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Purification method for vitamin D3

A purification method and vitamin technology, which is applied in the field of vitamins, can solve problems such as difficult industrial application, high industrial cost, and expensive modified silica gel, and achieve the effects of mild reaction, low application cost, and no solid waste discharge

Active Publication Date: 2019-12-03
XIAMEN KINGDOMWAY VI TAMIN INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The supercritical column separation method requires the use of high-pressure equipment above 7MPa, which requires high equipment safety and requires expensive modified silica gel. The industrialization cost is high and it is difficult to apply in industrialization

Method used

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  • Purification method for vitamin D3
  • Purification method for vitamin D3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Put resinous vitamin D in the dissolution kettle 3 Crude product (unit 25.5 million IU / g) 20g (0.052mol), add 5.04g (0.057mol) butyric acid, dissolve in 160ml n-hexane, use a pump to pass through DN10×500 fat containing 20g Novozymes 435 at a flow rate of 0.65ml / min Enzyme column A (residence time 1h), pass through the column at a temperature of 35°C to obtain an esterification solution with a conversion rate of 99.5%, use a pump to inject 95% water into the extraction column A according to the volume flow ratio of methanol water:esterification solution 0.8:1 Extract with methanol and esterification solution to obtain the upper organic phase, control the internal temperature to be less than 35°C and concentrate to dryness, and the concentrated n-hexane can be reused to obtain vitamin D 3 Esters, dissolved in 24ml of acetone, slowly cooled to -20°C, left to stand for 3 hours, filtered, washed and dried to obtain 98.8% vitamin D 3 Esters 12.79g, Vitamin D 3 The total yi...

Embodiment 2

[0058] Put resinous vitamin D in the dissolution kettle 3 Crude product (25.5 million IU / g) 20g (0.052mol), add 6.87g (0.078mol) butyric acid, dissolve in 160ml n-hexane, use a pump to pass through DN10×500 fat containing 20g Novozymes 435 at a flow rate of 0.65ml / min Enzyme column A (residence time 1h), the column temperature is 35°C, and the esterification liquid is obtained, the conversion rate is 99.8%, and the volume flow ratio of methanol water: esterification liquid is 0.8:1, and the 95% water content is injected into the extraction tower A respectively. Extract with methanol and esterification solution to obtain the upper organic phase, control the internal temperature to be less than 35°C and concentrate to dryness, and the concentrated n-hexane can be reused to obtain vitamin D 3 Esters, dissolved in 24ml of acetone, slowly cooled to -20°C, left to stand for 3 hours, filtered, washed and dried to obtain 98.6% vitamin D 3 Esters 12.50g, Vitamin D 3 The total yield o...

Embodiment 3

[0060] Put resinous vitamin D in the dissolution kettle 3 Crude product (unit 25.5 million IU / g) 20g (0.052mol), add 4.52g (0.029mol) butyric anhydride, dissolve in 160ml n-hexane, use a pump to pass through DN10×500 fat containing 20g Novozymes 435 at a flow rate of 0.65ml / min Enzyme column A (residence time 1h), pass through the column at a temperature of 35°C to obtain an esterification solution with a conversion rate of 99.6%, use a pump to inject 95% water into the extraction column A according to the volume flow ratio of methanol water:esterification solution 0.8:1 Extract with methanol and esterification solution to obtain the upper organic phase, control the internal temperature to be less than 35°C and concentrate to dryness, and the concentrated n-hexane can be reused to obtain vitamin D 3 Esters, dissolved in 24ml of acetone, slowly cooled to -20°C, left to stand for 3 hours, filtered, washed and dried to obtain 98.8% vitamin D 3 Esters 12.80g, Vitamin D 3 The tot...

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Abstract

The invention discloses a purification method for vitamin D3. The purification method specially comprises the following steps of: taking a vitamin D3 crude product as a substrate, and mixing with a weak organic acid or acid anhydride in a non-aqueous phase solvent; carrying out esterification through a lipase column A; carrying out extraction by an extraction agent; concentrating an obtained organic layer; then, after a crystallization solvent is added for solving, carrying out cooling crystallization, and filtering and drying to obtain a vitamin D3 ester crystal; after dissolving is carried out, carrying out saponification through a lipase column B, and then, carrying out extraction; enabling an obtained organic layer to return to the lipase column B to carry out saponification and extraction, and stopping circulation until vitamin D3 ester residues in an organic phase are less than 1wt%; finally, concentrating, crystallizing and drying the organic layer to obtain vitamin D3 crystal quality goods; and after a crystalized mother liquor is processed, reusing the crystalized mother liquor as the substrate. The method has a higher yield, high-toxicity raw materials are not used, mostraw materials can be reused, the emission of waste residues and waste water difficult in processing is avoided, and the purification method is an environmentally-friendly and economic purification method, which has low cost, for vitamin D3.

Description

technical field [0001] The invention relates to the field of vitamins, in particular to a vitamin D 3 purification method. Background technique [0002] Vitamin D 3 , also known as cholecalciferol, has the physiological functions of promoting intestinal calcium absorption, regulating calcium and phosphorus metabolism, and inducing bone calcium and phosphorus deposition. It can promote bone growth and prevent rickets. It is also used in large doses for skin tuberculosis, skin and Various types of mucous membrane lupus erythematosus and so on. [0003] Vitamin D synthesized by photochemical reaction 3 Contains tachysterol, photosterol and residual raw material 7-dehydrocholesterol produced by side reactions, generally only 20-30 million IU / g of vitamin D can be obtained 3 , these by-products are difficult to further separate and purify because of their similar structures and properties. [0004] current vitamin D 3 Purification methods mainly include chemical method and ...

Claims

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Application Information

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IPC IPC(8): C12P7/02
CPCC12P7/02
Inventor 蔡育森余曦何剑洋王志强许德兴魏高宁
Owner XIAMEN KINGDOMWAY VI TAMIN INC
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