reaction kettle, add 10g of skeleton nickel, and 8 times the mass of the intermediate product (mass percentage concentration is 7%) Hydroxide Potassium solution, hydrogen pressure 1.0Mpa, react at 45°C for 16h, filter and recover the skeleton nickel, adjust the filtrate to pH=6, let it stand for 12h, filter to obtain phloretin coarse crystals, use coarse crystals with 10 times the mass of the coarse crystals (mass The percentage concentration is 50%) methanol, 2% of the coarse crystal mass of activated carbon i...

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Abstract

The invention discloses a method for preparing high-purity phloretin by utilizing shaddock peels. The method comprises the following steps: after crushing dried shaddock peels, extracting through water refluxing to obtain an extracting solution; adding an acid solution into the extracting solution, and carrying out an acid hydrolysis reaction; carrying out a hydrogenation reaction on a hydrolysis reaction product; acidifying and recrystallizing a hydrolysis reaction product in sequence to obtain the product. The method takes the shaddock peels as the direct raw material, so that the cost is low; the method has the advantages of simple process steps, high phloretin yield and high purity, and meets industrial production requirements.

Description

technical field [0001] The invention relates to a method for preparing high-purity phloretin from pomelo peel, which belongs to the field of separation and purification of natural medicines. Background technique [0002] [0003] Phloretin chemical name: 3-(4-hydroxyphenyl)-1-(2,4,6-trihydroxyphenyl)-1-propanone. Mainly distributed in the peel and root bark of juicy fruits such as apples and pears. Phloretin is a new type of natural skin whitening agent recently developed by foreign countries, and researches and develops new drugs by studying the relationship between compound structure and curative effect, and studies its mechanism of action and metabolic process in vivo. in progress. Studies have shown that phloretin has the following effects: [0004] (1) Anti-oxidation and anti-free radical effects: Phloretin has strong anti-oxidation properties, and the anti-oxidation concentration of oil is between 10 and 30ppm, which can remove free radicals in the skin, and free...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C49/83
CPCC07C45/78C07C49/83
Inventor 魏有何肖业成
Owner LIANYUAN KANGLU BIOLOGICAL TECH CO LTD
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