Method for separating vitamin D3 from tachysterol T3

A vitamin and tachysterol technology, applied in the field of chemical engineering, can solve the problems of small processing capacity, low recovery rate, and large solvent consumption

Active Publication Date: 2012-07-11
ZHEJIANG UNIV
View PDF9 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] existing vitamin D 3 The separation and purification methods are as follows: U.S. Patent US3665020 uses 3,5-dinitrobenzoyl chloride or butyryl chloride esterification crystallization separation and purification method, but this method has many steps and serious environmental pollution, and in view of the limitations of chemical separation methods , the yield is lower
Preparation of vitamin D from isomer mixture by supercritical column chromatography introduced in Chinese patent ZL99108675.9 3 or precursor vitamin D 3 The method requires high equipment and needs to be operated in a high-pressure environment, which is costly and difficult to industrialize
Chinese patent ZL200510040330.4 reports the separation of vitamin D by alumina column chromatography and freeze crystallization 3 , can be separated to obtain products with higher purity, which has certain application value, but at the same time, there are shortcomings such as small processing capacity, low recovery rate, large solvent consumption, and difficulty in reusing the adsorbent.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for separating vitamin D3 from tachysterol T3
  • Method for separating vitamin D3 from tachysterol T3
  • Method for separating vitamin D3 from tachysterol T3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Dissolve 7-dehydrocholesterol in a mixture of n-hexane, ethanol, and 2,6-di-tert-butyl-p-methoxyphenol, and conduct a photochemical reaction at 20°C for 1 hour. The resulting product is concentrated and subjected to silica gel column chromatography get vitamin d 3 tachysterol T 3 The sum of the mass percentages is 95%, vitamin D 3 tachysterol T 3 The mass ratio of actinic oil pretreatment is 4:1. Synthesis of actinic oil pretreatment with n-hexane to form vitamin D 3 tachysterol T 3 The total concentration is 7.5 grams per liter of raw material liquid, with dimethyl sulfoxide as extractant, with n-hexane as detergent, the flow ratio of extractant, detergent, raw material liquid three is 7.5:5:1,40 at figure 1 Fractional extraction is carried out in the fractionation extraction device shown (there are 10 stages in the extraction section and 10 stages in the washing section). The fractionation extraction is divided into an extraction section and a washing section. ...

Embodiment 2

[0042] Dissolve 7-dehydrocholesterol in a mixture of n-hexane, ethanol, and 2,6-di-tert-butyl-p-methoxyphenol, and conduct a photochemical reaction at 20°C for 1 hour. The resulting product is concentrated and subjected to silica gel column chromatography get vitamin d 3 tachysterol T 3 The sum of the mass percentages is 96%, vitamin D 3 tachysterol T 3 The mass ratio of actinic oil pretreatment is 6:1. Formulating actinic oil pretreatment with n-heptane into vitamin D 3 tachysterol T 3 The total concentration is 80 grams per liter of raw material liquid, with N-methylpyrrolidone as extractant, with n-heptane as detergent, the flow ratio of extractant, detergent, raw material liquid three is 3.6:8:1, -20°C at figure 1 Fractional extraction is carried out in the fractionation extraction device shown (there are 8 stages in the extraction section and 8 stages in the washing section). The fractionation extraction is divided into an extraction section and a washing section. ...

Embodiment 3

[0044]Dissolve 7-dehydrocholesterol in a mixture of n-hexane, ethanol, and 2,6-di-tert-butyl-p-methoxyphenol, and conduct a photochemical reaction at 20°C for 1 hour. The resulting product is concentrated and subjected to silica gel column chromatography get vitamin d 3 tachysterol T 3 The sum of the mass percentages is 94%, vitamin D 3 tachysterol T 3 The mass ratio of actinic oil pretreatment is 5:1. Formulating actinic oil pretreatment with cyclohexane to form vitamin D 3 tachysterol T 3 The total concentration is 0.5 grams per liter of raw material liquid, with 1,2-propanediol as extractant, with cyclohexane as detergent, the flow ratio of extractant, detergent, raw material liquid three is 60:15:1, 30°C at figure 1 Fractional extraction is carried out in the fractionation extraction device shown (there are 10 stages in the extraction section and 10 stages in the washing section). The fractionation extraction is divided into an extraction section and a washing sectio...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
quality scoreaaaaaaaaaa
quality scoreaaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for separating vitamin D3 from tachysterol T3. According to the method, high-purity vitamin D3 and tachysterol T3 are efficiently separated from a mixture containing the vitamin D3 and the tachysterol T3 by a fractional extraction method, wherein a medium polar to polar organic solvent, ionic liquid or a binary mixed solvent consisting of the ionic liquid and the medium polar to polar organic solvent serves as an extracting agent. The method has the advantages of high separation efficiency, low solvent consumption, high yield, safety, environmental friendliness, easiness in industrialized production and the like.

Description

technical field [0001] The invention relates to a method for separating compounds, belongs to the technical field of chemical engineering, and in particular relates to a method for separating vitamin D 3 tachysterol T 3 Methods. Background technique [0002] Vitamin D, also known as anti-rickets vitamin, is one of the essential vitamins for human health, normal growth and reproduction of livestock and poultry, and has the functions of regulating calcium and phosphorus metabolism, promoting bone growth, regulating cell growth and differentiation, and regulating immune function effect. Vitamin D exists in many forms, two of the most important being vitamin D 2 (ergocalciferol) and vitamin D 3 (cholecalciferol). [0003] Vitamin D 3 (Vitamin D 3 , the structural formula is as figure 1 (shown) synthesis generally starts from cholesterol, which is first transformed into 7-dehydrocholesterol through a series of chemical reactions, and then undergoes a ring-opening reaction...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCY02P20/54
Inventor 任其龙梁瑞斯鲍宗必苏宝根邢华斌杨启炜杨亦文苏云
Owner ZHEJIANG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap