Purification process of vitamin K1

A vitamin and process technology, applied in the field of purification process of vitamin K1, can solve problems such as the difficult problem of vitamin K1 to prepare vitamin K1 raw materials, and achieve the effects of saving time and labor cost, simple operation, and saving solvent consumption

Active Publication Date: 2020-08-25
ZHEJIANG CHENGYI PAHRMACEUTICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Purification of vitamin K1 is a difficult problem in the preparation of vitamin K1 raw materials, especially how to remove the above-mentioned impurities, and there are very few reports in the prior art

Method used

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  • Purification process of vitamin K1
  • Purification process of vitamin K1
  • Purification process of vitamin K1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] VK1 column chromatography process (single batch of crude product 9kg batch)

[0064] 1. Process 1: DAC600 column chromatography (C18 reversed-phase silica gel column)

[0065] 1. Material and equipment information

[0066] 1-1 Material ratio

[0067] Material name Proportion (W / W) Feeding amount (kg) Crude VK1 1 9.00 Methanol 200 2000 ethyl acetate 94.44 850

[0068] 1-2 Device information

[0069]

[0070] 2. Experimental conditions

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Abstract

The invention relates to a purification process of vitamin K1, which comprises the following steps: 1, carrying out chromatographic purification on synthesized crude VK1 by using a DAC600 preparativechromatographic column taking a C18 reversed-phase silica gel column as a filler and using a mixed solution of methanol and ethyl acetate as a mobile phase; and 2, further carrying out chromatographicpurification on the VK1 obtained in the step 1 and subjected to chromatographic purification by the reversed-phase silica gel column by taking normal-phase chromatographic silica gel as a filler andtaking normal hexane as a mobile phase.

Description

Technical field: [0001] The invention relates to a method for purifying raw materials, in particular to a process for purifying vitamin K1. Background technique: [0002] Vitamin K1, English name Vitamin K1, alias: phytonadione; 2-methyl-3-(3,7,11,15-tetramethylhexadecan-2-enyl)-1,4-naphthoquinone, Molecular formula C31H46O2, molecular weight 450.71, structural formula: [0003] [0004] Vitamin k1 is used for vitamin and mineral deficiency medicine. [0005] Vitamin K1 Injection is a product in the 2009 edition of the National Essential Medicines List, and is mainly used for the treatment of various hemorrhagic diseases caused by vitamin K deficiency. Clinically used in the prevention and treatment of hypothrombin, vitamin K1 deficiency, neonatal spontaneous hemorrhage, and bleeding caused by obstructive jaundice, biliary fistula, chronic diarrhea, etc., caused by coumarins, sodium salicylate, etc. hypoprothrombinemia. Vitamins also have analgesic and relieving bronc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/10C07C50/14
CPCC07C46/10C07C2602/10C07C50/14
Inventor 王志伟沈海东陈小芳陈燕燕赵师靖
Owner ZHEJIANG CHENGYI PAHRMACEUTICAL
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