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Method for extracting phorbol from croton oil by using Girard's reagent

A technology of geralt reagent and phorbol, applied in the field of natural medicine extraction, can solve the problems of many operation steps, large solvent consumption, long time consumption, etc., and achieve the effects of high purity, low solvent consumption, and short time consumption

Inactive Publication Date: 2020-06-12
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 there are many operation steps, long time consumption, large solvent consumption and difficulty in industrial application. There are still some defects and deficiencies in the relevant literature reports on separating phorbol alcohol, so the present invention provides a method for extracting phorbol alcohol from croton oil by utilizing Geraldt reagent

Method used

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  • Method for extracting phorbol from croton oil by using Girard's reagent
  • Method for extracting phorbol from croton oil by using Girard's reagent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] S1. Prepare various reagents:

[0032] (1) Preparation of the methanol saturated solution of Girard's reagent T: add a sufficient amount of Girard's reagent T (acetylhydrazide trimethylammonium chloride) solid to the methanol solvent, and place it in a 75°C water bath to reflux After cooling for 2 hours, a methanol-saturated solution of Gerard's reagent T was obtained, which was set aside.

[0033] (2) Preparation of dilute hydrochloric acid: it is prepared by adding 3 volumes of concentrated hydrochloric acid to 7 volumes of purified water and set aside.

[0034] (3) Preparation of alkaline alcohol solution: add enough anhydrous potassium carbonate to methanol with a content ≥ 99%, reflux in a water bath at 70°C for 2 hours, and prepare potassium carbonate-methanol saturated solution for subsequent use.

[0035] (4) Preparation of acidic methanol solution: add 10% volume concentrated hydrochloric acid to methanol with content ≥ 99% and mix evenly to form a 10% hydroch...

Embodiment 2

[0044] S1. Prepare various reagents:

[0045] (1) Methanol saturated solution of Girard's reagent P: add a sufficient amount of Girard's reagent P (acetylhydrazide pyridine chloride) solid to the methanol solvent, place it in a water bath at 75°C and reflux for 2 hours, after cooling Obtain the saturated methanol solution of Gerald's reagent P for later use.

[0046] (2) preparation of dilute hydrochloric acid: with embodiment 1.

[0047] (3) preparation of alkaline alcohol solution: with embodiment 1.

[0048] (4) preparation of acid methanol solution: with embodiment 1.

[0049] S2. Reaction with Girard Reagent: Accurately measure 2ml of croton oil, add Girard Reagent P saturated solution according to the ratio of material to liquid 1:15, stir and react at 50°C for 60min, then take out the reaction solution ;

[0050] S3, the concentration of reaction solution: with embodiment 1.

[0051] S4, remove croton oil: same as embodiment 1.

[0052] S5. pH adjustment-petroleum...

Embodiment 3

[0057] S1. Prepare various reagents:

[0058] (1) Preparation of the saturated methanol solution of Gerard's reagent T: same as in Example 1.

[0059] (2) preparation of dilute hydrochloric acid: with embodiment 1.

[0060] (3) preparation of alkaline alcohol solution: with embodiment 1.

[0061] (4) preparation of acid methanol solution: with embodiment 1.

[0062] S2. Reaction with Girard Reagent: Accurately measure 2ml of croton oil, add Girard Reagent T saturated solution according to the ratio of material to liquid 1:15, stir and react at 40°C for 90min, then take out the reaction solution ;

[0063] S3, the concentration of reaction solution: with embodiment 1.

[0064] S4, remove croton oil: same as embodiment 1.

[0065] S5. pH adjustment-petroleum ether extraction: same as in Example 1.

[0066] S6, concentrated petroleum ether phase: same as Example 1.

[0067] S7. Obtaining the crude product of phorbol alcohol: the same as in Example 1.

[0068] S8, the meth...

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Abstract

The invention relates to the technical field of natural medicine extraction, and particularly discloses a method for extracting phorbol from croton oil by using a Girard's reagent. The method comprises the following steps: S1, mixing 1 part of croton oil with 5-25 parts of a methanol saturated solution of a Girard's reagent according to a feed liquid volume ratio, and carrying out a stirring reaction at 18-50 DEG C for 30-180 min to obtain a reaction solution; S2, concentrating a reaction solution; S3, extracting and removing croton oil by using petroleum ether to obtain a water phase containing the phorbol Girard's reagent salt; S4, adjusting the pH value to 2-3, and extracting the phorbol in the water phase by using petroleum ether; S5, concentrating the petroleum ether phase to obtain an oily substance; and S6, carrying out alcoholysis, acidification and filtration on the oily substance to obtain a crude product of the phorbol. According to the method, carbonyl reacts with a Girard's reagent, and then a large amount of impurities can be removed by an extraction method due to different polarities of the components, so that a crude product of the phorbol with relatively high purity is obtained. The method has the characteristics of simplicity and convenience in operation, short time consumption and low solvent consumption, and is easy to popularize and apply industrially.

Description

technical field [0001] The invention belongs to the technical field of natural medicine extraction, and in particular relates to a method for extracting phorbol from croton oil by using Gerard reagent. Background technique [0002] Croton tiglium L. is a plant of the genus Croton in the Euphorbiaceae (Euphorbiaceae), also known as Jiangzi, Gangzi, Laoyangzi, etc. It was first recorded in "Shen Nong's Materia Medica", mainly grown in Fujian, Guangxi, Guangdong, Yunnan and other regions. From ancient times to the present, croton is an important medicinal material used by doctors. Modern medicine believes that croton has a good curative effect on digestive system diseases and malignant tumor diseases. Croton has natural advantages such as sufficient raw materials and low price, and as the material with the highest phorbol ester content in nature, croton is undoubtedly the best raw material for extracting phorbol ester at present. [0003] Phorbol esters have pleiotropic biolo...

Claims

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Application Information

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IPC IPC(8): C07C45/78C07C45/81C07C45/85C07C45/80C07C49/727
CPCC07C45/78C07C45/80C07C45/81C07C45/85C07C2603/40C07C49/727
Inventor 范杰平高意张风炎
Owner NANCHANG UNIV
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