Method for separating phorbol alcohol by 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: 2021-07-20
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 are still some defects and deficiencies in the relevant literature reports on the separation of phorbol alcohol, so the present invention provides a method for separating phorbol alcohol from croton oil using ultrasonic-assisted alcoholysis-extraction coupling technology

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  • Method for separating phorbol alcohol by ultrasonic-assisted alcoholysis-extraction coupling technology
  • Method for separating phorbol alcohol by 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 a sufficient amount of anhydrous potassium carbonate to methanol with a content ≥ 99%, reflux in a water bath at 70°C for 2 hours, and prepare a potassium carbonate-methanol saturated solution for later use;

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

[0029] S3 Alcoholysis-extraction: Precisely measure 1ml of croton oil and put it in a 15ml centrifuge tube, add potassium carbonate-methanol saturated solution according to the ratio of solid to liquid 1:10, shake and shake well, under the condition of ultrasonic power of 300W and temperature of 40℃ Under extraction for 30min. Standing and separating to obtain upper clarified liquid and lower layer oil phase liquid;

[0030] S4 adjust the pH: use a needle to take the supernatant liquid a...

Embodiment 2

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

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

[0035] S3 alcoholysis-extraction: Precisely measure 1ml of croton oil and place it in a 15ml centrifuge tube, add barium hydroxide-methanol saturated solution according to the ratio of solid to liquid 1:10, oscillate and shake well, in the ultrasonic power of 240W, the temperature is 40℃ Conditions for extraction of 30min. Standing and separating to obtain upper clarified liquid and lower layer oil phase liquid;

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

Embodiment 3

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

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

[0043] S3 Alcoholysis-extraction: Precisely measure 50ml of croton oil and put it in a 2000ml beaker, add potassium hydroxide-methanol saturated solution according to the ratio of solid to liquid 1:10, shake and shake well, under the condition of ultrasonic power of 240W and temperature of 40℃ Under extraction for 30min. Go to in the separating funnel, leave standstill to separate, obtain upper layer clarified liquid and lower layer oil phase liquid;

[0044] S4 repeated extraction: remo...

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Abstract

The invention relates to the technical field of extraction of natural medicines, and specifically discloses a method for separating phorbol by ultrasonic-assisted alcoholysis-extraction coupling technology. The method includes the following steps: S1. According to the volume ratio of the material to the liquid, mix 1 part of croton oil with 5-25 parts of saturated alkaline alcohol solution evenly, carry out alcoholysis-extraction under the action of ultrasonic waves, stand and separate, and obtain phorbol-containing Alcohol alkaline supernatant and croton oil lower phase; S2. Adjust the obtained alkaline supernatant to neutral pH with an acidic alcohol solution, remove the precipitate, and obtain a neutral alcohol solution containing phorbol alcohol. The present invention utilizes ultrasonic-assisted alcoholysis-extraction coupling method to extract phorbol alcohol from croton oil, the method alcoholysis and extraction are carried out synchronously, and alcoholysis-extraction coupling is beneficial to improve the efficiency of alcoholysis, and with the assistance of ultrasonic waves, alcoholysis ‑Extraction is faster and more efficient, saving time and improving the purity of phorbol. The method has the advantages of few operation steps, short time consumption, small solvent consumption and easy popularization and application.

Description

technical field [0001] The invention belongs to the technical field of extraction of natural medicines, and in particular relates to a method for separating phorbol by ultrasonic-assisted alcoholysis-extraction coupling technology. Background technique [0002] Croton tiglium L. is a plant of the genus Croton in the family Euphorbiaceae, also known as Jiangzi, Gangzi, Laoyangzi, etc. It was first recorded in "Shen Nong's Materia Medica", and it mainly grows in Fujian, Guangxi, and Guangdong. , Yunnan and other regions. Since ancient times, croton has been an important medicinal material used by doctors. Modern medicine believes that croton has good curative effects on digestive system diseases and malignant tumor diseases. Croton has natural advantages such as sufficient raw materials and low price, and as the substance with the highest phorbol ester content in nature, croton is undoubtedly the best raw material for extracting phorbol ester at present. [0003] Phorbol est...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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