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Preparation method and application of vitamin B6 impurity compound

A technology of vitamins and compounds, applied in organic chemistry, instruments, analytical materials, etc., can solve problems such as limitations, impurity-free preparation methods, and impact on the safety of clinical drug use of products, and achieve the effect of low-cost and large-scale preparation

Pending Publication Date: 2022-05-06
TIANJIN CREATRON BIOTECHNOLOGY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vitamin B 6 The use of injection includes subcutaneous injection and intravenous injection. If the impurity research is not thorough, it will seriously affect the safety of clinical drug use of the product, and the existing official pharmacopoeias have no strict restrictions on specific impurities.
"New dimer of pyridoxol (vitamin B 6 )” Journal of Organic Chemistry (1969), 34(6), 1993-6, “Analysis of photo- and heat-reaction products of vitamin B 6 》Bitamin (1999), 73(10), 599-606, JP11209221A, JP11080122A reported the degradation pathway of impurities, but there is no detailed preparation method of impurities, and vitamin B cannot be provided 6 Preparation method of impurity reference substances that must be used in quality control and quality research

Method used

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  • Preparation method and application of vitamin B6 impurity compound
  • Preparation method and application of vitamin B6 impurity compound
  • Preparation method and application of vitamin B6 impurity compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0122] Example 1 Preparation and identification of compounds of formula (II)

[0123] 1. Preparation of enriched mother liquor

[0124] Preparation of enriched mother liquor containing the compound of the above formula (II): take vitamin B 6 Raw material about 2g, add 30%H 2 o 2 About 10ml, heated in a water bath at 80°C for 8 hours, took it out, put it in an oven at 60°C overnight, and added 30% H 2 o 2 From about 10ml", repeat 3 cycles to obtain the enriched mother liquor of the compound of formula (II), which is yellow and clear liquid, and is sealed and stored at 2~8°C.

[0125] Alternatively, the temperature of the water bath can be varied within an appropriate range, such as 75 °C-100 °C, H 2 o 2 The concentration can also be changed within an appropriate range, such as 8%-30%H 2 o 2 .

[0126] Two, the HPLC analysis method of formula (II) enrichment mother liquor

[0127] Take the enriched mother liquor of the compound of formula (II), dilute it with water to ...

Embodiment 2

[0154] Example 2 Preparation and identification of compounds of formula (III)

[0155] 1. Preparation of enriched mother liquor

[0156] Take Vitamin B 6 Add 1g of raw material drug to about 500ml of water to dissolve, adjust the pH to 5.0-6.0 with 1mol / L sodium hydroxide, fill with nitrogen for 30-60min, seal it, and light it for 20-30 days to obtain the enriched mother liquor of the compound of formula (III) in the form of Yellow clear liquid, stored at room temperature. In order to enrich enough crude product, 10 mother liquors were prepared in parallel.

[0157] Two, the HPLC analysis method of formula (III) enrichment mother liquor

[0158] Using the HPLC method, the enriched mother liquor of the compound of formula (III) is directly injected for analysis, and the generation of formula (III) is detected and its content is estimated by the area normalization method. The HPLC spectrum is shown in figure 2 . The amount of the compound of formula (III) gradually increas...

Embodiment 3

[0180] Example 3 Preparation and identification of compounds of formula (IV)

[0181] 1. Preparation of enriched mother liquor

[0182] Take Vitamin B 6 Add 2g of raw material medicine, add about 40ml of water to dissolve, and adjust the pH to 3.0-5.0 with 1mol / L sodium hydroxide. Put the solution in a vial, crimp the cap and seal it, and sterilize at 121°C for 1-2 hours to obtain the enriched mother solution of the compound of formula (IV), which is a light yellow clear liquid and stored at room temperature.

[0183] Two, the HPLC analysis method of formula (IV) compound mother liquor

[0184] Take the enriched mother liquor of the compound of formula (IV), dilute it with water to an appropriate concentration, use the HPLC method to detect the formation of the formula (IV) and estimate its content with the area normalization method, the HPLC spectrum is shown in image 3 . The content of the compound of formula (IV) in the solution sterilized for 2 hours is about 6%~7%, a...

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Abstract

The invention provides a preparation, separation and purification method of a vitamin B6 degradation impurity reference substance, which can be used for rapidly preparing a large amount of high-purity B6 degradation impurity reference substances at low cost, and solves the problem of lack of impurity reference substances in quality control and impurity research of vitamin B6 raw materials and preparations thereof at present. The invention provides favorable technical support for further improving the quality safety of vitamin B6 and preparation products thereof, guaranteeing the body health of consumers and the like, and has important practical significance.

Description

technical field [0001] The invention relates to the field of chemical pharmacy. More specifically, the present invention relates to vitamin B 6 Preparation, standardization and structural identification of impurities in APIs and marketed products, as well as their application as impurity reference substances. Background technique [0002] Vitamin B 6 , also known as pyridoxine. English name: Vitamin B 6 (abbreviation: VB 6 ), Chinese chemical name: 6-methyl-5-hydroxyl-3,4-pyridinedimethanol hydrochloride, chemical structural formula, the following formula (I): [0003] [0004] Vitamin B 6 As a water-soluble vitamin, it is more abundant in yeast, liver, grains, meat, fish, eggs, beans and peanuts. Vitamin B 6 As a component of coenzymes in the human body, it participates in a variety of metabolic reactions, especially closely related to amino acid metabolism. Vitamin B 6 The injection was first launched in Japan in 1957, with specifications of 1ml: 10mg and 1ml:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/444C07D213/66C07D213/68G01N30/02G01N30/06G01N30/34
CPCC07D207/444C07D213/68C07D213/66G01N30/02G01N30/06G01N30/34G01N2030/047G01N2030/062
Inventor 贾慧娟任晓慧侯伟李世奇
Owner TIANJIN CREATRON BIOTECHNOLOGY CO LTD
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