Method for separating phorbol by utilizing ultrasonic-assisted alcoholysis-extraction coupling technology

A technology of ultrasonic wave and phorbol alcohol, which is applied in the field of ultrasonic-assisted alcoholysis-extraction coupling technology to separate phorbol alcohol. short time effect

Active Publication Date: 2020-05-12
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by the present invention is: in the prior art, phorbol esters are extracted from Jatropha curcas seeds, and the operation steps are many, time-consuming, solvent consumption is large and difficult to be applied in industry. There

Method used

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  • Method for separating phorbol by utilizing ultrasonic-assisted alcoholysis-extraction coupling technology
  • Method for separating phorbol by utilizing ultrasonic-assisted alcoholysis-extraction coupling technology
  • Method for separating phorbol by utilizing ultrasonic-assisted alcoholysis-extraction coupling technology

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of S1 saturated alkaline methanol solution: Add enough anhydrous potassium carbonate to methanol with a content of ≥99%, reflux in a water bath at 70°C for 2 hours, and prepare a saturated potassium carbonate-methanol solution for use;

[0028] Preparation of S2 acidic methanol solution: Add 10% volume of concentrated hydrochloric acid to 1 volume content ≥99% of methanol and mix it evenly to prepare a hydrochloric acid-methanol mixed solution for use;

[0029] S3 alcoholysis-extraction: accurately measure 1ml of croton oil in a 15ml centrifuge tube, add potassium carbonate-methanol saturated solution according to the material-to-liquid ratio of 1:10, shake and shake, under the conditions of ultrasonic power of 300W and temperature of 40℃ Extract for 30min. Set aside for separation to obtain the upper clear liquid and the lower oil phase liquid;

[0030] S4 Adjust pH: Take the supernatant liquid and the mixed solution of hydrochloric acid-methanol with a needle, a...

Embodiment 2

[0033] Preparation of S1 saturated alkaline methanol solution: Add sufficient anhydrous barium hydroxide to methanol with a content of ≥99%, reflux in a water bath at 70°C for 2 hours to prepare a saturated solution of barium hydroxide-methanol for use;

[0034] Preparation of S2 acidic methanol solution: Add 10% volume of concentrated hydrochloric acid to 1 volume content ≥99% of methanol and mix it evenly to prepare a hydrochloric acid-methanol mixed solution for use;

[0035] S3 alcoholysis-extraction: accurately measure 1ml of croton oil and place it in a 15ml centrifuge tube, add a saturated solution of barium hydroxide-methanol according to the material-to-liquid ratio of 1:10, shake and shake it evenly, the ultrasonic power is 240W, the temperature is 40℃ Extract for 30min under conditions. Set aside for separation to obtain the upper clear liquid and the lower oil phase liquid;

[0036] S4 repeated extraction: remove the lower oil phase liquid and continue alcoholysis-extrac...

Embodiment 3

[0041] Preparation of S1 saturated alkaline methanol solution: Add sufficient anhydrous potassium hydroxide to methanol with a content of ≥99%, reflux in a water bath at 70°C for 2 hours, and prepare a saturated potassium hydroxide-methanol solution for use;

[0042] Preparation of S2 acidic methanol solution: Add 10% volume of concentrated hydrochloric acid to 1 volume content ≥99% of methanol and mix it evenly to prepare a hydrochloric acid-methanol mixed solution for use;

[0043] S3 alcoholysis-extraction: accurately measure 50ml of croton oil in a 2000ml beaker, add a saturated solution of potassium hydroxide-methanol according to the material-to-liquid ratio of 1:10, shake and shake, under the condition of ultrasonic power of 240W and temperature of 40℃ Extract for 30min. Transfer to a separatory funnel, stand still and separate to obtain the upper clear liquid and the lower oil phase liquid;

[0044] S4 repeated extraction: remove the lower oil phase liquid and continue alcoh...

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Abstract

The invention relates to the technical field of natural medicine extraction, and particularly discloses a method for separating phorbol by utilizing an ultrasonic-assisted alcoholysis-extraction coupling technology. The method comprises the following steps: S1, uniformly mixing 1 part of croton oil with 5-25 parts of a saturated alkaline alcoholic solution according to a volume ratio of feed liquid, carrying out alcoholysis-extraction under the action of ultrasonic waves, and carrying out standing separation to obtain an alkaline supernatant containing phorbol and a croton oil lower phase liquid; and S2, adjusting the pH value of the obtained alkaline supernatant to be neutral by using an acidic alcohol solution, and removing the obtained precipitate to obtain a neutral alcohol solution containing the phorbol. The ultrasonic-assisted alcoholysis-extraction coupling technology is used for extracting the phorbol from the croton oil, alcoholysis and extraction are carried out synchronously, and alcoholysis-extraction coupling is carried out, so the alcoholysis efficiency is improved advantageously, alcoholysis-extraction is fast and efficient under the assistance of ultrasonic waves,time is saved, and the purity of the phorbol is improved. The method has the advantages of few operation steps, short time consumption, low solvent consumption and easiness in promotion and application.

Description

Technical field [0001] The invention belongs to the technical field of natural medicine extraction, and specifically relates to a method for separating phorbol by using ultrasonic assisted alcoholysis-extraction coupling technology. Background technique [0002] Croton (Croton tiglium L.) is Euphorbiaceae (Euphorbiaceae) Croton, also known as Jiangzi, Gangzi, Laoyangzi, etc. It was originally recorded in the "Shen Nong's Ben Cao Jing" and mainly grows in Fujian, Guangxi, and Guangdong. , Yunnan and other regions. Since ancient times, croton has been used by doctors blindly and importantly. Modern medicine believes that croton has good effects on digestive system diseases and malignant tumor diseases. Croton has natural advantages such as abundant raw materials and low price. As the substance with the highest phorbol ester content in nature, croton is undoubtedly the best raw material for extracting phorbol esters at present. [0003] Porbol ester compounds have pleiotropic biolog...

Claims

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Application Information

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IPC IPC(8): C07C49/727C07C45/64C07C45/78C07C45/80
CPCC07C45/64C07C45/78C07C45/80C07C2603/40C07C49/727
Inventor 范杰平高意张风炎
Owner NANCHANG UNIV
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