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Method for separating and extracting cholesterol in lanolin alcohol

A technology of lanolin alcohol and cholesterol, applied in the direction of steroids, organic chemistry, etc., can solve the problems of large investment in supercritical fluid equipment, difficulty in natural cholesterol, high operating costs, etc., achieve less consumption of chemical auxiliary materials, and realize industrialization Production, light color effect

Inactive Publication Date: 2010-09-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method is short and does not require a large amount of organic solvent, but the investment in supercritical fluid equipment is large and the operating cost is high
[0009] The properties of higher fatty alcohols, sterols and triterpene alcohols contained in lanolin alcohol are very similar, so it is difficult to obtain high-purity natural cholesterol from it by one method

Method used

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  • Method for separating and extracting cholesterol in lanolin alcohol
  • Method for separating and extracting cholesterol in lanolin alcohol
  • Method for separating and extracting cholesterol in lanolin alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The method for separating cholesterol in lanolin alcohol by applying molecular distillation-solvent selective crystallization technology mainly comprises the following steps:

[0033] 1) Purification of lanolin alcohol by molecular distillation: take 50 g of raw material lanolin alcohol (10.5% cholesterol content), and enter it into a wiped-film molecular distillation device at a rate of 2.0 ml / min. The molecular distillation operating conditions are: system pressure 0.1Pa, preheating temperature 60°C, condensation surface temperature 50°C, distillation temperature 160°C, wiper speed 200rpm, and 28.6g light yellow light phase fraction was collected.

[0034] 2) The molecular distillation light phase fraction was heated in 858g of methanol until it was completely dissolved, then cooled to 20°C, kept warm for 8h, and vacuum filtered to obtain 10.29g of white needle-like crystals, which were crude lanosterol with a content of 70%.

[0035] 3) The filtrate in step 2) was di...

Embodiment 2

[0038] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0039]1) Purification of lanolin alcohol by molecular distillation: take 50 g of raw material lanolin alcohol (content of cholesterol 8.42%), and enter into a wiped-film molecular distillation device at a rate of 4.0 ml / min. The molecular distillation operating conditions are: system pressure 5Pa, preheating temperature 80°C, condensation surface temperature 70°C, distillation temperature 200°C, wiper speed 300rpm, and 29.2g light yellow light phase fraction was collected.

[0040] 2) Heat the molecular distillation light phase fraction in 467.2g of a mixed solvent composed of methanol and acetone (methanol volume percentage is 50%) until completely dissolved, then cool down to 10°C, vacuum filter after insulation for 8h, and obtain 11.43g of white Needle-like crystals, crude lanosterol with a content of 62.95%.

[0041] 3) The filtrate in step 2) was distilled under reduced pressu...

Embodiment 3

[0044] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0045] 1) Purification of lanolin alcohol by molecular distillation: take 50 g of raw material lanolin alcohol (cholesterol content 10.5%), and enter it into a wiped-film molecular distillation device at a rate of 6.0 ml / min. The molecular distillation operating conditions are: system pressure 0.4Pa, preheating temperature 70°C, condensation surface temperature 60°C, distillation temperature 180°C, wiper speed 250rpm, and 27.4g light yellow light phase fraction was collected.

[0046] 2) Heat the molecular distillation light phase fraction in 548g of a mixed solvent composed of methanol and acetone (methanol volume percentage 80%) until it is completely dissolved, then cool down to 15°C, keep warm for 8h and then vacuum filter to obtain 10.76g of white needles The crystal is crude lanosterol with a content of 67.61%.

[0047] 3) The filtrate in step 2) was distilled under reduced p...

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Abstract

The invention relates to a method for separating and extracting cholesterol in lanolin alcohol, which comprises the following steps: carrying out molecular distillation on lanolin alcohol, collecting the light-phase fraction which is refined lanolin alcohol, heating the refined lanolin alcohol in a mixed solvent of methanol and acetone until the refined lanolin alcohol is completely dissolved, and cooling to cooling temperature, wherein the remainder of the filtrate after reduced pressure distillation is the primary concentrate of cholesterol; heating to dissolve the primary concentrate of cholesterol in acetone, cooling to precipitate, filtering, and carrying out reduced pressure distillation on the filtrate to recover the solvent, wherein the balance is the secondary concentrate of cholesterol; heating to dissolve the secondary concentrate of cholesterol in an alcohol solvent, cooling to cooling temperature, keeping the temperature for 6-12 hours, and vacuum-filtering to obtain the white acerose cholesterol crude product; and recrystallizing the cholesterol crude product through a methanol-acetone mixed solvent to obtain the refined cholesterol product. The refined cholesterol product selectively recrystallizes through the solvent to obtain the byproduct lanosterol accounting for 63-70% and the cholesterol product of which the purity is more than 90%.

Description

technical field [0001] The invention relates to the technical field of separating and extracting cholesterol, in particular to a method for separating and extracting cholesterol in lanolin alcohol. Background technique [0002] Cholesterol is also known as cholesterol, and its oxidation product 7-dehydrocholesterol is synthesized into vitamin D after subcutaneous exposure to ultraviolet rays in sunlight 3 , and thus human vitamin D 3 Its unique biological properties and chiral characteristics, the cholesteric liquid crystal prepared from it as a skeleton is an important part, it has special optical properties that make it useful in many fields such as display devices and various optical components. Wide application prospects; natural biological activity makes cholesterol used in cosmetics to play the role of emollient, sunscreen, shrink pores, reduce wrinkles and restore skin elasticity. [0003] Lanolin alcohol is the product of lanolin saponification, containing 20-30% c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 丁辉张星华徐世民张艳华
Owner TIANJIN UNIV
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