Method for extracting cholesterol from lanoline

A technology of cholesterol and lanolin, which is applied in the preparation of steroids, chemical instruments and methods, steroids, etc., to achieve the effects of easy post-processing, easy operation, and simple processing procedures

Inactive Publication Date: 2007-05-09
ZHEJIANG UNIV
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  • Abstract
  • Description
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  • Application Information

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Examples

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Effect test

Embodiment 1

[0018] Transesterification reaction: put 500g of lanolin raw material and 1000ml of anhydrous methanol into a 2500ml three-necked flask, heat in a water bath to maintain the temperature at 70°C, slowly add 50g of 40% sodium methoxide methanol solution, and react for 2h at a stirring speed of 25rpm to obtain a brown color. Viscous liquid. After the reaction was terminated, 13 g of phosphoric acid was added to the reaction solution to neutralize the excess alkali.

[0019] Short-path distillation: Preheat the neutralized reaction solution to 110°C, and enter the short-path distillation device at a rate of 0.18L / h. The operating conditions of short-path distillation are: primary heating temperature 130°C, vacuum degree 150Pa; secondary heating temperature 200°C, vacuum degree 0.1Pa, short-path distiller scraper speed 400rpm, condensing temperature 50°C. 218 g of light-phase fractions from secondary distillation were collected, which was a pale yellow crude product of cholesterol...

Embodiment 2

[0025] Transesterification: same as Example 1.

[0026] Short-path distillation: Preheat the neutralized reaction solution to 110°C, and enter the short-path distillation device at a rate of 0.18L / h. The operating conditions of short-path distillation are: primary heating temperature 130°C, vacuum degree 150Pa; secondary heating temperature 200°C, vacuum degree 0.1Pa, short-path distiller scraper speed 400rpm, condensing temperature 50°C. 218 g of light-phase fractions from secondary distillation were collected, which was a pale yellow crude product of cholesterol, and the content of cholesterol was 22.9%.

[0027] Chromatographic separation: 36g of crude cholesterol product was weighed and dissolved in 300ml of petroleum ether / toluene (70 / 30, v / v) mixture at 30°C, and uploaded to a φ5cm×25cm chromatography at a rate of 0.1BV / h. On the column, the adsorption filler used in the chromatography column is 500 g of 90-120 mesh silica gel. After the sample is loaded, use 70:30 (v / ...

Embodiment 3

[0030] The steps of transesterification, short-path distillation and chromatographic separation are the same as those in Example 1.

[0031] The cholesterol white powder obtained by chromatography separation I and chromatography separation II in Example 1 was mixed, dissolved in petroleum ether and evaporated to dryness to obtain 20.1 g of white powder with a cholesterol purity of 89.1%.

[0032] 10.0 g of the above cholesterol was taken in a three-necked flask, heated in a water bath, and dissolved in 255 ml of acetone at 56°C. Then, it was cooled to a final temperature of 30°C in an air bath with stirring at 10 rpm, and the crystals were aged by maintaining the final temperature of 30°C for 3 hours. Finally, the crystals were filtered and dried to obtain 7.2 g of cholesterol white needle-shaped crystals with a purity of 93.1% and a yield of 75.2%.

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Abstract

This invention discloses a method for extracting high-purity cholesterol from lanolin. The method comprises: (1) dissociating cholesterol from lanolin by transesterification reaction; (2) performing short-path distillation to obtain cholesterol crude product; (3) purifying by silica gel column chromatography; (4) crystallizing to obtain refined cholesterol with purity higher than 95% and yield higher than 70%. The method has such advantages as high product consumption, little pollution, simple process and easy operation, thus is suitable for mass production.

Description

technical field [0001] This patent relates to a method for extracting cholesterol, specifically a method for extracting high-purity cholesterol from lanolin by adopting a new process of transesterification-short-path distillation-column chromatography-crystallization. Background technique [0002] Cholesterol is an important pharmaceutical intermediate, through which vitamin D3 and a series of steroid anti-inflammatory drugs can be synthesized; in addition, cholesterol has become an indispensable additive in high-end cosmetics due to its excellent lubricating properties to the skin. At present, there are roughly two ways to prepare cholesterol: one is to extract from the brainstem and internal organs of animals; the other is to extract from lanolin. Due to doubts about the potential harm of disease-causing genes in animal organs to humans, the former route is gradually being replaced by the latter, which is increasingly restricted by the international market. [0003] Lanol...

Claims

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Application Information

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IPC IPC(8): C07J9/00C07J75/00
Inventor 杨亦文魏作君苏宝根吴彩娟苏云黄梅潘水泉吴平东任其龙
Owner ZHEJIANG UNIV
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