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Separation and purification method of caffeine impurity I

A technology for separation and purification of caffeine, applied in organic chemistry and other fields, can solve problems such as inability to locate and analyze

Inactive Publication Date: 2020-11-06
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] When the company was carrying out the filing of caffeine raw materials, it was found that there was an unknown impurity in the caffeine finished product. Although the content was less than 0.1%, it was necessary to carry out research on the caffeine impurity profile. Research, since it is impossible to conduct positioning analysis with known caffeine impurities on the market, it must be separated and purified, and then to explore the cause of its formation

Method used

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  • Separation and purification method of caffeine impurity I
  • Separation and purification method of caffeine impurity I
  • Separation and purification method of caffeine impurity I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 10g of caffeine finished product into 50-100 mesh silica gel to mix the sample and set aside.

[0031] Use 200-300 mesh silica gel to fill the column, and use 10:1 ethyl acetate:petroleum ether as the eluent to elute. After the column is equilibrated, put the mixed sample on the column, TLC monitoring, Rf=0.5, intercept target components. The obtained components were characterized by NMR, and compared with the fingerprint peaks, the purity of the target product in the components was about 30%.

Embodiment 2

[0033] Add 10g of caffeine finished product to 100-200 mesh silica gel to mix the sample and set aside.

[0034] Use 300-400 mesh silica gel to fill the column, and use 100:1 dichloromethane:methanol as the eluent to elute. After the column is equilibrated, put the mixed sample on the column, TLC monitoring, Rf=0.5, intercept the target material components. The obtained components were characterized by NMR, and compared with the fingerprint peaks, the purity of the target product in the components was about 80%.

Embodiment 3

[0036] Add 10g of caffeine finished product into 200-300 mesh silica gel to mix the sample and set aside.

[0037] Use 400-500 mesh silica gel to fill the column, and use 20:1 ethyl acetate:methanol as the eluent to elute. After the column is equilibrated, put the mixed sample on the column, TLC monitoring, Rf=0.5, intercept the target material components. The obtained components were characterized by NMR, and compared with the fingerprint peaks, the purity of the target product in the components was about 40%.

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Abstract

The invention provides a separation and purification method of a caffeine impurity I. The separation and purification method comprises the following steps of: (1) mixing a caffeine finished product with a sample, performing eluting with a normal-phase silica gel column, intercepting a target component, and conducting reduced pressure concentration to obtain a target crude product; and (2) carryingout secondary column chromatography on the target crude product obtained in the step (1), performing eluting with an eluent, collecting target components, and carrying out mixing concentration to obtain a pure target; and then carrying out nuclear magnetism and mass spectrometry analysis, and determining that the structure is the caffeine impurity I, namely 7-amino-1, 3-dimethyl-2, 4-dicarbonyl-1, 2, 3, 4-tetrahydropteridine-6-carboxylic acid.

Description

technical field [0001] The present invention relates to a new impurity of caffeine, especially 7-amino-1,3-dimethyl-2,4-dicarbonyl-1,2,3,4-tetrahydropteridine-6-carboxylic acid (referred to as impurity The separation and purification of I) belongs to the technical field of drug synthesis. Background technique [0002] Caffeine (Caffeine, caffeine) is a xanthine alkaloid, the chemical name is 1,3,7-trimethyl-3,7-dihydro-1H-purine-2,6-dione monohydrate, white crystal Powder, odorless, bitter taste, weathering. Caffeine is the main alkaloid in plants such as tea leaves, coffee beans, cocoa, and kola nuts, and has a strong excitatory central system effect. Widely used in medicine, food, cosmetics and other fields. Caffeine has physiological effects such as exciting the heart, skeletal muscle and central nervous system, anti-oxidation, relaxing blood vessels, and relaxing smooth muscle; it is commonly found in various foods such as tea, coffee, and cocoa. In recent years, caf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D475/02
CPCC07D475/02
Inventor 张富强常森易晓清
Owner SHANDONG XINHUA PHARMA CO LTD