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Preparation method of high-purity caffeine

A caffeine, high-purity technology, applied in separation methods, chemical instruments and methods, organic chemistry, etc., can solve the problems of affecting separation effect, limited separation capacity, complex extracts, etc., to improve preparation efficiency and high sample loading capacity. , the effect of high recovery rate

Active Publication Date: 2022-05-10
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, tea extracts are often very complex, and the traditional sublimation method for extracting caffeine has the disadvantage of high energy consumption; the traditional chromatographic separation method has limited separation ability. Although the traditional chromatographic method CN 202110628342. Methods Caffeine was extracted from coffee, the purity of which was only 81.32%-87.38%, which could not meet the development needs of caffeine standard products
There is also research (patent application number: 201811069217.2) to prepare caffeine from camellia powder by combining high-speed countercurrent chromatography and semi-preparative chromatography; When the concentration is 1mg, the separation of caffeine is overloaded, which affects the separation effect
In addition, the purity of caffeine prepared by this method is only 94.05%, which still cannot reach the level of standard product development

Method used

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  • Preparation method of high-purity caffeine
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  • Preparation method of high-purity caffeine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Take 1 kg of dried tea leaves, add ethanol at a ratio of 1:5 to liquid, and heat to reflux for 30 minutes. The resulting solution was concentrated to dryness by rotary evaporator. Add 1L of water, ultrasonically disperse and dissolve, then filter to obtain the filtrate;

[0032] The obtained filtrate is loaded onto a HPD 300 macroporous resin (inner diameter 10 cm, column bed height 30 cm) chromatographic column for adsorption. And wash the chromatographic column with water as the eluting reagent until the eluate is colorless. The macroporous resin chromatographic column is eluted with ethanol as the elution solvent, and the eluate is concentrated to dryness with a rotary evaporator, redissolved with water, and freeze-dried to obtain a brown-yellow tea extract. Take 100 mg of the tea extract, dissolve it in 2 mL of water, dissolve it by ultrasonic, remove the precipitate by centrifugation, and use it as the first sample injection solution;

[0033] A reversed-phas...

Embodiment 2

[0040] a. Take 1 kg of dried tea leaves, add ethanol at a ratio of 1:2 to liquid, and heat to reflux for 30 minutes. The resulting solution was concentrated to dryness by rotary evaporator. Add 1L of water, ultrasonically disperse and dissolve, then filter to obtain the filtrate;

[0041] The obtained filtrate is loaded onto a HPD 300 macroporous resin (inner diameter 10 cm, column bed height 30 cm) chromatographic column for adsorption. And wash the chromatographic column with water as the eluting reagent until the eluate is colorless. The macroporous resin chromatographic column is eluted with ethanol as the elution solvent, and the eluate is concentrated to dryness with a rotary evaporator, redissolved with water, and freeze-dried to obtain a brown-yellow tea extract. Take 100 mg of the tea extract, dissolve it in 5 mL of water, dissolve it by ultrasonic, remove the precipitate by centrifugation, and use it as the first sample injection solution;

[0042] b. A reversed-p...

Embodiment 3

[0046] a. Take 1 kg of dried tea leaves, add ethanol at a ratio of 1:3 to liquid, and heat to reflux for 30 minutes. The resulting solution was concentrated to dryness by rotary evaporator. Add 1L of water, ultrasonically disperse and dissolve, then filter to obtain the filtrate;

[0047] The obtained filtrate is loaded onto a HPD 300 macroporous resin (inner diameter 10 cm, column bed height 30 cm) chromatographic column for adsorption. And wash the chromatographic column with water as the eluting reagent until the eluate is colorless. The macroporous resin chromatographic column is eluted with ethanol as the elution solvent, and the eluate is concentrated to dryness with a rotary evaporator, redissolved with water, and freeze-dried to obtain a brown-yellow tea extract. Take 100mg of the tea extract, dissolve it in 1.42mL of water, dissolve it by ultrasonic, remove the precipitate by centrifugation, and use it as the first sample injection solution;

[0048] b. A reversed-...

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Abstract

The invention relates to a preparation method of high-purity caffeine, which comprises the following steps: combining two different reversed-phase chromatography methods, and purifying a tea extract to obtain a caffeine standard product with the purity higher than 98% by optimizing the relationship between the sample loading amount and the purity. Due to the fact that the removal effects of the two chromatography methods on different impurities are different, different types of impurities can be removed through combined use of the two chromatography methods, the sample loading capacity is increased, the preparation efficiency is improved, and the recovery rate can reach 85%. The method is simple and economical, and the obtained caffeine is high in purity, can be used as a reference substance for quality standard research work of tea leaves, can also be used for high-level plant raw materials, and provides effective assistance for related scientific research work.

Description

technical field [0001] The invention relates to the technical field of tea extracts, in particular to a method for preparing high-purity caffeine. Background technique [0002] As a means of separation, chromatography is widely used in pharmaceutical, chemical and other fields in modern society. Utilizing the differences in principles such as adsorption force, distribution coefficient, solubility, etc., the target compound can obtain continuous distribution on the chromatographic column, forming separable "color bands" (colorless substances will show different absorption peaks under specific detectors) ). Chromatographic technology has a wide range of applications, and the requirements for chromatographic technology are quite different under different needs. Combining chromatographic methods with different separation mechanisms can remove different types of impurities around the target compound, thereby achieving a more efficient purification effect than a single chromatog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/12B01D11/02B01D15/10B01D15/20B01D15/42
CPCC07D473/12B01D11/0265B01D15/424B01D15/203B01D15/10
Inventor 孙光映方辉平李长江史建俊李伟伟关婷婷姚武柯仲成杨李影
Owner HUANGSHAN UNIV
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