Vitamin D separating, purifying and crystallizing method

A vitamin and crystallization technology, applied in the direction of organic chemistry, can solve the problems of high safety requirements, low yield, high loss of vitamin D, etc., and achieve the effects of reducing environmental pollution, simple process, and cost reduction

Active Publication Date: 2005-12-21
TAIZHOU HISOUND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because it is a chemical separation method, there is a lot of loss of vitamin D, and there are incomplete esterification, so the yield is low
The chromatographic method uses benzene as a solvent, which is highly toxic.
The s

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] According to the weight ratio of 0.4-0.6:1, or 50 grams of vitamin D with 23.86 million IU 3 Dissolve actinic oil (crude product) in 100 grams of petroleum ether, and evenly add it to a chromatographic column with an inner diameter of 4 cm, a height of 1 meter, and 1 kg of alumina through a porous plate, and elute with ethyl acetate after the flow is over Separate and collect in sections of 5 liters each, tracked with thin plates. Pure vitamin D that will be collected 3 The components were evaporated to dryness under reduced pressure, added ethyl acetate as a crystallization solvent, frozen and crystallized, filtered for 12 hours, and then vacuum-dried to obtain needle-shaped vitamin D 3 8.2 grams of crystals, with a purity of 99.7%, an optical rotation of 111.0°, and vitamin D that meets the requirements of the Pharmacopoeia 3 .

Embodiment 2

[0023] 400 grams of 24.52 million IU vitamin D 3 Actinic oil (crude product) was dissolved in 800 milliliters of n-hexane, added to a chromatographic column with an inner diameter of 10 centimeters, a height of 2 meters, and 10 kilograms of alumina inside, and was eluted and separated with dichloromethane after the flow was completed, and segmented Collect, 500ml each, track with a thin plate. Evaporate the collected pure vitamin D components to dryness under reduced pressure, add 200ml of crystallization solvent methyl ester methyl ester, freeze and crystallize, filter, and vacuum-dry to obtain needle-shaped vitamin D 3 65.5 g of crystals. The purity is 100.1%, the optical rotation is 111.9°, and it meets the requirements of Pharmacopoeia for vitamin D 3 .

Embodiment 3

[0025] 50 grams of 18 million IU of vitamin D 2 The actinic oil was dissolved in 100 milliliters of ethyl acetate, added into the alumina adsorption column as in Example 1, and operated according to the procedures in Example 1. Vitamin D that will be collected 2 The components are crystallized with methanol to obtain 6.5 grams of needle-shaped vitamin D that meets the requirements of the Pharmacopoeia 2 crystallization.

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PUM

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Abstract

This invention involves the separating purification and crystallization method to vitamin D2, D3, D4. Dissolve the actinic oil of vitamin D in absorption solvent by weight ratio of 0.3-3, feed it into chromatography column which has installed alumina inside; Elute separating by elution solvents, collect by subsection, track the part of pure vitamin D with the folium analytical approach, until vitamin D is totally washed out; The pure vitamin D component that has been collected decompresses to remove solvents, put into the crystal solvent, when -5 to -10 deg. C, freeze and crystal, filter after 10-16 hours, vacuum getting dry vitamin D crystallisation. This invention improves accepting rate and purity, the craft is simple, lower costs and has reduced the environmental pollution.

Description

technical field [0001] The invention belongs to the field of photochemical synthesis of vitamin D, in particular to vitamin D 2 、D 3 、D 4 Methods of purification, separation and crystallization. Background technique [0002] Vitamin D is one of the important vitamins essential for human health, normal growth and reproduction of livestock and poultry. There are a lot of impurities such as tachysterol and photosterol and residual 7-dehydrocholesterol in the products of photochemical synthesis of vitamin D. These by-products Due to the similar structure and properties, it seriously affects the separation, purification and crystallization of vitamin D. Among them, tachysterol is also a toxic by-product, so it must be separated and removed. The classic method to remove these impurities is to adopt 3,5-dinitrobenzoyl chloride or butyryl chloride esterification crystallization separation and purification method. This method has a long process flow, high toxicity and a lot of thr...

Claims

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Application Information

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IPC IPC(8): C07C401/00
Inventor 杨琳陈济谷
Owner TAIZHOU HISOUND PHARMA CO LTD
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