Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark

A technology of phellodendron lactone and berberine, applied in the field of preparing phellodendron lactone, can solve the problems of polluting the environment, no separation of phellodendron lactone, waste of Phellodendron phellodendri resources, etc.

Inactive Publication Date: 2015-01-07
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the process of extracting berberine from phellodendron bark, the phellodendron lactone is not separated and utilized, thus wasting a lot of resources and causing great pollution to the environment
After research, it is found that the waste liquid after extracting berberine from Phellodendron bark contains a large amount of Phellodendron lactones. In the previous process, this part of the liquid was discarded, which not only polluted the environment, but also greatly wasted Phellodendron cortex resources.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0005] Use the waste liquid obtained after separating berberine from the extract of berberine from Phellodendron bark by ethanol extraction as raw material, measure 10L of waste liquid, adjust the pH value of the filtrate to about 5-7 with ammonia water, and heat to maintain the temperature at 50 At about ℃, add 50g of compound enzyme to the filtrate, enzymatically hydrolyze for 30 minutes, raise the temperature to 90℃, let the enzyme inactivate, and naturally settle for 5-10 hours to obtain a precipitate. After separating the obtained precipitate, add 5-8 times the volume of ethanol to reflux for extraction, filter after extraction to obtain a filtrate, and concentrate the filtrate to 200 mL under reduced pressure. Choose D101 macroporous adsorption resin, pretreat the resin, fully swell and remove the unpolymerized organic solvent contained in it. Pack 500mL volume of macroporous adsorption resin into a glass column or stainless steel column, wet-load 200mL concentrate, and ...

Embodiment 2

[0007] Use the waste liquid obtained after separating berberine from the berberine extract from Phellodendron bark by ethanol extraction as raw material, measure 100L of waste liquid, first concentrate it under reduced pressure to 20L, and adjust the pH value of the filtrate to 5- 7 or so, heat to keep the temperature at about 50°C, add 0.1% compound enzyme to the filtrate, enzymatically hydrolyze for 30 minutes, raise the temperature to 90°C, let the enzyme inactivate, settle naturally for 5-10 hours, and obtain about 800g of precipitate. After separating the obtained precipitate, add ethanol with 5-8 times the liquid-to-solid ratio for reflux extraction, filter after extraction to obtain the filtrate, and concentrate the filtrate under reduced pressure to about 1000 mL. Select the pretreated AB-8 macroporous adsorption resin, pack 2000mL volume of macroporous adsorption resin into a glass column or stainless steel column, apply 1000mL concentrated solution by wet method, ...

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Abstract

The invention discloses a method for preparing obakulactone from an ethanol waste liquid of separating berberine from phellodendron bark, which comprises the following steps: by using a filtrate which is obtained by separating a crude product berberine from a phellodendron bark ethanol extracting solution as a raw material, carrying out enzymolysis with composite enzymes to obtain a precipitate, carrying out reflux extraction with ethanol, filtering to obtain a filtrate, and concentrating the filtrate under reduced pressure to recover ethanol to obtain a concentrated solution; and enriching the concentrated solution by a macroporous adsorbent resin process, eluting to obtain an eluate, concentrating the eluate, crystallizing and drying to obtain the obakulactone product. The yield of the obtained obakulactone is up to 0.35% (relative to the phellodendron raw material) or so, and the content is up to 80% above. The method can comprehensively utilize the phellodendron resources, changes wastes into valuable substances, reduces the environmental pollution, has the advantages of simple separation technique, high recovery rate and high limonin content, does not use any toxic organic solvent, is environment-friendly and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing phellodendron lactone from the waste liquid after extracting berberine from cortex cortex, in particular to an enzyme treatment technology combined with a macroporous adsorption resin separation technology from the waste liquid after berberine is extracted from phellodendron bark A method for preparing phellodactone. Background technique [0002] Phellodendron amurense Rupr., also known as limonin, limonene, and dictamnus lactone, is a triterpenoid bitter substance, mainly derived from the bark of Phellodendron amurense Rupr. leather etc. It has been proved to have anthelmintic, anti-ulcer, hypoglycemic effects, and can also relax the intestines, shorten the sleep time of mice caused by α-chloralose and urethane, and other physiological effects. Phellodendron Phellodendron is a traditional medicinal material in Chinese medicine. It has the functions of clearing heat and dampness, purging fire and steami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
CPCC07J73/008
Inventor 谢红旗曾建国
Owner HUNAN AGRICULTURAL UNIV
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