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Preparation method and device of hydroxycobalamin salt

A hydroxocobalamin salt and a preparation device technology, which is applied in the field of medicine, can solve the problems of large amount of post-treatment solvent, unfavorable industrialization, macroporous resin residue, etc., and achieve simple reaction product components, shorten production cycle, and reduce pH value Effect

Pending Publication Date: 2022-07-01
INST OF MATERIA MEDICA CHINESE ACAD OF MEDICAL SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of preparation method does not need to use toxic reagents, and the conversion rate is relatively high, but the reaction and post-treatment solvent (acetone) used in the production process is relatively large, and the macroporous resin is used for purification, which may introduce macroporous resin residues, cumbersome operation, and work. Low efficiency, not conducive to the realization of industrialization

Method used

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  • Preparation method and device of hydroxycobalamin salt
  • Preparation method and device of hydroxycobalamin salt
  • Preparation method and device of hydroxycobalamin salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1: Preparation of Hydroxocobalamin acetate

[0048] Add 90g of methylcobalamin and 6000ml of deionized water to the stirred reaction flask, and after dissolving, use 80wt% glacial acetic acid to adjust the pH of the reaction solution to 2.0-2.8; in a state of stirring, the temperature of the ice-water bath is controlled at 20-30°C, and at 10,000- Under the light of 15000 lux, the pressurized pump was used to ventilate the air for 4-7 hours, and the raw material methylcobalamin was monitored by HPLC to be less than or equal to 0.1%, and the reaction was terminated.

[0049] Slowly add 60000ml of acetone to the above reaction system, stand at -20~-10℃ for crystallization for 16h, filter, wash the filter cake with cold acetone-water mixed solution, and dry at room temperature for about 12h to obtain 81.0g of dark red crystalline solid, yield: 90%.

[0050] The HPLC chromatogram was measured, and the test conditions of the HPLC chromatogram were referred to the USP...

Embodiment 2

[0051] Example 2: Preparation of Hydroxocobalamin Sulfate

[0052] Add 120g of methylcobalamin and 6000ml of deionized water to a stirred reaction flask, and after dissolving, use 10wt% sulfuric acid to adjust the pH of the reaction solution to 2.0-2.8; in a stirring state, the temperature of the ice-water bath is controlled at 20-30°C, and the temperature is 10,000-15,000 lux. Under the light, the pressurized pump was used to blow air for 4-7 hours at the same time, and the raw material methylcobalamin was monitored by HPLC to be less than or equal to 0.1%, and the reaction was terminated.

[0053] Slowly add 60000ml of acetone to the above reaction system, stand at -20~-10℃ for crystallization for 16h, filter, wash the filter cake with cold acetone-water mixed solution, and dry at room temperature for about 12h to obtain 110.40g of dark red crystalline solid, yield: 92%.

[0054] HPLC chromatogram was measured, and the results are shown in the attached figure 2 , with a p...

Embodiment 3

[0055] Example 3: Preparation of Hydroxocobalamin Hydrochloride

[0056] 180.0g of methylcobalamin and 6000ml of deionized water were added to the stirred reaction flask, and after dissolving, 10wt% hydrochloric acid was used to adjust the pH of the reaction solution to 2.0~2.8. Under the light of 15000 lux, the pressure pump was used to blow air at the same time for about 4 to 7 hours, and the raw material was monitored by HPLC to be less than or equal to 0.1%, and the reaction was terminated.

[0057] Slowly add 60000ml of acetone to the above reaction system, stand at -20~-10°C for crystallization for 16h, filter, wash the filter cake with cold acetone-water mixed solution, and dry at room temperature for about 12h to obtain 167.4g of dark red crystalline solid with a yield of 167.4g. : 93%.

[0058] HPLC chromatogram was measured, and the results are shown in the attached image 3 , with a purity of 99.3%.

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Abstract

The invention belongs to the technical field of medicine, and provides a preparation method and device of hydroxycobalamin salt, the method comprises the following steps: S1) taking mecobalamin, dissolving mecobalamin with water, and adjusting the pH to 2.0-5.0 with acid to obtain a mecobalamin supersaturated solution to be reacted; s2) in a stirring state, irradiating the to-be-reacted liquid with 15000-50000lux strong light, simultaneously and continuously blowing in oxygen-containing gas, and controlling the temperature to be 5-30 DEG C for reaction, so that mecobalamin is converted into hydroxycobalamin salt to obtain a reaction liquid; and S3) adding acetone into the reaction liquid, and standing to separate out crystals, thereby obtaining the hydroxycobalamin salt. The method and the device for preparing the hydroxycobalamin salt are simple, convenient, effective, low in cost and environment-friendly, the hydroxycobalamin salt with good stability and high purity can be obtained, and industrial popularization and application are facilitated.

Description

technical field [0001] The present application relates to the technical field of medicine, in particular to a preparation method and device of hydroxocobalamin. Background technique [0002] Vitamin B12 is the largest and most complex one of the known vitamins. In fact, it is not a single substance, but a series of closely related compounds with very similar structures and similar activities. Vitamin B12 (also known as cobalamin) remains in the body for a long time and is known as long-acting B12. It is widely used as a treatment and nutritional supplement in the fields of clinical medicine, feed and food. Vitamin B12 is the only vitamin that contains metallic elements, which are octahedral structures centered on metallic cobalt ions. Vitamin B12 is cobalamin, which is a general term for a class of corrin compounds containing Co. According to the different functional groups of Co, it is divided into deoxyadenosylcobalamin (abbreviated as adenosylcobalamin) and methylcobala...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H23/00C07H1/00C07H1/06A61K31/714A61K9/08A61K47/02A61K47/12A61P7/06A61P1/16A61P17/00A61P39/02A61P3/02A61P29/00A61P25/04B01J19/12
CPCC07H23/00C07H1/00C07H1/06A61K31/714A61K9/08A61K9/0019A61K47/02A61K47/12A61P7/06A61P1/16A61P17/00A61P39/02A61P3/02A61P29/00A61P25/04B01J19/12C07B2200/07
Inventor 冯文化马春英杨柳修利伟谈敦潮苏晓会吴诚邹德超陈先红
Owner INST OF MATERIA MEDICA CHINESE ACAD OF MEDICAL SCI
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