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Method for separating and purifying solanesol by urea column chromatography

A technology for separation and purification of solanesol, applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., can solve the problems of lack of wax removal procedures and low product purity, and achieve large batches, high product purity, and easy industrialization Effect

Active Publication Date: 2011-02-16
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned methods generally lack effective wax removal procedures. In the products obtained by crystallization and recrystallization, a certain amount of waxy substances will still remain, and the product purity is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Extraction saponification: the 10g solanesol extract obtained by extracting potato leaves with petroleum ether and having a solanesol content of 20wt% is fully stirred in 100g KOH-methanol solution of 1wt%, saponified at 30°C for 4h, The reaction solution was neutralized with hydrochloric acid, concentrated to obtain saponified solanesol extract;

[0028] (2) Preparation of urea stationary phase: 100g urea was dissolved in methanol, 10g gac was added in the methanol solution, and rotary evaporation was performed to obtain the stationary phase;

[0029] (3) Urea column chromatography: the prepared stationary phase is packed into a column, then the saponified solanesol extract is put on the column, and petroleum ether is injected into the chromatography column at a uniform speed for elution, and the eluted fractions of different periods are collected, and the enriched The eluted fractions containing solanesol were combined, concentrated and evaporated to dryness;

[...

Embodiment 2

[0032] (1) Saponification of extract: 20 g of solanesol extract obtained by extracting potato leaves with ethanol and having a solanesol content of 20 wt %, fully stirred in 100 g of KOH-ethanol solution of 5 wt %, saponified at 40 ° C for 3.5 h, The reaction solution is neutralized with sulfuric acid, concentrated to obtain saponified solanesol extract;

[0033] (2) Preparation of urea stationary phase: 100g of urea was dissolved in methanol, 100g of silica gel was added in the methanol solution, and the stationary phase was obtained by rotary evaporation;

[0034] (3) Urea column chromatography: the prepared stationary phase is packed into a column, then the saponified solanesol extract is put on the column, and n-hexane is injected into the chromatography column at a constant speed for eluting, and the eluted fractions of different periods are collected, and the enriched The fractions containing solanesol were combined, concentrated and evaporated to dryness.

[0035] (4) ...

Embodiment 3

[0037] (1) Extraction saponification: 50 g of solanesol extract obtained by ethanol extraction of tobacco leaves with a solanesol content of 10 wt %, fully stirred in 100 g of NaOH-methanol solution of 30 wt %, saponified at 50 ° C for 3 h, and the reaction solution Neutralize with hydrochloric acid, concentrate to obtain saponified solanesol extract;

[0038] (2) Preparation of urea stationary phase: 100g urea was dissolved in 80wt% ethanol aqueous solution, 200g aluminum oxide was added in the methanol solution, and the stationary phase was obtained by rotary evaporation;

[0039](3) Urea column chromatography: the prepared stationary phase is packed into a column, then the saponified solanesol extract is put on the column, and chloroform is uniformly injected into the chromatography column for eluting, and the eluted fractions of different periods are collected, and the The eluted fractions of solanesol were combined, concentrated and evaporated to dryness.

[0040] (4) cr...

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PUM

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Abstract

The invention relates to a method for separating and purifying solanesol by urea column chromatography. The method comprises the following steps of: fully stirring solanesol concrete in alcoholic-alkaline solution; saponifying the mixture at the temperature of between 30 and 80 DEG C for 0.5 to 4 hours; neutralizing the reaction solution by using acid; concentrating to obtain saponified solanesolconcrete; dissolving urea into a loaded solvent; adding carriers to ensure that the urea is loaded on the carriers; removing the solvent to prepare a stationary phase; loading the prepared stationaryphase to a column; loading the saponified solanesol concrete to the column; eluting by injecting a mobile phase into a chromatography column at a uniform speed; collecting elution partitions at different stages; merging the elution partitions rich in the solanesol; concentrating and evaporating to dryness; dissolving solanesol solution after the urea column chromatography into methanol, ethanol or acetonitrile in reflux; saturating the solution; freezing and crystallizing; filtering; and drying to obtain the solanesol. The method has the advantages of mild operation condition, high process yield, high product purity, simple process and low operation cost.

Description

technical field [0001] The invention relates to a method for separating and purifying solanesol from potato leaves and tobacco leaf extracts. Background technique [0002] Solanesol Solanesol is a polyprenyl alcohol with the molecular formula C 45 h 74 The simplified structure of O is H[CH 2 C(CH 3 )CHCH 2 ] 9 OH, relative molecular weight: 631, pure product is white waxy solid, melting point 41°C. Weak polarity, easily soluble in organic solvents. Solanesol is a long-chain fatty alcohol with multiple non-conjugated double bonds in its structure and has a very strong ability to absorb free radicals. It mainly exists in tobacco leaves, tobacco stems, and potato leaves. Solanesol is an important pharmaceutical intermediate, which can be used to synthesize vitamin K 2 and coenzyme Q 10 It can also be used as a raw material for the synthesis of some antiallergic drugs, antiulcer drugs, hypolipidemic drugs or anticancer drugs, and it is also a substance with medical effe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C33/02
Inventor 侯相林邓天昇韩蕊蕊
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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